 
data_23051z
 
_audit_creation_method            'SHELXL-2018/3'
_shelx_SHELXL_version_number      '2018/3'
_chemical_name_systematic         ?
_chemical_name_common             23051z
_chemical_melting_point           ?
_chemical_formula_moiety          '2(C30 H16 N2 O4), C H2 Cl2'
_chemical_formula_sum             'C61 H34 Cl2 N4 O8' 
_chemical_formula_weight          1021.82

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'
 'Cl'  'Cl'   0.1484   0.1585
 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
 'N'  'N'   0.0061   0.0033
 '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'
 
_space_group_crystal_system       orthorhombic
_space_group_IT_number            61
_space_group_name_H-M_alt         'P b c a'
_space_group_name_Hall            '-P 2ac 2ab'
 
_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.
;
 
loop_
 _space_group_symop_operation_xyz
 'x, y, z'
 '-x+1/2, -y, z+1/2'
 '-x, y+1/2, -z+1/2'
 'x+1/2, -y+1/2, -z'
 '-x, -y, -z'
 'x-1/2, y, -z-1/2'
 'x, -y-1/2, z-1/2'
 '-x-1/2, y-1/2, z'
 
_cell_length_a                    12.8560(9)
_cell_length_b                    13.2882(10)
_cell_length_c                    54.898(4)
_cell_angle_alpha                 90
_cell_angle_beta                  90
_cell_angle_gamma                 90
_cell_volume                      9378.3(12)
_cell_formula_units_Z             8
_cell_measurement_temperature     130(2)
_cell_measurement_reflns_used     2995
_cell_measurement_theta_min       2.23
_cell_measurement_theta_max       25.71

_exptl_crystal_description       'needle'
_exptl_crystal_colour            'red'
_exptl_crystal_density_meas       ?
_exptl_crystal_density_method     ?
_exptl_crystal_density_diffrn     1.447          
_exptl_crystal_F_000              4208
_exptl_transmission_factor_min    0.6212
_exptl_transmission_factor_max    0.7454
_exptl_crystal_size_max           0.230
_exptl_crystal_size_mid           0.060
_exptl_crystal_size_min           0.035
_exptl_absorpt_coefficient_mu     0.206
_shelx_estimated_absorpt_T_min    0.954
_shelx_estimated_absorpt_T_max    0.993
_exptl_absorpt_correction_type    multi-scan
_exptl_absorpt_correction_T_min   0.6212
_exptl_absorpt_correction_T_max   0.7454
_exptl_absorpt_process_details    'SADABS-2016/2, (Sheldrick, 2016)'
_exptl_absorpt_special_details    ?
_exptl_special_details            'Prof. D. Cao - Macalester College'
_diffrn_ambient_temperature       130(2)
_diffrn_radiation_wavelength      0.71073
_diffrn_radiation_type            MoK\a
_diffrn_source                    'micro-focus'
_diffrn_measurement_device_type   'Bruker PHOTON-III CPAD'
_diffrn_measurement_method        'φ and ω scans'
_diffrn_detector_area_resol_mean  ?
_diffrn_reflns_number             63324
_diffrn_reflns_av_unetI/netI      0.0495
_diffrn_reflns_av_R_equivalents   0.0661
_diffrn_reflns_limit_h_min        -11
_diffrn_reflns_limit_h_max        15
_diffrn_reflns_limit_k_min        -15
_diffrn_reflns_limit_k_max        16
_diffrn_reflns_limit_l_min        -53
_diffrn_reflns_limit_l_max        68
_diffrn_reflns_theta_min          2.226
_diffrn_reflns_theta_max          26.231
_diffrn_reflns_theta_full         25.242
_diffrn_measured_fraction_theta_max   0.996
_diffrn_measured_fraction_theta_full  0.998
_diffrn_reflns_Laue_measured_fraction_max    0.996
_diffrn_reflns_Laue_measured_fraction_full   0.998
_diffrn_reflns_point_group_measured_fraction_max   0.996
_diffrn_reflns_point_group_measured_fraction_full  0.998
_reflns_number_total              9387
_reflns_number_gt                 6975
_reflns_threshold_expression      'I > 2σ(I)'
_reflns_Friedel_coverage          0.000
_reflns_Friedel_fraction_max      .
_reflns_Friedel_fraction_full     .
 
_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.
;
 
_computing_data_collection       'Bruker APEX4'
_computing_cell_refinement       'Bruker SAINT'
_computing_data_reduction        'Bruker SAINT'
_computing_structure_solution    'SHELXT-2018/2 (Sheldrick, 2018)'
_computing_structure_refinement  'SHELXL-2018/3 (Sheldrick, 2018)'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_refine_special_details           ?
_refine_ls_structure_factor_coef  Fsqd
_refine_ls_matrix_type            full
_refine_ls_weighting_scheme       calc
_refine_ls_weighting_details
'w=1/[σ²(Fo²)+(0.0609P)²+13.8679P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary      ?
_atom_sites_solution_secondary    ?
