data_exp_344-sr
_audit_creation_date              2018-03-21
_audit_creation_method
;
Olex2 1.2
(compiled 2017.08.10 svn.r3458 for OlexSys, GUI svn.r5381)
;
_shelx_SHELXL_version_number      '2016/6'
_publ_contact_author_address      ?
_publ_contact_author_email        ?
_publ_contact_author_id_orcid     ?
_publ_contact_author_name         ''
_publ_contact_author_phone        ?
_publ_section_references
;
Dolomanov, O.V., Bourhis, L.J., Gildea, R.J, Howard, J.A.K. & Puschmann, H.
 (2009), J. Appl. Cryst. 42, 339-341.

Palatinus, L. & Chapuis, G. (2007). J. Appl. Cryst., 40, 786-790;
Palatinus, L. & van der Lee, A. (2008). J. Appl. Cryst. 41, 975-984;
Palatinus, L., Prathapa, S. J. & van Smaalen, S. (2012). J. Appl. Cryst. 45,
 575-580.

Sheldrick, G.M. (2015). Acta Cryst. C71, 3-8.
;
_chemical_name_common             ?
_chemical_name_systematic         ?
_chemical_formula_moiety          'C64 H45 B N6 Pd'
_chemical_formula_sum             'C64 H45 B N6 Pd'
_chemical_formula_weight          1015.27
_chemical_melting_point           ?
_chemical_oxdiff_formula          'C100 H100 B2 N12 Pd2 Cl4'
loop_
  _atom_type_symbol
  _atom_type_description
  _atom_type_scat_dispersion_real
  _atom_type_scat_dispersion_imag
  _atom_type_scat_source
 'C' 'C' 0.0181 0.0091 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
 'H' 'H' 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
 'B' 'B' 0.0090 0.0039 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
 'N' 'N' 0.0311 0.0180 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
 'Pd' 'Pd' 0.1215 3.9337 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_shelx_space_group_comment
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;
_space_group_crystal_system       'triclinic'
_space_group_IT_number            2
_space_group_name_H-M_alt         'P -1'
_space_group_name_Hall            '-P 1'
loop_
  _space_group_symop_operation_xyz
 'x, y, z'
 '-x, -y, -z'

_cell_length_a                    11.0064(3)
_cell_length_b                    14.0560(3)
_cell_length_c                    18.4924(5)
_cell_angle_alpha                 82.748(2)
_cell_angle_beta                  78.001(2)
_cell_angle_gamma                 87.7004(19)
_cell_volume                      2775.71(12)
_cell_formula_units_Z             2
_cell_measurement_reflns_used     18831
_cell_measurement_temperature     100.01(10)
_cell_measurement_theta_max       72.5200
_cell_measurement_theta_min       3.7800
_shelx_estimated_absorpt_T_max    ?
_shelx_estimated_absorpt_T_min    ?
_exptl_absorpt_coefficient_mu     3.031
_exptl_absorpt_correction_T_max   1.00000
_exptl_absorpt_correction_T_min   0.56646
_exptl_absorpt_correction_type    multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.38.46 (Rigaku Oxford Diffraction, 2015)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_absorpt_special_details    ?
_exptl_crystal_colour             'dark brown'
_exptl_crystal_colour_modifier    dark
_exptl_crystal_colour_primary     brown
_exptl_crystal_density_diffrn     1.215
_exptl_crystal_density_meas       ?
_exptl_crystal_density_method     ?
_exptl_crystal_description        plate
_exptl_crystal_F_000              1044
_exptl_crystal_recrystallization_method ?
_exptl_crystal_size_max           0.2
_exptl_crystal_size_mid           0.1
_exptl_crystal_size_min           0.02
_exptl_transmission_factor_max    ?
_exptl_transmission_factor_min    ?
_diffrn_reflns_av_R_equivalents   0.0758
_diffrn_reflns_av_unetI/netI      0.0624
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_limit_h_min -13
_diffrn_reflns_limit_h_max 13
_diffrn_reflns_limit_k_min -17
_diffrn_reflns_limit_k_max 17
_diffrn_reflns_limit_l_min -22
_diffrn_reflns_limit_l_max 22
_diffrn_reflns_number             9791
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_theta_full         66.598
_diffrn_reflns_theta_max          66.598
_diffrn_reflns_theta_min          3.772
_diffrn_ambient_environment       N~2~
_diffrn_ambient_temperature       100.01(10)
_diffrn_detector                  'CCD plate'
_diffrn_detector_area_resol_mean  8.0697
_diffrn_detector_type             EosS2
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_details
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  tₑₓₚ   ω     θ     κ     φ   Frames
--------------------------------------------------------------------------
  1  ω    -12.00  38.00   1.00    3.00    --   34.48 -38.00 -60.00   50
  2  ω     53.00 106.00   1.00    3.00    --   34.48  19.00 -90.00   53
  3  ω     74.00 101.00   1.00    3.00    --   34.48  77.00-120.00   27
  4  ω     66.00 101.00   1.00    3.00    --   34.48  77.00-180.00   35
  5  ω    115.00 174.00   1.00   12.00    --  107.46  77.00-120.00   59
  6  ω    136.00 169.00   1.00   12.00    --  107.46  61.00-150.00   33
