data_1
_audit_creation_date               2020-01-28
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3510 for OlexSys, GUI svn.r5506)
;
_shelx_SHELXL_version_number       '2018/3'
_audit_contact_author_address      ?
_audit_contact_author_email        ?
_audit_contact_author_name         ''
_audit_contact_author_phone        ?
_publ_contact_author_id_orcid      ?
_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.

Sheldrick, G.M. (2015). Acta Cryst. C71, 3-8.
;
_chemical_name_common              ?
_chemical_name_systematic          ?
_chemical_formula_moiety           'C78 H84 B6 O12, 2(C5 H12)'
_chemical_formula_sum              'C88 H108 B6 O12'
_chemical_formula_weight           1422.60
_chemical_melting_point            ?
_chemical_oxdiff_formula           'C H B O Cl'
loop_
  _atom_type_symbol
  _atom_type_description
  _atom_type_scat_dispersion_real
  _atom_type_scat_dispersion_imag
  _atom_type_scat_source
 'C' 'C' 0.0033 0.0016 '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' 0.0013 0.0007 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
 'O' 'O' 0.0106 0.0060 '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        'cubic'
_space_group_IT_number             205
_space_group_name_H-M_alt          'P a -3'
_space_group_name_Hall             '-P 2ac 2ab 3'
loop_
  _space_group_symop_operation_xyz
 'x, y, z'
 'z, x, y'
 'y, z, x'
 '-y+1/2, -z, x+1/2'
 'z+1/2, -x+1/2, -y'
 '-y, z+1/2, -x+1/2'
 '-z+1/2, -x, y+1/2'
 '-z, x+1/2, -y+1/2'
 'y+1/2, -z+1/2, -x'
 '-x+1/2, -y, z+1/2'
 'x+1/2, -y+1/2, -z'
 '-x, y+1/2, -z+1/2'
 '-x, -y, -z'
 '-z, -x, -y'
 '-y, -z, -x'
 'y-1/2, z, -x-1/2'
 '-z-1/2, x-1/2, y'
 'y, -z-1/2, x-1/2'
 'z-1/2, x, -y-1/2'
 'z, -x-1/2, y-1/2'
 '-y-1/2, z-1/2, x'
 'x-1/2, y, -z-1/2'
 '-x-1/2, y-1/2, z'
 'x, -y-1/2, z-1/2'

_cell_length_a                     19.9143(8)
_cell_length_b                     19.9143(8)
_cell_length_c                     19.9143(8)
_cell_angle_alpha                  90
_cell_angle_beta                   90
_cell_angle_gamma                  90
_cell_volume                       7897.6(10)
_cell_formula_units_Z              4
_cell_measurement_reflns_used      2031
_cell_measurement_temperature      123(2)
_cell_measurement_theta_max        25.7200
_cell_measurement_theta_min        2.0380
_shelx_estimated_absorpt_T_max     ?
_shelx_estimated_absorpt_T_min     ?
_exptl_absorpt_coefficient_mu      0.076
_exptl_absorpt_correction_T_max    1.00000
_exptl_absorpt_correction_T_min    0.89190
_exptl_absorpt_correction_type     multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.40.39a (Rigaku Oxford Diffraction, 2019)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_absorpt_special_details     ?
_exptl_crystal_colour              yellow
_exptl_crystal_colour_primary      yellow
_exptl_crystal_density_diffrn      1.196
_exptl_crystal_density_meas        ?
_exptl_crystal_density_method      ?
_exptl_crystal_description         block
_exptl_crystal_F_000               3048
_exptl_crystal_size_max            0.2
_exptl_crystal_size_mid            0.2
_exptl_crystal_size_min            0.2
_exptl_transmission_factor_max     ?
_exptl_transmission_factor_min     ?