_atom_sites_solution_hydrogens    geom
_refine_ls_hydrogen_treatment     constr
_refine_ls_extinction_method      none
_refine_ls_extinction_coef        .
_refine_ls_number_reflns          9387
_refine_ls_number_parameters      676
_refine_ls_number_restraints      0
_refine_ls_R_factor_all           0.0914
_refine_ls_R_factor_gt            0.0631
_refine_ls_wR_factor_ref          0.1577
_refine_ls_wR_factor_gt           0.1457
_refine_ls_goodness_of_fit_ref    1.076
_refine_ls_restrained_S_all       1.076
_refine_ls_shift/su_max           0.001
_refine_ls_shift/su_mean          0.000
 
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
O1A O 0.76856(15) 0.39498(16) 0.42886(3) 0.0250(5) Uani 1 1 d . . . . .
O2A O 0.47548(14) 0.38773(15) 0.38139(3) 0.0210(4) Uani 1 1 d . . . . .
O3A O 0.49638(15) 0.41970(15) 0.32639(3) 0.0231(4) Uani 1 1 d . . . . .
O4A O 0.82257(16) 0.43383(19) 0.29311(4) 0.0348(6) Uani 1 1 d . . . . .
N1A N 0.60582(17) 0.39331(17) 0.41074(4) 0.0182(5) Uani 1 1 d . . . . .
N2A N 0.64889(17) 0.43207(19) 0.30382(4) 0.0209(5) Uani 1 1 d . . . . .
C1A C 0.7145(2) 0.3936(2) 0.41087(5) 0.0181(6) Uani 1 1 d . . . . .
C2A C 0.7477(2) 0.39509(19) 0.38468(5) 0.0155(5) Uani 1 1 d . . . . .
C3A C 0.6592(2) 0.39768(19) 0.37064(5) 0.0148(5) Uani 1 1 d . . . . .
C4A C 0.5660(2) 0.3928(2) 0.38669(5) 0.0161(6) Uani 1 1 d . . . . .
C5A C 0.5899(2) 0.4191(2) 0.32536(5) 0.0182(6) Uani 1 1 d . . . . .
C6A C 0.6692(2) 0.40699(19) 0.34505(5) 0.0159(6) Uani 1 1 d . . . . .
C7A C 0.7672(2) 0.4121(2) 0.33528(5) 0.0174(6) Uani 1 1 d . . . . .
C8A C 0.7558(2) 0.4272(2) 0.30834(5) 0.0213(6) Uani 1 1 d . . . . .
C9A C 0.8506(2) 0.3987(2) 0.37519(5) 0.0161(6) Uani 1 1 d . . . . .
C10A C 0.9403(2) 0.3949(2) 0.38950(5) 0.0184(6) Uani 1 1 d . . . . .
H10A H 0.933793 0.387452 0.406646 0.022 Uiso 1 1 calc R U . . .
C11A C 1.0391(2) 0.4016(2) 0.37919(5) 0.0188(6) Uani 1 1 d . . . . .
C12A C 1.1310(2) 0.3995(2) 0.39366(5) 0.0225(6) Uani 1 1 d . . . . .
H12A H 1.125495 0.391273 0.410803 0.027 Uiso 1 1 calc R U . . .
C13A C 1.2265(2) 0.4090(2) 0.38333(6) 0.0257(7) Uani 1 1 d . . . . .
H13A H 1.286865 0.407682 0.393305 0.031 Uiso 1 1 calc R U . . .
C14A C 1.2369(2) 0.4208(2) 0.35766(6) 0.0249(7) Uani 1 1 d . . . . .
H14A H 1.304062 0.428083 0.350672 0.030 Uiso 1 1 calc R U . . .
C15A C 1.1514(2) 0.4218(2) 0.34307(5) 0.0234(6) Uani 1 1 d . . . . .
H15A H 1.159555 0.428651 0.325951 0.028 Uiso 1 1 calc R U . . .
C16A C 1.0493(2) 0.4125(2) 0.35317(5) 0.0191(6) Uani 1 1 d . . . . .
C17A C 0.9601(2) 0.4153(2) 0.33867(5) 0.0183(6) Uani 1 1 d . . . . .
H17A H 0.967031 0.422049 0.321517 0.022 Uiso 1 1 calc R U . . .
C18A C 0.8609(2) 0.4084(2) 0.34893(5) 0.0164(6) Uani 1 1 d . . . . .
C19A C 0.5425(2) 0.3963(2) 0.43221(5) 0.0188(6) Uani 1 1 d . . . . .
C20A C 0.5674(2) 0.3365(2) 0.45191(5) 0.0271(7) Uani 1 1 d . . . . .
H20A H 0.625400 0.292302 0.451164 0.032 Uiso 1 1 calc R U . . .
C21A C 0.5070(3) 0.3414(3) 0.47282(6) 0.0371(8) Uani 1 1 d . . . . .
H21A H 0.523580 0.300172 0.486408 0.044 Uiso 1 1 calc R U . . .