  7  ω    122.00 172.00   1.00   12.00    --  107.46  77.00 -60.00   50
  8  ω    123.00 168.00   1.00   12.00    --  107.46  77.00   0.00   45
  9  ω    130.00 170.00   1.00   12.00    --  107.46  77.00  60.00   40
 10  ω    125.00 172.00   1.00   12.00    --  107.46  77.00 120.00   47
 11  ω    123.00 169.00   1.00   12.00    --  107.46  77.00 150.00   46
 12  ω    117.00 175.00   1.00   12.00    --  107.46  77.00  90.00   58
 13  ω    114.00 170.00   1.00   12.00    --  107.46  77.00 -30.00   56
 14  ω    121.00 147.00   1.00   12.00    --  107.46  61.00-120.00   26
 15  ω    123.00 174.00   1.00   12.00    --  107.46  77.00-180.00   51
 16  ω    119.00 171.00   1.00   12.00    --  107.46  77.00 -90.00   52
 17  ω     86.00 113.00   1.00   12.00    --  107.46  30.00-150.00   27
 18  ω     89.00 116.00   1.00   12.00    --  107.46  61.00-120.00   27
 19  ω     89.00 116.00   1.00   12.00    --  107.46  61.00 -90.00   27
 20  ω     89.00 115.00   1.00   12.00    --  107.46  61.00 -60.00   26
 21  ω     90.00 115.00   1.00   12.00    --  107.46  61.00 -30.00   25
 22  ω     89.00 115.00   1.00   12.00    --  107.46  61.00   0.00   26
 23  ω     90.00 117.00   1.00   12.00    --  107.46  61.00  30.00   27
 24  ω     90.00 125.00   1.00   12.00    --  107.46  61.00  60.00   35
 25  ω     86.00 112.00   1.00   12.00    --  107.46  30.00  90.00   26
 26  ω     89.00 115.00   1.00   12.00    --  107.46  61.00  90.00   26
 27  ω     89.00 116.00   1.00   12.00    --  107.46  61.00 120.00   27
 28  ω     89.00 116.00   1.00   12.00    --  107.46  61.00 150.00   27
 29  ω     81.00 107.00   1.00   12.00    --  107.46  77.00 120.00   26
 30  ω     81.00 107.00   1.00   12.00    --  107.46  77.00 150.00   26
 31  ω     81.00 107.00   1.00   12.00    --  107.46  77.00  90.00   26
 32  ω     81.00 107.00   1.00   12.00    --  107.46  77.00  60.00   26
 33  ω     81.00 175.00   1.00   12.00    --  107.46  77.00  30.00   94
 34  ω     86.00 116.00   1.00   12.00    --  107.46  30.00-120.00   30
 35  ω     90.00 115.00   1.00   12.00    --  107.46  61.00-150.00   25
 36  ω     90.00 115.00   1.00   12.00    --  107.46  61.00-180.00   25
 37  ω     82.00 111.00   1.00   12.00    --  107.46  77.00-120.00   29
 38  ω     81.00 107.00   1.00   12.00    --  107.46  77.00 -90.00   26
 39  ω     81.00 107.00   1.00   12.00    --  107.46  77.00 -60.00   26
 40  ω     81.00 107.00   1.00   12.00    --  107.46  77.00 -30.00   26
 41  ω     81.00 107.00   1.00   12.00    --  107.46  77.00   0.00   26
 42  ω     86.00 122.00   1.00   12.00    --  107.46  30.00 -30.00   36
 43  ω     86.00 118.00   1.00   12.00    --  107.46  30.00   0.00   32
 44  ω     86.00 113.00   1.00   12.00    --  107.46  30.00  30.00   27
 45  ω     86.00 112.00   1.00   12.00    --  107.46  30.00  60.00   26
 46  ω     69.00 103.00   1.00   12.00    --  107.46  15.00 150.00   34
 47  ω     86.00 119.00   1.00   12.00    --  107.46  30.00 150.00   33
 48  ω     75.00 102.00   1.00    3.00    --   34.48  77.00  30.00   27
 49  ω     73.00 104.00   1.00    3.00    --   34.48  38.00  90.00   31
 50  ω     64.00  97.00   1.00    3.00    --   34.48  57.00  90.00   33
 51  ω     63.00  90.00   1.00    3.00    --   34.48  77.00   0.00   27
 52  ω     62.00  89.00   1.00    3.00    --   34.48  38.00 -30.00   27
 53  ω     25.00  61.00   1.00    3.00    --   34.48  77.00  30.00   36
 54  ω     22.00  50.00   1.00    3.00    --   34.48  38.00  90.00   28
 55  ω     21.00  61.00   1.00    3.00    --   34.48  57.00  90.00   40
 56  ω     19.00  98.00   1.00    3.00    --   34.48  57.00   0.00   79
 57  ω     86.00 118.00   1.00   12.00    --  107.46  30.00 -90.00   32
 58  ω     86.00 113.00   1.00   12.00    --  107.46  30.00 -60.00   27
 59  ω     81.00 107.00   1.00   12.00    --  107.46  77.00-150.00   26
 60  ω     81.00 107.00   1.00   12.00    --  107.46  77.00-180.00   26
 61  ω     86.00 113.00   1.00   12.00    --  107.46  30.00-180.00   27
 62  ω     42.00  85.00   1.00   12.00    --  107.46 -77.00-180.00   43
 63  ω    103.00 134.00   1.00   12.00    --  107.46 -77.00-180.00   31
 64  ω     58.00 103.00   1.00   12.00    --  107.46-111.00 -90.00   45
 65  ω     55.00 115.00   1.00   12.00    --  107.46-111.00   0.00   60
 66  ω     78.00 107.00   1.00   12.00    --  107.46 -94.00  90.00   29
 67  ω     45.00 109.00   1.00   12.00    --  107.46 -94.00 150.00   64
 68  ω     38.00  64.00   1.00   12.00    --  107.46 -94.00  90.00   26
 69  ω     40.00 125.00   1.00   12.00    --  107.46 -77.00   0.00   85
 70  ω     36.00  88.00   1.00    3.00    --   34.48-125.00 -90.00   52
 71  ω    -14.00  48.00   1.00    3.00    --   34.48 -57.00   0.00   62
 72  ω     24.00  88.00   1.00    3.00    --   34.48-125.00 120.00   64
 73  ω      5.00  42.00   1.00    3.00    --   34.48  19.00 -90.00   37