_diffrn_reflns_av_R_equivalents    0.0529
_diffrn_reflns_av_unetI/netI       0.0729
_diffrn_reflns_Laue_measured_fraction_full  0.996
_diffrn_reflns_Laue_measured_fraction_max  0.817
_diffrn_reflns_limit_h_max         23
_diffrn_reflns_limit_h_min         -13
_diffrn_reflns_limit_k_max         18
_diffrn_reflns_limit_k_min         -4
_diffrn_reflns_limit_l_max         16
_diffrn_reflns_limit_l_min         -14
_diffrn_reflns_number              8158
_diffrn_reflns_point_group_measured_fraction_full  0.996
_diffrn_reflns_point_group_measured_fraction_max  0.817
_diffrn_reflns_theta_full          25.000
_diffrn_reflns_theta_max           27.931
_diffrn_reflns_theta_min           2.045
_diffrn_ambient_temperature        123(2)
_diffrn_detector                   'CCD plate'
_diffrn_detector_area_resol_mean   5.8140
_diffrn_detector_type              'Pilatus 200K'
_diffrn_measured_fraction_theta_full  0.996
_diffrn_measured_fraction_theta_max  0.817
_diffrn_measurement_details
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  tₑₓₚ   ω     θ     κ     φ   Frames
--------------------------------------------------------------------------
  1  ω      2.00  56.00   0.50   32.81    --   11.29  36.00 128.00  108
;
_diffrn_measurement_device         'four-circle diffractometer'
_diffrn_measurement_device_type    'ROD, Synergy Custom system, Pilatus 200K'
_diffrn_measurement_method         'ω scans'
_diffrn_measurement_specimen_support  'Mitegen 50um'
_diffrn_orient_matrix_type        
 'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11        -0.0013720000
_diffrn_orient_matrix_UB_12        -0.0105919000
_diffrn_orient_matrix_UB_13        -0.0339679000
_diffrn_orient_matrix_UB_21        -0.0330037000
_diffrn_orient_matrix_UB_22        -0.0123589000
_diffrn_orient_matrix_UB_23        0.0051782000
_diffrn_orient_matrix_UB_31        -0.0133419000
_diffrn_orient_matrix_UB_32        0.0316911000
_diffrn_orient_matrix_UB_33        -0.0093205000
_diffrn_oxdiff_digest_frames
;
0146fe26d4e4d62c60e640b82889a34190000255bce
;
_diffrn_oxdiff_digest_hkl
;
01e82df7ace1101f60aeb6995c9a2510afcec7
;
_diffrn_radiation_monochromator    mirror
_diffrn_radiation_probe            x-ray
_diffrn_radiation_type             MoK\a
_diffrn_radiation_wavelength       0.71073
_diffrn_source                     'Rotating-anode X-ray tube'
_diffrn_source_type                'Rigaku (Mo) X-ray Source'
_reflns_Friedel_coverage           0.000
_reflns_Friedel_fraction_full      .
_reflns_Friedel_fraction_max       .
_reflns_number_gt                  1570
_reflns_number_total               2594
_reflns_odcompleteness_completeness  99.26
_reflns_odcompleteness_iscentric   1
_reflns_odcompleteness_theta       25.01
_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 1.171.40.39a (Rigaku OD, 2019)'
_computing_data_collection         'CrysAlisPro 1.171.40.39a (Rigaku OD, 2019)'
_computing_data_reduction          'CrysAlisPro 1.171.40.39a (Rigaku OD, 2019)'
_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      'ShelXD (Sheldrick, 2008)'
_refine_diff_density_max           0.521
_refine_diff_density_min           -0.309
_refine_diff_density_rms           0.061
_refine_ls_extinction_coef         .
_refine_ls_extinction_method       none
_refine_ls_goodness_of_fit_ref     1.093
_refine_ls_hydrogen_treatment      constr
_refine_ls_matrix_type             full
_refine_ls_number_parameters       194
_refine_ls_number_reflns           2594
_refine_ls_number_restraints       28
_refine_ls_R_factor_all            0.1252
_refine_ls_R_factor_gt             0.0733
_refine_ls_restrained_S_all        1.105
_refine_ls_shift/su_max            0.000
_refine_ls_shift/su_mean           0.000
_refine_ls_structure_factor_coef   Fsqd
_refine_ls_weighting_details      
 'w=1/[σ²(Fo²)+(0.1366P)²+0.3202P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme        calc
_refine_ls_wR_factor_gt            0.2041
_refine_ls_wR_factor_ref           0.2378
_refine_special_details            ?
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Restrained distances
 C14-C15 = C15-C16 = C16-C17 = C17-C18
 1.54 with sigma of 0.02
 C14-C16 = C16-C18 = C15-C17
 2.54 with sigma of 0.02
3. Rigid body (RIGU) restrains
 C14, C15, C16, C17, C18
 with sigma for 1-2 distances of 0.0007 and sigma for 1-3 distances of 0.0007
4. Others
 Fixed Sof: C14(0.33333) H14A(0.33333) H14B(0.33333) H14C(0.33333)
 C15(0.33333) H15A(0.33333) H15B(0.33333) C16(0.33333) H16A(0.33333)
 H16B(0.33333) C17(0.33333) H17A(0.33333) H17B(0.33333) C18(0.33333)
 H18A(0.33333) H18B(0.33333) H18C(0.33333)
5.a Secondary CH2 refined with riding coordinates:
 C15(H15A,H15B), C16(H16A,H16B), C17(H17A,H17B)
5.b Me refined with riding coordinates:
 C14(H14A,H14B,H14C), C18(H18A,H18B,H18C)
5.c Aromatic/amide H refined with riding coordinates:
 C4(H4), C6(H6)
5.d Idealised Me refined as rotating group:
 C10(H10A,H10B,H10C), C11(H11A,H11B,H11C), C12(H12A,H12B,H12C), C13(H13A,H13B,
 H13C)
;
_atom_sites_solution_hydrogens     geom
_atom_sites_solution_primary       ?