C22A C 0.4230(3) 0.4057(3) 0.47400(6) 0.0391(9) Uani 1 1 d . . . . .
H22A H 0.382634 0.409508 0.488470 0.047 Uiso 1 1 calc R U . . .
C23A C 0.3975(3) 0.4644(3) 0.45422(6) 0.0327(8) Uani 1 1 d . . . . .
H23A H 0.338687 0.507571 0.454974 0.039 Uiso 1 1 calc R U . . .
C24A C 0.4575(2) 0.4608(2) 0.43309(5) 0.0237(6) Uani 1 1 d . . . . .
H24A H 0.440492 0.501803 0.419482 0.028 Uiso 1 1 calc R U . . .
C25A C 0.6053(2) 0.4553(2) 0.28045(5) 0.0205(6) Uani 1 1 d . . . . .
C26A C 0.6422(2) 0.5384(2) 0.26776(5) 0.0270(7) Uani 1 1 d . . . . .
H26A H 0.696613 0.578259 0.274385 0.032 Uiso 1 1 calc R U . . .
C27A C 0.5994(2) 0.5627(2) 0.24541(5) 0.0298(7) Uani 1 1 d . . . . .
H27A H 0.624538 0.619091 0.236574 0.036 Uiso 1 1 calc R U . . .
C28A C 0.5194(2) 0.5043(3) 0.23594(5) 0.0283(7) Uani 1 1 d . . . . .
H28A H 0.488923 0.521722 0.220747 0.034 Uiso 1 1 calc R U . . .
C29A C 0.4839(2) 0.4207(2) 0.24861(5) 0.0273(7) Uani 1 1 d . . . . .
H29A H 0.429689 0.380569 0.241973 0.033 Uiso 1 1 calc R U . . .
C30A C 0.5272(2) 0.3956(2) 0.27091(5) 0.0228(6) Uani 1 1 d . . . . .
H30A H 0.503547 0.338052 0.279548 0.027 Uiso 1 1 calc R U . . .
O1B O 0.49109(15) 0.18676(16) 0.31119(3) 0.0256(5) Uani 1 1 d . . . . .
O2B O 0.20686(15) 0.17058(15) 0.36126(3) 0.0239(5) Uani 1 1 d . . . . .
O3B O 0.24053(15) 0.14260(17) 0.41689(4) 0.0280(5) Uani 1 1 d . . . . .
O4B O 0.57303(15) 0.09469(17) 0.44482(4) 0.0285(5) Uani 1 1 d . . . . .
N1B N 0.33283(18) 0.18727(18) 0.33127(4) 0.0205(5) Uani 1 1 d . . . . .
N2B N 0.39712(18) 0.11554(19) 0.43688(4) 0.0241(6) Uani 1 1 d . . . . .
C1B C 0.4409(2) 0.1822(2) 0.32987(5) 0.0202(6) Uani 1 1 d . . . . .
C2B C 0.4780(2) 0.1679(2) 0.35545(5) 0.0170(6) Uani 1 1 d . . . . .
C3B C 0.3933(2) 0.1639(2) 0.37054(5) 0.0169(6) Uani 1 1 d . . . . .
C4B C 0.2963(2) 0.1738(2) 0.35545(5) 0.0183(6) Uani 1 1 d . . . . .
C5B C 0.3336(2) 0.1369(2) 0.41652(5) 0.0206(6) Uani 1 1 d . . . . .
C6B C 0.4090(2) 0.1484(2) 0.39569(5) 0.0184(6) Uani 1 1 d . . . . .
C7B C 0.5079(2) 0.1385(2) 0.40435(5) 0.0180(6) Uani 1 1 d . . . . .
C8B C 0.5029(2) 0.1138(2) 0.43091(5) 0.0219(6) Uani 1 1 d . . . . .
C9B C 0.5830(2) 0.1587(2) 0.36358(5) 0.0181(6) Uani 1 1 d . . . . .
C10B C 0.6693(2) 0.1620(2) 0.34808(5) 0.0180(6) Uani 1 1 d . . . . .
H10B H 0.659101 0.169189 0.331030 0.022 Uiso 1 1 calc R U . . .
C11B C 0.7701(2) 0.1547(2) 0.35733(5) 0.0201(6) Uani 1 1 d . . . . .
C12B C 0.8596(2) 0.1584(2) 0.34183(5) 0.0224(6) Uani 1 1 d . . . . .
H12B H 0.850673 0.164915 0.324731 0.027 Uiso 1 1 calc R U . . .
C13B C 0.9572(2) 0.1526(2) 0.35126(6) 0.0261(7) Uani 1 1 d . . . . .
H13B H 1.015599 0.155365 0.340690 0.031 Uiso 1 1 calc R U . . .
C14B C 0.9726(2) 0.1423(2) 0.37684(6) 0.0258(7) Uani 1 1 d . . . . .
H14B H 1.041233 0.138589 0.383218 0.031 Uiso 1 1 calc R U . . .
C15B C 0.8898(2) 0.1379(2) 0.39215(6) 0.0229(6) Uani 1 1 d . . . . .