 74  ω     16.00  52.00   1.00    3.00    --   34.48  38.00 -30.00   36
 75  ω     13.00  48.00   1.00    3.00    --   34.48  77.00   0.00   35
 76  ω     10.00  76.00   1.00    3.00    --   34.48  77.00 -60.00   66
 77  ω     10.00  46.00   1.00    3.00    --   34.48  77.00-180.00   36
 78  ω      8.00  60.00   1.00    3.00    --   34.48  77.00-120.00   52
 79  ω     -2.00  23.00   1.00    3.00    --   34.48  95.00  -4.52   25
 80  ω      8.00 102.00   1.00    3.00    --   34.48  77.00 120.00   94
 81  ω    -30.00  -5.00   1.00    3.00    --  -34.48 125.00   0.00   25
 82  ω    -25.00  50.00   1.00    3.00    --   34.48 -57.00-180.00   75
 83  ω    -31.00  51.00   1.00    3.00    --   34.48 -57.00 -90.00   82
 84  ω    -35.00  50.00   1.00    3.00    --   34.48 -38.00  90.00   85
 85  ω    -84.00 -58.00   1.00    3.00    --  -34.48 125.00   0.00   26
;
_diffrn_measurement_device        'four-circle diffractometer'
_diffrn_measurement_device_type   'SuperNova, Dual, Cu at zero, EosS2'
_diffrn_measurement_method        'ω scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11       0.0673916000
_diffrn_orient_matrix_UB_12       0.0764621000
_diffrn_orient_matrix_UB_13       -0.0605359000
_diffrn_orient_matrix_UB_21       0.0968433000
_diffrn_orient_matrix_UB_22       -0.0759479000
_diffrn_orient_matrix_UB_23       -0.0286572000
_diffrn_orient_matrix_UB_31       -0.0809941000
_diffrn_orient_matrix_UB_32       -0.0243962000
_diffrn_orient_matrix_UB_33       -0.0536205000
_diffrn_radiation_monochromator   mirror
_diffrn_radiation_probe           x-ray
_diffrn_radiation_type            CuK\a
_diffrn_radiation_wavelength      1.54184
_diffrn_source                    'micro-focus sealed X-ray tube'
_diffrn_source_type               'SuperNova (Cu) X-ray Source'
_reflns_Friedel_coverage          0.000
_reflns_Friedel_fraction_full     .
_reflns_Friedel_fraction_max      .
_reflns_number_gt                 8686
_reflns_number_total              9791
_reflns_odcompleteness_completeness 99.97
_reflns_odcompleteness_iscentric  1
_reflns_odcompleteness_theta      66.97
_reflns_special_details
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
;
_reflns_threshold_expression      'I > 2σ(I)'
_computing_cell_refinement        'CrysAlisPro 1.171.38.46 (Rigaku OD, 2015)'
_computing_data_collection        'CrysAlisPro 1.171.38.46 (Rigaku OD, 2015)'
_computing_data_reduction         'CrysAlisPro 1.171.38.46 (Rigaku OD, 2015)'
_computing_molecular_graphics     'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material   'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement   'ShelXL (Sheldrick, 2015)'
_computing_structure_solution
;
Superflip (Palatinus & Chapuis, 2007;Palatinus & van der Lee, 2008;
Palatinus et al., 2012)
;
_refine_diff_density_max          0.964
_refine_diff_density_min          -1.373
_refine_diff_density_rms          0.098
_refine_ls_extinction_coef        .
_refine_ls_extinction_method      none
_refine_ls_goodness_of_fit_ref    1.057
_refine_ls_hydrogen_treatment     constr
_refine_ls_matrix_type            full
_refine_ls_number_parameters      654
_refine_ls_number_reflns          9791
_refine_ls_number_restraints      0
_refine_ls_R_factor_all           0.0570
_refine_ls_R_factor_gt            0.0487
_refine_ls_restrained_S_all       1.057
_refine_ls_shift/su_max           0.001
_refine_ls_shift/su_mean          0.000
_refine_ls_structure_factor_coef  Fsqd
_refine_ls_weighting_details
'w=1/[σ²(Fo²)+(0.0827P)²+0.9128P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme       calc
_refine_ls_wR_factor_gt           0.1262
_refine_ls_wR_factor_ref          0.1303
_refine_special_details           ?
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2.a Aromatic/amide H refined with riding coordinates:
 C2(H2), C3(H3), C7(H7), C13(H13), C17(H17), C18(H18), C22(H22), C23(H23),
 C27(H27), C28(H28), C31(H31), C32(H32), C34(H34), C35(H35), C38(H38), C39(H39),
  C41(H41), C42(H42), C45(H45), C46(H46), C48(H48), C49(H49), C52(H52),
 C53(H53), C55(H55), C56(H56), C59(H59), C60(H60), C62(H62), C63(H63)
2.b Idealised Me refined as rotating group:
 C36(H36A,H36B,H36C), C43(H43A,H43B,H43C), C50(H50A,H50B,H50C), C57(H57A,H57B,
 H57C), C64(H64A,H64B,H64C)
;
_atom_sites_solution_hydrogens    geom
_atom_sites_solution_primary      iterative
_atom_sites_solution_secondary    ?
loop_
  _atom_site_label
  _atom_site_type_symbol
  _atom_site_fract_x
  _atom_site_fract_y
  _atom_site_fract_z
  _atom_site_U_iso_or_equiv
  _atom_site_adp_type
  _atom_site_occupancy
  _atom_site_site_symmetry_order
  _atom_site_calc_flag
  _atom_site_refinement_flags_posn
  _atom_site_refinement_flags_adp
  _atom_site_refinement_flags_occupancy
  _atom_site_disorder_assembly
  _atom_site_disorder_group
 Pd1 Pd 0.93343(2) 0.69622(2) -0.02749(2) 0.01588(9) Uani 1 1 d . . . . .