_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
 C1 C 0.44320(13) 0.98160(13) 0.03851(13) 0.0219(6) Uani 1 1 d . . . . .
 C2 C 0.38420(13) 0.96393(13) 0.07678(12) 0.0211(6) Uani 1 1 d . . . . .
 C3 C 0.36401(13) 1.00335(13) 0.13251(13) 0.0225(7) Uani 1 1 d . . . . .
 C4 C 0.30175(14) 0.99141(14) 0.16213(13) 0.0275(7) Uani 1 1 d . . . . .
 H4 H 0.287980 1.018625 0.198812 0.033 Uiso 1 1 calc R . . . .
 C5 C 0.25920(13) 0.94090(14) 0.13965(14) 0.0269(7) Uani 1 1 d . . . . .
 C6 C 0.28185(13) 0.89897(13) 0.08852(13) 0.0260(7) Uani 1 1 d . . . . .
 H6 H 0.254233 0.862696 0.074461 0.031 Uiso 1 1 calc R . . . .
 C7 C 0.34365(13) 0.90850(13) 0.05733(13) 0.0235(7) Uani 1 1 d . . . . .
 B1 B 0.18657(17) 0.93421(16) 0.16732(16) 0.0288(8) Uani 1 1 d . . . . .
 O1 O 0.16083(10) 0.97340(10) 0.21657(11) 0.0379(6) Uani 1 1 d . . . . .
 C8 C 0.08849(15) 0.96123(17) 0.21899(17) 0.0427(9) Uani 1 1 d . . . . .
 C9 C 0.08297(15) 0.88990(17) 0.18728(16) 0.0419(9) Uani 1 1 d . . . . .
 O2 O 0.14158(10) 0.88895(10) 0.14243(10) 0.0373(6) Uani 1 1 d . . . . .
 C10 C 0.05521(18) 1.0145(2) 0.1761(2) 0.0637(12) Uani 1 1 d . . . . .
 H10A H 0.068432 1.059118 0.192156 0.096 Uiso 1 1 calc GR . . . .
 H10B H 0.006314 1.009828 0.179123 0.096 Uiso 1 1 calc GR . . . .
 H10C H 0.069346 1.009080 0.129281 0.096 Uiso 1 1 calc GR . . . .
 C11 C 0.06551(17) 0.9643(2) 0.29181(19) 0.0604(11) Uani 1 1 d . . . . .
 H11A H 0.092408 0.933165 0.318821 0.091 Uiso 1 1 calc GR . . . .
 H11B H 0.018041 0.951589 0.294572 0.091 Uiso 1 1 calc GR . . . .
 H11C H 0.071267 1.010061 0.308922 0.091 Uiso 1 1 calc GR . . . .
 C12 C 0.02088(17) 0.8772(2) 0.1459(2) 0.0615(11) Uani 1 1 d . . . . .
 H12A H 0.017640 0.911129 0.110374 0.092 Uiso 1 1 calc GR . . . .
 H12B H -0.018893 0.879859 0.174759 0.092 Uiso 1 1 calc GR . . . .
 H12C H 0.023514 0.832452 0.125646 0.092 Uiso 1 1 calc GR . . . .
 C13 C 0.09320(18) 0.83412(17) 0.23570(19) 0.0537(10) Uani 1 1 d . . . . .
 H13A H 0.098257 0.791782 0.211120 0.081 Uiso 1 1 calc GR . . . .
 H13B H 0.054321 0.831113 0.265715 0.081 Uiso 1 1 calc GR . . . .
 H13C H 0.133774 0.842638 0.262210 0.081 Uiso 1 1 calc GR . . . .