H15B H 0.901080 0.131039 0.409172 0.027 Uiso 1 1 calc R U . . .
C16B C 0.7860(2) 0.1435(2) 0.38307(5) 0.0197(6) Uani 1 1 d . . . . .
C17B C 0.6999(2) 0.1383(2) 0.39861(5) 0.0194(6) Uani 1 1 d . . . . .
H17B H 0.710446 0.129969 0.415620 0.023 Uiso 1 1 calc R U . . .
C18B C 0.5987(2) 0.1450(2) 0.38951(5) 0.0180(6) Uani 1 1 d . . . . .
C19B C 0.2665(2) 0.1968(2) 0.31038(5) 0.0203(6) Uani 1 1 d . . . . .
C20B C 0.2781(2) 0.2795(2) 0.29521(5) 0.0252(7) Uani 1 1 d . . . . .
H20B H 0.327582 0.330375 0.298907 0.030 Uiso 1 1 calc R U . . .
C21B C 0.2161(3) 0.2870(3) 0.27444(6) 0.0339(8) Uani 1 1 d . . . . .
H21B H 0.223471 0.342863 0.263790 0.041 Uiso 1 1 calc R U . . .
C22B C 0.1437(3) 0.2127(3) 0.26937(6) 0.0359(8) Uani 1 1 d . . . . .
H22B H 0.102291 0.217235 0.255083 0.043 Uiso 1 1 calc R U . . .
C23B C 0.1315(3) 0.1320(3) 0.28500(6) 0.0342(8) Uani 1 1 d . . . . .
H23B H 0.080373 0.082299 0.281615 0.041 Uiso 1 1 calc R U . . .
C24B C 0.1933(2) 0.1230(2) 0.30552(5) 0.0268(7) Uani 1 1 d . . . . .
H24B H 0.185576 0.066988 0.316132 0.032 Uiso 1 1 calc R U . . .
C25B C 0.3584(2) 0.0968(2) 0.46100(5) 0.0256(7) Uani 1 1 d . . . . .
C26B C 0.3873(2) 0.0106(3) 0.47319(6) 0.0332(8) Uani 1 1 d . . . . .
H26B H 0.432490 -0.036680 0.465656 0.040 Uiso 1 1 calc R U . . .
C27B C 0.3499(3) -0.0068(3) 0.49664(6) 0.0427(9) Uani 1 1 d . . . . .
H27B H 0.370300 -0.065481 0.505294 0.051 Uiso 1 1 calc R U . . .
C28B C 0.2828(3) 0.0617(3) 0.50724(6) 0.0448(10) Uani 1 1 d . . . . .
H28B H 0.256507 0.049719 0.523145 0.054 Uiso 1 1 calc R U . . .
C29B C 0.2539(3) 0.1475(3) 0.49482(6) 0.0421(9) Uani 1 1 d . . . . .
H29B H 0.207080 0.193778 0.502147 0.051 Uiso 1 1 calc R U . . .
C30B C 0.2927(2) 0.1667(3) 0.47171(6) 0.0313(7) Uani 1 1 d . . . . .
H30B H 0.274435 0.226760 0.463353 0.038 Uiso 1 1 calc R U . . .
C1S C 0.9222(3) 0.2628(3) 0.46222(7) 0.0485(10) Uani 1 1 d . . . . .
H1SA H 0.889997 0.321588 0.454080 0.058 Uiso 1 1 calc R U . . .
H1SB H 0.934774 0.281107 0.479453 0.058 Uiso 1 1 calc R U . . .
Cl1S Cl 1.04103(8) 0.23597(8) 0.44821(2) 0.0558(3) Uani 1 1 d . . . . .
Cl2S Cl 0.83483(9) 0.16009(9) 0.46107(2) 0.0591(3) 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
O1A C1A 1.208(3) . ?
O2A C4A 1.201(3) . ?
O3A C5A 1.204(3) . ?
O4A C8A 1.201(3) . ?
N1A C1A 1.398(3) . ?
N1A C4A 1.416(3) . ?
N1A C19A 1.434(3) . ?
N2A C8A 1.399(4) . ?
N2A C5A 1.415(3) . ?
N2A C25A 1.433(3) . ?
C1A C2A 1.500(4) . ?
C2A C3A 1.375(4) . ?
C2A C9A 1.423(4) . ?
C3A C6A 1.416(4) . ?
C3A C4A 1.489(4) . ?
C5A C6A 1.494(4) . ?
C6A C7A 1.371(4) . ?
C7A C18A 1.419(4) . ?
C7A C8A 1.500(4) . ?
C9A C10A 1.396(4) . ?
C9A C18A 1.453(4) . ?
C10A C11A 1.393(4) . ?
C10A H10A 0.9500 . ?
C11A C12A 1.425(4) . ?
C11A C16A 1.442(4) . ?
C12A C13A 1.358(4) . ?
C12A H12A 0.9500 . ?
C13A C14A 1.424(4) . ?
C13A H13A 0.9500 . ?