 N1 N 1.1143(2) 0.78169(17) 0.24560(15) 0.0182(5) Uani 1 1 d . . . . .
 N2 N 1.0438(2) 0.84745(17) 0.13656(15) 0.0177(5) Uani 1 1 d . . . . .
 N3 N 0.9766(2) 0.69307(18) 0.19807(14) 0.0173(5) Uani 1 1 d . . . . .
 N4 N 1.0238(2) 0.81618(18) -0.08786(15) 0.0192(5) Uani 1 1 d . . . . .
 N5 N 0.8871(3) 0.66200(18) -0.12410(14) 0.0190(5) Uani 1 1 d . . . . .
 N6 N 0.8642(2) 0.56602(18) 0.02657(15) 0.0186(5) Uani 1 1 d . . . . .
 C1 C 1.1344(3) 0.7053(2) 0.29504(18) 0.0221(7) Uani 1 1 d . . . . .
 C2 C 1.2353(3) 0.7326(2) 0.32618(19) 0.0257(7) Uani 1 1 d . . . . .
 H2 H 1.267892 0.696382 0.363517 0.031 Uiso 1 1 calc R . . . .
 C3 C 1.2750(3) 0.8210(2) 0.29158(19) 0.0254(7) Uani 1 1 d . . . . .
 H3 H 1.339234 0.855205 0.301349 0.031 Uiso 1 1 calc R . . . .
 C4 C 1.2002(3) 0.8520(2) 0.23731(18) 0.0200(6) Uani 1 1 d . . . . .
 C5 C 1.2065(3) 0.9253(2) 0.17652(18) 0.0208(7) Uani 1 1 d . . . . .
 C6 C 1.1340(3) 0.9148(2) 0.12254(17) 0.0193(6) Uani 1 1 d . . . . .
 C7 C 1.1556(3) 0.9444(2) 0.04379(18) 0.0190(6) Uani 1 1 d . . . . .
 H7 H 1.208574 0.992765 0.017830 0.023 Uiso 1 1 calc R . . . .
 C8 C 1.0837(3) 0.8884(2) 0.01351(18) 0.0191(6) Uani 1 1 d . . . . .
 C9 C 1.0170(3) 0.8229(2) 0.07264(17) 0.0165(6) Uani 1 1 d . . . . .
 C10 C 0.9595(3) 0.7361(2) 0.06868(16) 0.0149(6) Uani 1 1 d . . . . .
 C11 C 0.9454(3) 0.6716(2) 0.13432(17) 0.0175(6) Uani 1 1 d . . . . .
 C12 C 0.9255(3) 0.5703(2) 0.14556(17) 0.0175(6) Uani 1 1 d . . . . .
 C13 C 0.9568(3) 0.5339(2) 0.21273(18) 0.0205(7) Uani 1 1 d . . . . .
 H13 H 0.953419 0.470037 0.233498 0.025 Uiso 1 1 calc R . . . .
 C14 C 0.9954(3) 0.6136(2) 0.24442(17) 0.0200(6) Uani 1 1 d . . . . .
 C15 C 1.0672(3) 0.6188(2) 0.29949(18) 0.0223(7) Uani 1 1 d . . . . .
 C16 C 1.0829(3) 0.8843(2) -0.06358(18) 0.0194(6) Uani 1 1 d . . . . .
 C17 C 1.1451(3) 0.9487(2) -0.12417(18) 0.0208(7) Uani 1 1 d . . . . .
 H17 H 1.189895 1.002089 -0.120890 0.025 Uiso 1 1 calc R . . . .
 C18 C 1.1271(3) 0.9180(2) -0.18732(19) 0.0221(7) Uani 1 1 d . . . . .
 H18 H 1.157908 0.945928 -0.235688 0.027 Uiso 1 1 calc R . . . .
 C19 C 1.0514(3) 0.8340(2) -0.16582(18) 0.0198(6) Uani 1 1 d . . . . .
 C20 C 1.0056(3) 0.7856(2) -0.21410(18) 0.0229(7) Uani 1 1 d . . . . .
 C21 C 0.9182(3) 0.7098(2) -0.19467(18) 0.0217(7) Uani 1 1 d . . . . .
 C22 C 0.8551(3) 0.6709(2) -0.24404(19) 0.0256(7) Uani 1 1 d . . . . .
 H22 H 0.862459 0.690230 -0.294722 0.031 Uiso 1 1 calc R . . . .
 C23 C 0.7821(3) 0.5999(2) -0.20231(19) 0.0248(7) Uani 1 1 d . . . . .
 H23 H 0.727720 0.562727 -0.218769 0.030 Uiso 1 1 calc R . . . .
 C24 C 0.8047(3) 0.5930(2) -0.12843(18) 0.0204(6) Uani 1 1 d . . . . .
 C25 C 0.7642(3) 0.5171(2) -0.07153(18) 0.0210(7) Uani 1 1 d . . . . .
 C26 C 0.7994(3) 0.5023(2) -0.00374(18) 0.0185(6) Uani 1 1 d . . . . .