 C14 C 0.1889(6) 0.7115(6) 0.1109(6) 0.059(3) Uani 0.3333 1 d D U P A -1
 H14A H 0.169693 0.674943 0.084141 0.089 Uiso 0.3333 1 calc R . P A -1
 H14B H 0.155981 0.726334 0.144381 0.089 Uiso 0.3333 1 calc R . P A -1
 H14C H 0.200332 0.749183 0.081382 0.089 Uiso 0.3333 1 calc R . P A -1
 C15 C 0.2495(10) 0.6878(10) 0.1449(9) 0.093(6) Uani 0.3333 1 d D U P A -1
 H15A H 0.280756 0.671287 0.110025 0.112 Uiso 0.3333 1 calc R . P A -1
 H15B H 0.236646 0.648563 0.172684 0.112 Uiso 0.3333 1 calc R . P A -1
 C16 C 0.2890(11) 0.7368(8) 0.1905(9) 0.139(7) Uani 0.3333 1 d D U P A -1
 H16A H 0.271605 0.783097 0.185312 0.166 Uiso 0.3333 1 calc R . P A -1
 H16B H 0.337207 0.736532 0.178528 0.166 Uiso 0.3333 1 calc R . P A -1
 C17 C 0.2791(10) 0.7121(7) 0.2646(7) 0.102(5) Uani 0.3333 1 d D U P A -1
 H17A H 0.304480 0.742139 0.294981 0.122 Uiso 0.3333 1 calc R . P A -1
 H17B H 0.230934 0.715981 0.276414 0.122 Uiso 0.3333 1 calc R . P A -1
 C18 C 0.3012(8) 0.6410(7) 0.2769(7) 0.072(4) Uani 0.3333 1 d D U P A -1
 H18A H 0.293499 0.629336 0.324030 0.108 Uiso 0.3333 1 calc R . P A -1
 H18B H 0.275521 0.610618 0.247976 0.108 Uiso 0.3333 1 calc R . P A -1
 H18C H 0.349180 0.636817 0.266571 0.108 Uiso 0.3333 1 calc R . P A -1


_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
 C1 C1 1.415(2) 17_664 ?
 C1 C1 1.415(2) 16_566 ?
 C1 C2 1.444(3) . ?
 C2 C3 1.418(4) . ?
 C2 C7 1.422(4) . ?
 C3 C4 1.394(4) . ?
 C3 C7 1.472(4) 16_566 ?
 C4 C5 1.389(4) . ?
 C5 C6 1.392(4) . ?
 C5 B1 1.554(4) . ?
 C6 C7 1.391(4) . ?
 B1 O1 1.354(4) . ?
 B1 O2 1.364(4) . ?
 O1 C8 1.462(4) . ?
 C8 C9 1.558(5) . ?
 C8 C10 1.515(5) . ?
 C8 C11 1.522(5) . ?
 C9 O2 1.470(4) . ?
 C9 C12 1.507(5) . ?
 C9 C13 1.485(5) . ?
 C14 C15 1.462(15) . ?
 C15 C16 1.548(16) . ?
 C16 C17 1.568(14) . ?
 C17 C18 1.502(15) . ?

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
 C1 C1 C1 120.004(2) 17_664 16_566 ?
 C1 C1 C2 119.9(2) 16_566 . ?
 C1 C1 C2 120.0(2) 17_664 . ?
 C3 C2 C1 120.6(2) . . ?
 C3 C2 C7 118.8(2) . . ?
 C7 C2 C1 120.5(2) . . ?
 C2 C3 C7 119.1(2) . 16_566 ?
 C4 C3 C2 119.3(2) . . ?
 C4 C3 C7 121.6(2) . 16_566 ?
 C5 C4 C3 122.0(3) . . ?
 C4 C5 C6 118.2(3) . . ?
 C4 C5 B1 121.0(2) . . ?
 C6 C5 B1 120.6(2) . . ?
 C7 C6 C5 122.1(2) . . ?
 C2 C7 C3 118.9(2) . 17_664 ?
 C6 C7 C2 119.1(2) . . ?
 C6 C7 C3 122.0(2) . 17_664 ?
 O1 B1 C5 124.0(3) . . ?
 O1 B1 O2 113.3(3) . . ?
 O2 B1 C5 122.6(3) . . ?
 B1 O1 C8 107.5(2) . . ?
 O1 C8 C9 102.0(2) . . ?
 O1 C8 C10 107.2(3) . . ?
 O1 C8 C11 108.7(3) . . ?
 C10 C8 C9 112.3(3) . . ?
 C10 C8 C11 112.2(3) . . ?
 C11 C8 C9 113.7(3) . . ?
 O2 C9 C8 101.7(2) . . ?
 O2 C9 C12 108.5(3) . . ?
 O2 C9 C13 106.0(3) . . ?
 C12 C9 C8 115.6(3) . . ?
 C13 C9 C8 114.1(3) . . ?
 C13 C9 C12 110.0(3) . . ?
 B1 O2 C9 107.0(2) . . ?
 C14 C15 C16 119.2(15) . . ?
 C15 C16 C17 106.8(12) . . ?
 C18 C17 C16 114.3(12) . . ?

_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  1.069
_oxdiff_exptl_absorpt_empirical_full_min  0.905