C14A C15A 1.360(4) . ?
C14A H14A 0.9500 . ?
C15A C16A 1.430(4) . ?
C15A H15A 0.9500 . ?
C16A C17A 1.396(4) . ?
C17A C18A 1.398(4) . ?
C17A H17A 0.9500 . ?
C19A C20A 1.380(4) . ?
C19A C24A 1.389(4) . ?
C20A C21A 1.387(4) . ?
C20A H20A 0.9500 . ?
C21A C22A 1.379(5) . ?
C21A H21A 0.9500 . ?
C22A C23A 1.376(5) . ?
C22A H22A 0.9500 . ?
C23A C24A 1.394(4) . ?
C23A H23A 0.9500 . ?
C24A H24A 0.9500 . ?
C25A C30A 1.382(4) . ?
C25A C26A 1.390(4) . ?
C26A C27A 1.383(4) . ?
C26A H26A 0.9500 . ?
C27A C28A 1.388(4) . ?
C27A H27A 0.9500 . ?
C28A C29A 1.388(4) . ?
C28A H28A 0.9500 . ?
C29A C30A 1.386(4) . ?
C29A H29A 0.9500 . ?
C30A H30A 0.9500 . ?
O1B C1B 1.213(3) . ?
O2B C4B 1.194(3) . ?
O3B C5B 1.199(3) . ?
O4B C8B 1.208(3) . ?
N1B C1B 1.393(4) . ?
N1B C4B 1.419(3) . ?
N1B C19B 1.435(3) . ?
N2B C8B 1.399(4) . ?
N2B C5B 1.413(4) . ?
N2B C25B 1.436(4) . ?
C1B C2B 1.495(4) . ?
C2B C3B 1.369(4) . ?
C2B C9B 1.426(4) . ?
C3B C6B 1.411(4) . ?
C3B C4B 1.503(4) . ?
C5B C6B 1.507(4) . ?
C6B C7B 1.363(4) . ?
C7B C18B 1.427(4) . ?
C7B C8B 1.496(4) . ?
C9B C10B 1.399(4) . ?
C9B C18B 1.449(4) . ?
C10B C11B 1.396(4) . ?
C10B H10B 0.9500 . ?
C11B C12B 1.432(4) . ?
C11B C16B 1.435(4) . ?
C12B C13B 1.359(4) . ?
C12B H12B 0.9500 . ?
C13B C14B 1.425(4) . ?
C13B H13B 0.9500 . ?
C14B C15B 1.359(4) . ?
C14B H14B 0.9500 . ?
C15B C16B 1.426(4) . ?
C15B H15B 0.9500 . ?
C16B C17B 1.399(4) . ?
C17B C18B 1.396(4) . ?
C17B H17B 0.9500 . ?
C19B C24B 1.386(4) . ?
C19B C20B 1.387(4) . ?
C20B C21B 1.395(4) . ?
C20B H20B 0.9500 . ?
C21B C22B 1.384(5) . ?
C21B H21B 0.9500 . ?
C22B C23B 1.383(5) . ?
C22B H22B 0.9500 . ?
C23B C24B 1.383(4) . ?
C23B H23B 0.9500 . ?
C24B H24B 0.9500 . ?
C25B C26B 1.378(5) . ?
C25B C30B 1.386(4) . ?
C26B C27B 1.394(4) . ?
C26B H26B 0.9500 . ?
C27B C28B 1.383(6) . ?
C27B H27B 0.9500 . ?
C28B C29B 1.379(6) . ?
C28B H28B 0.9500 . ?
C29B C30B 1.386(4) . ?
C29B H29B 0.9500 . ?
C30B H30B 0.9500 . ?
C1S Cl1S 1.748(4) . ?
C1S Cl2S 1.769(4) . ?
C1S H1SA 0.9900 . ?
C1S H1SB 0.9900 . ?
 
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
C1A N1A C4A 111.5(2) . . ?
C1A N1A C19A 124.3(2) . . ?
C4A N1A C19A 124.1(2) . . ?
C8A N2A C5A 111.9(2) . . ?
C8A N2A C25A 123.6(2) . . ?
C5A N2A C25A 124.4(2) . . ?
O1A C1A N1A 125.4(2) . . ?
O1A C1A C2A 128.4(2) . . ?
N1A C1A C2A 106.2(2) . . ?
C3A C2A C9A 124.3(2) . . ?
C3A C2A C1A 107.6(2) . . ?
C9A C2A C1A 128.0(2) . . ?
C2A C3A C6A 118.9(2) . . ?
C2A C3A C4A 109.5(2) . . ?
C6A C3A C4A 131.6(2) . . ?
O2A C4A N1A 125.2(2) . . ?
O2A C4A C3A 129.7(2) . . ?
N1A C4A C3A 105.1(2) . . ?
O3A C5A N2A 125.0(2) . . ?
O3A C5A C6A 130.4(2) . . ?
N2A C5A C6A 104.6(2) . . ?
C7A C6A C3A 118.4(2) . . ?
C7A C6A C5A 109.8(2) . . ?