 C27 C 0.7745(3) 0.4177(2) 0.04941(19) 0.0221(7) Uani 1 1 d . . . . .
 H27 H 0.730781 0.364464 0.044407 0.027 Uiso 1 1 calc R . . . .
 C28 C 0.8261(3) 0.4294(2) 0.10775(18) 0.0205(7) Uani 1 1 d . . . . .
 H28 H 0.827472 0.384935 0.149326 0.025 Uiso 1 1 calc R . . . .
 C29 C 0.8782(3) 0.5232(2) 0.09354(17) 0.0175(6) Uani 1 1 d . . . . .
 C30 C 0.8831(3) 0.8396(2) 0.26557(18) 0.0202(6) Uani 1 1 d . . . . .
 C31 C 0.8930(3) 0.8806(2) 0.32856(19) 0.0248(7) Uani 1 1 d . . . . .
 H31 H 0.970492 0.881904 0.341051 0.030 Uiso 1 1 calc R . . . .
 C32 C 0.7908(4) 0.9197(2) 0.37370(19) 0.0289(8) Uani 1 1 d . . . . .
 H32 H 0.801057 0.945857 0.415763 0.035 Uiso 1 1 calc R . . . .
 C33 C 0.6749(4) 0.9201(3) 0.3567(2) 0.0337(9) Uani 1 1 d . . . . .
 C34 C 0.6628(3) 0.8809(3) 0.2923(2) 0.0359(9) Uani 1 1 d . . . . .
 H34 H 0.585912 0.881731 0.278819 0.043 Uiso 1 1 calc R . . . .
 C35 C 0.7649(3) 0.8411(3) 0.2490(2) 0.0291(8) Uani 1 1 d . . . . .
 H35 H 0.754560 0.814275 0.207210 0.035 Uiso 1 1 calc R . . . .
 C36 C 0.5615(5) 0.9617(4) 0.4057(3) 0.0576(14) Uani 1 1 d . . . . .
 H36A H 0.541583 0.921858 0.452551 0.086 Uiso 1 1 calc GR . . . .
 H36B H 0.492245 0.964113 0.381303 0.086 Uiso 1 1 calc GR . . . .
 H36C H 0.579241 1.025270 0.413946 0.086 Uiso 1 1 calc GR . . . .
 C37 C 1.2998(3) 1.0026(2) 0.15984(18) 0.0213(7) Uani 1 1 d . . . . .
 C38 C 1.2701(3) 1.0940(2) 0.12856(19) 0.0235(7) Uani 1 1 d . . . . .
 H38 H 1.190230 1.107162 0.120473 0.028 Uiso 1 1 calc R . . . .
 C39 C 1.3590(3) 1.1658(2) 0.1093(2) 0.0295(8) Uani 1 1 d . . . . .
 H39 H 1.337822 1.226155 0.088120 0.035 Uiso 1 1 calc R . . . .
 C40 C 1.4787(3) 1.1483(3) 0.1213(2) 0.0324(8) Uani 1 1 d . . . . .
 C41 C 1.5084(4) 1.0577(3) 0.1526(2) 0.0344(9) Uani 1 1 d . . . . .
 H41 H 1.588097 1.045232 0.161260 0.041 Uiso 1 1 calc R . . . .
 C42 C 1.4210(3) 0.9852(2) 0.1712(2) 0.0280(7) Uani 1 1 d . . . . .
 H42 H 1.443225 0.924675 0.191455 0.034 Uiso 1 1 calc R . . . .
 C43 C 1.5744(4) 1.2262(3) 0.1002(3) 0.0465(11) Uani 1 1 d . . . . .
 H43A H 1.537768 1.283767 0.079716 0.070 Uiso 1 1 calc GR . . . .
 H43B H 1.642998 1.206089 0.063870 0.070 Uiso 1 1 calc GR . . . .
 H43C H 1.603372 1.238216 0.143688 0.070 Uiso 1 1 calc GR . . . .
 C44 C 1.0810(3) 0.5347(2) 0.35359(18) 0.0247(7) Uani 1 1 d . . . . .
 C45 C 0.9764(4) 0.4821(3) 0.3899(2) 0.0302(8) Uani 1 1 d . . . . .
 H45 H 0.899428 0.500288 0.378885 0.036 Uiso 1 1 calc R . . . .
 C46 C 0.9846(4) 0.4033(3) 0.4421(2) 0.0380(10) Uani 1 1 d . . . . .
 H46 H 0.913361 0.369625 0.465728 0.046 Uiso 1 1 calc R . . . .
 C47 C 1.0979(5) 0.3742(3) 0.4594(2) 0.0393(10) Uani 1 1 d . . . . .
 C48 C 1.2041(4) 0.4249(3) 0.4217(2) 0.0351(9) Uani 1 1 d . . . . .
 H48 H 1.281333 0.405461 0.431683 0.042 Uiso 1 1 calc R . . . .
 C49 C 1.1955(4) 0.5038(2) 0.3695(2) 0.0298(8) Uani 1 1 d . . . . .
 H49 H 1.267045 0.536478 0.344910 0.036 Uiso 1 1 calc R . . . .
 C50 C 1.1059(5) 0.2906(3) 0.5184(2) 0.0494(12) Uani 1 1 d . . . . .
 H50A H 1.077403 0.310848 0.566831 0.074 Uiso 1 1 calc GR . . . .
 H50B H 1.190535 0.268453 0.513462 0.074 Uiso 1 1 calc GR . . . .
 H50C H 1.054879 0.239586 0.512368 0.074 Uiso 1 1 calc GR . . . .
 C51 C 1.0512(4) 0.8150(2) -0.29556(19) 0.0279(8) Uani 1 1 d . . . . .