C3A C6A C5A 131.7(2) . . ?
C6A C7A C18A 124.9(2) . . ?
C6A C7A C8A 107.6(2) . . ?
C18A C7A C8A 127.4(2) . . ?
O4A C8A N2A 125.1(3) . . ?
O4A C8A C7A 128.8(3) . . ?
N2A C8A C7A 106.1(2) . . ?
C10A C9A C2A 124.1(2) . . ?
C10A C9A C18A 119.1(2) . . ?
C2A C9A C18A 116.8(2) . . ?
C11A C10A C9A 121.4(2) . . ?
C11A C10A H10A 119.3 . . ?
C9A C10A H10A 119.3 . . ?
C10A C11A C12A 121.9(3) . . ?
C10A C11A C16A 119.5(2) . . ?
C12A C11A C16A 118.6(2) . . ?
C13A C12A C11A 121.0(3) . . ?
C13A C12A H12A 119.5 . . ?
C11A C12A H12A 119.5 . . ?
C12A C13A C14A 120.5(3) . . ?
C12A C13A H13A 119.7 . . ?
C14A C13A H13A 119.7 . . ?
C15A C14A C13A 120.5(3) . . ?
C15A C14A H14A 119.7 . . ?
C13A C14A H14A 119.7 . . ?
C14A C15A C16A 120.8(3) . . ?
C14A C15A H15A 119.6 . . ?
C16A C15A H15A 119.6 . . ?
C17A C16A C15A 122.0(3) . . ?
C17A C16A C11A 119.5(2) . . ?
C15A C16A C11A 118.4(2) . . ?
C16A C17A C18A 121.2(2) . . ?
C16A C17A H17A 119.4 . . ?
C18A C17A H17A 119.4 . . ?
C17A C18A C7A 124.0(2) . . ?
C17A C18A C9A 119.2(2) . . ?
C7A C18A C9A 116.7(2) . . ?
C20A C19A C24A 120.7(3) . . ?
C20A C19A N1A 119.8(3) . . ?
C24A C19A N1A 119.5(2) . . ?
C19A C20A C21A 119.4(3) . . ?
C19A C20A H20A 120.3 . . ?
C21A C20A H20A 120.3 . . ?
C22A C21A C20A 120.4(3) . . ?
C22A C21A H21A 119.8 . . ?
C20A C21A H21A 119.8 . . ?
C23A C22A C21A 120.0(3) . . ?
C23A C22A H22A 120.0 . . ?
C21A C22A H22A 120.0 . . ?
C22A C23A C24A 120.4(3) . . ?
C22A C23A H23A 119.8 . . ?
C24A C23A H23A 119.8 . . ?
C19A C24A C23A 119.0(3) . . ?
C19A C24A H24A 120.5 . . ?
C23A C24A H24A 120.5 . . ?
C30A C25A C26A 120.9(3) . . ?
C30A C25A N2A 120.0(3) . . ?
C26A C25A N2A 119.1(3) . . ?
C27A C26A C25A 119.6(3) . . ?
C27A C26A H26A 120.2 . . ?
C25A C26A H26A 120.2 . . ?
C26A C27A C28A 119.8(3) . . ?
C26A C27A H27A 120.1 . . ?
C28A C27A H27A 120.1 . . ?
C27A C28A C29A 120.2(3) . . ?
C27A C28A H28A 119.9 . . ?
C29A C28A H28A 119.9 . . ?
C30A C29A C28A 120.2(3) . . ?
C30A C29A H29A 119.9 . . ?
C28A C29A H29A 119.9 . . ?
C25A C30A C29A 119.3(3) . . ?
C25A C30A H30A 120.4 . . ?
C29A C30A H30A 120.4 . . ?
C1B N1B C4B 112.0(2) . . ?
C1B N1B C19B 123.6(2) . . ?
C4B N1B C19B 124.2(2) . . ?
C8B N2B C5B 112.3(2) . . ?
C8B N2B C25B 123.4(2) . . ?
C5B N2B C25B 124.3(2) . . ?
O1B C1B N1B 125.1(3) . . ?
O1B C1B C2B 129.1(3) . . ?
N1B C1B C2B 105.8(2) . . ?
C3B C2B C9B 124.0(2) . . ?
C3B C2B C1B 108.6(2) . . ?
C9B C2B C1B 127.3(2) . . ?
C2B C3B C6B 118.9(2) . . ?
C2B C3B C4B 108.8(2) . . ?
C6B C3B C4B 132.2(2) . . ?
O2B C4B N1B 124.9(3) . . ?
O2B C4B C3B 130.4(3) . . ?
N1B C4B C3B 104.6(2) . . ?
O3B C5B N2B 125.2(3) . . ?
O3B C5B C6B 130.5(3) . . ?
N2B C5B C6B 104.4(2) . . ?
C7B C6B C3B 119.3(2) . . ?
C7B C6B C5B 109.0(2) . . ?
C3B C6B C5B 131.7(2) . . ?
C6B C7B C18B 123.9(2) . . ?