 C52 C 0.9794(4) 0.8666(3) -0.3396(2) 0.0414(10) Uani 1 1 d . . . . .
 H52 H 0.899551 0.886142 -0.318505 0.050 Uiso 1 1 calc R . . . .
 C53 C 1.0253(5) 0.8901(3) -0.4160(2) 0.0502(12) Uani 1 1 d . . . . .
 H53 H 0.975023 0.924050 -0.445244 0.060 Uiso 1 1 calc R . . . .
 C54 C 1.1453(5) 0.8632(3) -0.4488(2) 0.0511(13) Uani 1 1 d . . . . .
 C55 C 1.2172(5) 0.8118(3) -0.4049(3) 0.0575(14) Uani 1 1 d . . . . .
 H55 H 1.297436 0.792911 -0.425779 0.069 Uiso 1 1 calc R . . . .
 C56 C 1.1703(5) 0.7879(3) -0.3288(2) 0.0463(11) Uani 1 1 d . . . . .
 H56 H 1.220095 0.752886 -0.299709 0.056 Uiso 1 1 calc R . . . .
 C57 C 1.1991(7) 0.8911(4) -0.5305(3) 0.0728(19) Uani 1 1 d . . . . .
 H57A H 1.133813 0.894986 -0.558092 0.109 Uiso 1 1 calc GR . . . .
 H57B H 1.259494 0.843736 -0.548221 0.109 Uiso 1 1 calc GR . . . .
 H57C H 1.238156 0.952330 -0.537113 0.109 Uiso 1 1 calc GR . . . .
 C58 C 0.6778(3) 0.4460(2) -0.08734(18) 0.0214(7) Uani 1 1 d . . . . .
 C59 C 0.5564(3) 0.4738(3) -0.0906(2) 0.0313(8) Uani 1 1 d . . . . .
 H59 H 0.531302 0.537200 -0.086618 0.038 Uiso 1 1 calc R . . . .
 C60 C 0.4719(3) 0.4077(3) -0.0999(3) 0.0387(10) Uani 1 1 d . . . . .
 H60 H 0.391478 0.427757 -0.103116 0.046 Uiso 1 1 calc R . . . .
 C61 C 0.5064(3) 0.3113(3) -0.1044(2) 0.0341(9) Uani 1 1 d . . . . .
 C62 C 0.6285(3) 0.2857(3) -0.1047(2) 0.0287(8) Uani 1 1 d . . . . .
 H62 H 0.654471 0.222985 -0.110978 0.034 Uiso 1 1 calc R . . . .
 C63 C 0.7142(3) 0.3512(2) -0.09574(19) 0.0250(7) Uani 1 1 d . . . . .
 H63 H 0.795862 0.331706 -0.095359 0.030 Uiso 1 1 calc R . . . .
 C64 C 0.4127(4) 0.2396(3) -0.1110(3) 0.0550(14) Uani 1 1 d . . . . .
 H64A H 0.417796 0.232808 -0.162534 0.082 Uiso 1 1 calc GR . . . .
 H64B H 0.330823 0.261364 -0.089779 0.082 Uiso 1 1 calc GR . . . .
 H64C H 0.429795 0.178726 -0.084781 0.082 Uiso 1 1 calc GR . . . .
 B1 B 1.0004(3) 0.7933(2) 0.2130(2) 0.0181(7) Uani 1 1 d . . . . .


_geom_special_details
;
 All esds (except the esd in the dihedral angle between two l.s. planes)
 are estimated using the full covariance matrix.  The cell esds are taken
 into account individually in the estimation of esds in distances, angles
 and torsion angles; correlations between esds in cell parameters are only
 used when they are defined by crystal symmetry.  An approximate (isotropic)
 treatment of cell esds is used for estimating esds involving l.s. planes.
;
loop_
  _geom_bond_atom_site_label_1
  _geom_bond_atom_site_label_2
  _geom_bond_distance
  _geom_bond_site_symmetry_2
  _geom_bond_publ_flag
 Pd1 N4 2.068(3) . ?
 Pd1 N5 2.073(3) . ?
 Pd1 N6 2.065(3) . ?
 Pd1 C10 2.009(3) . ?
 N1 C1 1.362(4) . ?
 N1 C4 1.367(4) . ?
 N1 B1 1.495(5) . ?
 N2 C6 1.362(4) . ?
 N2 C9 1.364(4) . ?
 N2 B1 1.511(4) . ?
 N3 C11 1.366(4) . ?
 N3 C14 1.356(4) . ?
 N3 B1 1.513(4) . ?
 N4 C16 1.349(4) . ?
 N4 C19 1.402(4) . ?
 N5 C21 1.372(4) . ?
 N5 C24 1.375(4) . ?
 N6 C26 1.403(4) . ?
 N6 C29 1.343(4) . ?
 C1 C2 1.438(5) . ?
 C1 C15 1.433(4) . ?
 C2 C3 1.368(5) . ?
 C3 C4 1.442(5) . ?
 C4 C5 1.418(5) . ?
 C5 C6 1.426(5) . ?
 C5 C37 1.484(4) . ?
 C6 C7 1.436(4) . ?
 C7 C8 1.381(5) . ?
 C8 C9 1.431(4) . ?
 C8 C16 1.436(5) . ?
 C9 C10 1.413(4) . ?
 C10 C11 1.406(4) . ?
 C11 C12 1.431(4) . ?
 C12 C13 1.388(5) . ?
 C12 C29 1.425(5) . ?
 C13 C14 1.445(4) . ?
 C14 C15 1.423(5) . ?
 C15 C44 1.473(5) . ?
 C16 C17 1.420(4) . ?
 C17 C18 1.348(5) . ?
 C18 C19 1.438(4) . ?
 C19 C20 1.372(5) . ?
 C20 C21 1.425(5) . ?
 C20 C51 1.496(4) . ?
 C21 C22 1.427(5) . ?
 C22 C23 1.360(5) . ?
 C23 C24 1.430(5) . ?
 C24 C25 1.415(5) . ?
 C25 C26 1.376(5) . ?
 C25 C58 1.500(4) . ?
 C26 C27 1.441(4) . ?
 C27 C28 1.349(5) . ?
 C28 C29 1.431(4) . ?
 C30 C31 1.388(5) . ?
 C30 C35 1.396(5) . ?
 C30 B1 1.614(4) . ?
 C31 C32 1.393(5) . ?
 C32 C33 1.376(6) . ?
 C33 C34 1.406(6) . ?
 C33 C36 1.525(5) . ?
 C34 C35 1.380(5) . ?
 C37 C38 1.396(5) . ?
 C37 C42 1.401(5) . ?
 C38 C39 1.395(5) . ?
 C39 C40 1.388(6) . ?
 C40 C41 1.387(6) . ?
 C40 C43 1.508(5) . ?
 C41 C42 1.391(5) . ?
 C44 C45 1.394(5) . ?
 C44 C49 1.394(6) . ?
 C45 C46 1.389(5) . ?
 C46 C47 1.384(7) . ?
 C47 C48 1.401(6) . ?
 C47 C50 1.512(5) . ?
 C48 C49 1.389(5) . ?
 C51 C52 1.374(6) . ?
 C51 C56 1.388(6) . ?
 C52 C53 1.399(6) . ?
 C53 C54 1.392(8) . ?
 C54 C55 1.372(8) . ?
 C54 C57 1.512(5) . ?
 C55 C56 1.397(6) . ?
 C58 C59 1.389(5) . ?
 C58 C63 1.395(5) . ?
 C59 C60 1.390(5) . ?
 C60 C61 1.400(5) . ?
 C61 C62 1.377(5) . ?
 C61 C64 1.504(5) . ?
 C62 C63 1.392(5) . ?

loop_
  _geom_angle_atom_site_label_1
  _geom_angle_atom_site_label_2
  _geom_angle_atom_site_label_3
  _geom_angle
  _geom_angle_site_symmetry_1
  _geom_angle_site_symmetry_3
  _geom_angle_publ_flag
 N4 Pd1 N5 89.21(11) . . ?
 N6 Pd1 N4 172.22(10) . . ?
 N6 Pd1 N5 89.14(11) . . ?
 C10 Pd1 N4 91.54(11) . . ?
 C10 Pd1 N5 173.63(11) . . ?
 C10 Pd1 N6 90.94(11) . . ?
 C1 N1 C4 112.6(3) . . ?
 C1 N1 B1 123.2(3) . . ?
 C4 N1 B1 123.6(3) . . ?
 C6 N2 C9 112.0(3) . . ?
 C6 N2 B1 122.3(3) . . ?
 C9 N2 B1 124.6(3) . . ?
 C11 N3 B1 124.4(3) . . ?
 C14 N3 C11 112.5(3) . . ?
 C14 N3 B1 122.8(3) . . ?
 C16 N4 Pd1 128.7(2) . . ?
 C16 N4 C19 105.9(3) . . ?
 C19 N4 Pd1 124.8(2) . . ?
 C21 N5 Pd1 128.0(2) . . ?
 C21 N5 C24 105.5(3) . . ?
 C24 N5 Pd1 126.1(2) . . ?
 C26 N6 Pd1 124.9(2) . . ?
 C29 N6 Pd1 127.9(2) . . ?
 C29 N6 C26 107.1(3) . . ?
 N1 C1 C2 105.4(3) . . ?
 N1 C1 C15 119.1(3) . . ?
 C15 C1 C2 135.1(3) . . ?
 C3 C2 C1 108.4(3) . . ?
 C2 C3 C4 108.2(3) . . ?
 N1 C4 C3 105.1(3) . . ?
 N1 C4 C5 118.1(3) . . ?
 C5 C4 C3 136.1(3) . . ?
 C4 C5 C6 117.8(3) . . ?
 C4 C5 C37 122.9(3) . . ?
 C6 C5 C37 118.4(3) . . ?
 N2 C6 C5 120.6(3) . . ?
 N2 C6 C7 105.8(3) . . ?
 C5 C6 C7 131.4(3) . . ?
 C8 C7 C6 107.8(3) . . ?
 C7 C8 C9 107.9(3) . . ?
 C7 C8 C16 128.5(3) . . ?
 C9 C8 C16 123.2(3) . . ?
 N2 C9 C8 105.9(3) . . ?
 N2 C9 C10 123.5(3) . . ?
 C10 C9 C8 129.0(3) . . ?
 C9 C10 Pd1 122.9(2) . . ?
 C11 C10 Pd1 121.8(2) . . ?
 C11 C10 C9 114.1(3) . . ?
 N3 C11 C10 123.1(3) . . ?
 N3 C11 C12 105.6(3) . . ?
 C10 C11 C12 129.9(3) . . ?
 C13 C12 C11 108.1(3) . . ?
 C13 C12 C29 130.3(3) . . ?
 C29 C12 C11 121.6(3) . . ?
 C12 C13 C14 107.3(3) . . ?
 N3 C14 C13 105.7(3) . . ?
 N3 C14 C15 120.2(3) . . ?
 C15 C14 C13 132.4(3) . . ?
 C1 C15 C44 122.0(3) . . ?
 C14 C15 C1 117.1(3) . . ?