C6B C7B C8B 108.8(2) . . ?
C18B C7B C8B 127.2(2) . . ?
O4B C8B N2B 125.5(3) . . ?
O4B C8B C7B 129.1(3) . . ?
N2B C8B C7B 105.4(2) . . ?
C10B C9B C2B 123.9(3) . . ?
C10B C9B C18B 119.4(2) . . ?
C2B C9B C18B 116.8(2) . . ?
C11B C10B C9B 120.9(3) . . ?
C11B C10B H10B 119.6 . . ?
C9B C10B H10B 119.6 . . ?
C10B C11B C12B 121.9(3) . . ?
C10B C11B C16B 119.8(2) . . ?
C12B C11B C16B 118.3(3) . . ?
C13B C12B C11B 120.9(3) . . ?
C13B C12B H12B 119.6 . . ?
C11B C12B H12B 119.6 . . ?
C12B C13B C14B 120.6(3) . . ?
C12B C13B H13B 119.7 . . ?
C14B C13B H13B 119.7 . . ?
C15B C14B C13B 120.3(3) . . ?
C15B C14B H14B 119.9 . . ?
C13B C14B H14B 119.9 . . ?
C14B C15B C16B 121.0(3) . . ?
C14B C15B H15B 119.5 . . ?
C16B C15B H15B 119.5 . . ?
C17B C16B C15B 121.6(3) . . ?
C17B C16B C11B 119.5(2) . . ?
C15B C16B C11B 118.9(2) . . ?
C18B C17B C16B 121.0(3) . . ?
C18B C17B H17B 119.5 . . ?
C16B C17B H17B 119.5 . . ?
C17B C18B C7B 123.7(3) . . ?
C17B C18B C9B 119.3(2) . . ?
C7B C18B C9B 117.0(2) . . ?
C24B C19B C20B 121.3(3) . . ?
C24B C19B N1B 119.6(3) . . ?
C20B C19B N1B 119.1(3) . . ?
C19B C20B C21B 119.0(3) . . ?
C19B C20B H20B 120.5 . . ?
C21B C20B H20B 120.5 . . ?
C22B C21B C20B 119.9(3) . . ?
C22B C21B H21B 120.1 . . ?
C20B C21B H21B 120.1 . . ?
C23B C22B C21B 120.3(3) . . ?
C23B C22B H22B 119.8 . . ?
C21B C22B H22B 119.8 . . ?
C22B C23B C24B 120.5(3) . . ?
C22B C23B H23B 119.8 . . ?
C24B C23B H23B 119.8 . . ?
C23B C24B C19B 119.0(3) . . ?
C23B C24B H24B 120.5 . . ?
C19B C24B H24B 120.5 . . ?
C26B C25B C30B 121.0(3) . . ?
C26B C25B N2B 119.9(3) . . ?
C30B C25B N2B 119.1(3) . . ?
C25B C26B C27B 119.5(3) . . ?
C25B C26B H26B 120.2 . . ?
C27B C26B H26B 120.2 . . ?
C28B C27B C26B 119.7(3) . . ?
C28B C27B H27B 120.2 . . ?
C26B C27B H27B 120.2 . . ?
C29B C28B C27B 120.3(3) . . ?
C29B C28B H28B 119.9 . . ?
C27B C28B H28B 119.9 . . ?
C28B C29B C30B 120.5(3) . . ?
C28B C29B H29B 119.7 . . ?
C30B C29B H29B 119.7 . . ?
C29B C30B C25B 118.9(3) . . ?
C29B C30B H30B 120.5 . . ?
C25B C30B H30B 120.5 . . ?
Cl1S C1S Cl2S 112.4(2) . . ?
Cl1S C1S H1SA 109.1 . . ?
Cl2S C1S H1SA 109.1 . . ?
Cl1S C1S H1SB 109.1 . . ?
Cl2S C1S H1SB 109.1 . . ?
H1SA C1S H1SB 107.9 . . ?
 
loop_
 _geom_torsion_atom_site_label_1
 _geom_torsion_atom_site_label_2
 _geom_torsion_atom_site_label_3
 _geom_torsion_atom_site_label_4
 _geom_torsion
 _geom_torsion_site_symmetry_1
 _geom_torsion_site_symmetry_2
 _geom_torsion_site_symmetry_3
 _geom_torsion_site_symmetry_4
 _geom_torsion_publ_flag
C4A N1A C1A O1A 179.3(3) . . . . ?
C19A N1A C1A O1A 1.1(4) . . . . ?
C4A N1A C1A C2A 1.0(3) . . . . ?
C19A N1A C1A C2A -177.2(2) . . . . ?
O1A C1A C2A C3A -177.0(3) . . . . ?
N1A C1A C2A C3A 1.2(3) . . . . ?
O1A C1A C2A C9A -0.1(5) . . . . ?
N1A C1A C2A C9A 178.1(3) . . . . ?
C9A C2A C3A C6A -1.6(4) . . . . ?
C1A C2A C3A C6A 175.4(2) . . . . ?