 C14 C15 C44 120.7(3) . . ?
 N4 C16 C8 123.6(3) . . ?
 N4 C16 C17 111.0(3) . . ?
 C17 C16 C8 125.4(3) . . ?
 C18 C17 C16 107.4(3) . . ?
 C17 C18 C19 107.1(3) . . ?
 N4 C19 C18 108.6(3) . . ?
 C20 C19 N4 126.3(3) . . ?
 C20 C19 C18 124.8(3) . . ?
 C19 C20 C21 126.6(3) . . ?
 C19 C20 C51 117.1(3) . . ?
 C21 C20 C51 116.2(3) . . ?
 N5 C21 C20 122.9(3) . . ?
 N5 C21 C22 110.8(3) . . ?
 C20 C21 C22 126.3(3) . . ?
 C23 C22 C21 106.4(3) . . ?
 C22 C23 C24 107.2(3) . . ?
 N5 C24 C23 110.1(3) . . ?
 N5 C24 C25 124.5(3) . . ?
 C25 C24 C23 124.7(3) . . ?
 C24 C25 C58 117.1(3) . . ?
 C26 C25 C24 125.3(3) . . ?
 C26 C25 C58 117.6(3) . . ?
 N6 C26 C27 107.6(3) . . ?
 C25 C26 N6 126.9(3) . . ?
 C25 C26 C27 125.5(3) . . ?
 C28 C27 C26 107.8(3) . . ?
 C27 C28 C29 107.0(3) . . ?
 N6 C29 C12 123.6(3) . . ?
 N6 C29 C28 110.4(3) . . ?
 C12 C29 C28 125.6(3) . . ?
 C31 C30 C35 116.3(3) . . ?
 C31 C30 B1 122.8(3) . . ?
 C35 C30 B1 120.9(3) . . ?
 C30 C31 C32 122.2(3) . . ?
 C33 C32 C31 120.7(3) . . ?
 C32 C33 C34 118.2(3) . . ?
 C32 C33 C36 121.6(4) . . ?
 C34 C33 C36 120.2(4) . . ?
 C35 C34 C33 120.1(4) . . ?
 C34 C35 C30 122.4(3) . . ?
 C38 C37 C5 120.3(3) . . ?
 C38 C37 C42 118.1(3) . . ?
 C42 C37 C5 121.5(3) . . ?
 C39 C38 C37 120.8(3) . . ?
 C40 C39 C38 120.8(3) . . ?
 C39 C40 C43 120.6(4) . . ?
 C41 C40 C39 118.6(3) . . ?
 C41 C40 C43 120.8(4) . . ?
 C40 C41 C42 121.1(4) . . ?
 C41 C42 C37 120.6(3) . . ?
 C45 C44 C15 119.4(3) . . ?
 C49 C44 C15 122.7(3) . . ?
 C49 C44 C45 117.9(3) . . ?
 C46 C45 C44 121.4(4) . . ?
 C47 C46 C45 120.6(4) . . ?
 C46 C47 C48 118.4(4) . . ?
 C46 C47 C50 120.5(4) . . ?
 C48 C47 C50 121.1(4) . . ?
 C49 C48 C47 120.8(4) . . ?
 C48 C49 C44 120.8(4) . . ?
 C52 C51 C20 122.8(3) . . ?
 C52 C51 C56 118.2(4) . . ?
 C56 C51 C20 119.0(4) . . ?
 C51 C52 C53 120.6(4) . . ?
 C54 C53 C52 120.9(5) . . ?
 C53 C54 C57 122.0(5) . . ?
 C55 C54 C53 118.6(4) . . ?
 C55 C54 C57 119.4(5) . . ?
 C54 C55 C56 120.2(5) . . ?
 C51 C56 C55 121.6(5) . . ?
 C59 C58 C25 119.4(3) . . ?
 C59 C58 C63 118.6(3) . . ?
 C63 C58 C25 121.9(3) . . ?
 C58 C59 C60 120.7(3) . . ?
 C59 C60 C61 120.8(4) . . ?
 C60 C61 C64 120.4(4) . . ?
 C62 C61 C60 117.9(3) . . ?
 C62 C61 C64 121.7(3) . . ?
 C61 C62 C63 121.8(3) . . ?
 C62 C63 C58 120.1(3) . . ?
 N1 B1 N2 104.4(3) . . ?
 N1 B1 N3 103.8(3) . . ?
 N1 B1 C30 113.9(3) . . ?
 N2 B1 N3 104.4(2) . . ?
 N2 B1 C30 116.0(3) . . ?
 N3 B1 C30 113.1(3) . . ?

_olex2_submission_special_instructions 'No special instructions were received'
_oxdiff_exptl_absorpt_empirical_details
;
Empirical correction (ABSPACK) includes:
- Absorption correction using spherical harmonics
- Frame scaling
;
_oxdiff_exptl_absorpt_empirical_full_max 2.419
_oxdiff_exptl_absorpt_empirical_full_min 0.420

# SQUEEZE RESULTS (APPEND TO CIF)
# Note: Data are Listed for all Voids in the P1 Unit Cell
# i.e. Centre of Gravity, Solvent Accessible Volume,
# Recovered number of Electrons in the Void and
# Details about the Squeezed Material
loop_
  _platon_squeeze_void_nr
  _platon_squeeze_void_average_x
  _platon_squeeze_void_average_y
  _platon_squeeze_void_average_z
  _platon_squeeze_void_volume
  _platon_squeeze_void_count_electrons
  _platon_squeeze_void_content
   1  0.500  0.500  0.500       597       168 ' '
   2  0.500  0.000  0.000        26         2 ' '
_platon_squeeze_details
;
;