C9A C2A C3A C4A -179.8(2) . . . . ?
C1A C2A C3A C4A -2.8(3) . . . . ?
C1A N1A C4A O2A 176.3(3) . . . . ?
C19A N1A C4A O2A -5.5(4) . . . . ?
C1A N1A C4A C3A -2.6(3) . . . . ?
C19A N1A C4A C3A 175.6(2) . . . . ?
C2A C3A C4A O2A -175.5(3) . . . . ?
C6A C3A C4A O2A 6.6(5) . . . . ?
C2A C3A C4A N1A 3.4(3) . . . . ?
C6A C3A C4A N1A -174.6(3) . . . . ?
C8A N2A C5A O3A -179.7(3) . . . . ?
C25A N2A C5A O3A 4.8(4) . . . . ?
C8A N2A C5A C6A 1.2(3) . . . . ?
C25A N2A C5A C6A -174.3(2) . . . . ?
C2A C3A C6A C7A 0.6(4) . . . . ?
C4A C3A C6A C7A 178.4(3) . . . . ?
C2A C3A C6A C5A -175.1(3) . . . . ?
C4A C3A C6A C5A 2.7(5) . . . . ?
O3A C5A C6A C7A -179.5(3) . . . . ?
N2A C5A C6A C7A -0.4(3) . . . . ?
O3A C5A C6A C3A -3.5(5) . . . . ?
N2A C5A C6A C3A 175.6(3) . . . . ?
C3A C6A C7A C18A 0.3(4) . . . . ?
C5A C6A C7A C18A 176.8(2) . . . . ?
C3A C6A C7A C8A -177.0(2) . . . . ?
C5A C6A C7A C8A -0.4(3) . . . . ?
C5A N2A C8A O4A 178.4(3) . . . . ?
C25A N2A C8A O4A -6.1(5) . . . . ?
C5A N2A C8A C7A -1.4(3) . . . . ?
C25A N2A C8A C7A 174.1(2) . . . . ?
C6A C7A C8A O4A -178.7(3) . . . . ?
C18A C7A C8A O4A 4.1(5) . . . . ?
C6A C7A C8A N2A 1.1(3) . . . . ?
C18A C7A C8A N2A -176.0(3) . . . . ?
C3A C2A C9A C10A -179.2(3) . . . . ?
C1A C2A C9A C10A 4.4(4) . . . . ?
C3A C2A C9A C18A 1.7(4) . . . . ?
C1A C2A C9A C18A -174.8(3) . . . . ?
C2A C9A C10A C11A -178.1(3) . . . . ?
C18A C9A C10A C11A 1.0(4) . . . . ?
C9A C10A C11A C12A 179.0(3) . . . . ?
C9A C10A C11A C16A -0.2(4) . . . . ?
C10A C11A C12A C13A -178.2(3) . . . . ?
C16A C11A C12A C13A 1.0(4) . . . . ?
C11A C12A C13A C14A -0.3(4) . . . . ?
C12A C13A C14A C15A -0.7(4) . . . . ?
C13A C14A C15A C16A 1.0(4) . . . . ?
C14A C15A C16A C17A 178.7(3) . . . . ?
C14A C15A C16A C11A -0.3(4) . . . . ?
C10A C11A C16A C17A -0.5(4) . . . . ?
C12A C11A C16A C17A -179.7(3) . . . . ?
C10A C11A C16A C15A 178.5(3) . . . . ?
C12A C11A C16A C15A -0.7(4) . . . . ?
C15A C16A C17A C18A -178.6(3) . . . . ?
C11A C16A C17A C18A 0.4(4) . . . . ?
C16A C17A C18A C7A 179.1(3) . . . . ?
C16A C17A C18A C9A 0.4(4) . . . . ?
C6A C7A C18A C17A -178.9(3) . . . . ?
C8A C7A C18A C17A -2.2(4) . . . . ?
C6A C7A C18A C9A -0.2(4) . . . . ?
C8A C7A C18A C9A 176.5(3) . . . . ?
C10A C9A C18A C17A -1.1(4) . . . . ?
C2A C9A C18A C17A 178.1(2) . . . . ?
C10A C9A C18A C7A -179.9(2) . . . . ?
C2A C9A C18A C7A -0.7(4) . . . . ?
C1A N1A C19A C20A -44.1(4) . . . . ?
C4A N1A C19A C20A 137.9(3) . . . . ?
C1A N1A C19A C24A 134.9(3) . . . . ?
C4A N1A C19A C24A -43.1(4) . . . . ?
C24A C19A C20A C21A -0.3(5) . . . . ?
N1A C19A C20A C21A 178.6(3) . . . . ?
C19A C20A C21A C22A -0.3(5) . . . . ?
C20A C21A C22A C23A 1.1(6) . . . . ?
C21A C22A C23A C24A -1.3(5) . . . . ?
C20A C19A C24A C23A 0.1(4) . . . . ?
N1A C19A C24A C23A -178.9(3) . . . . ?
C22A C23A C24A C19A 0.7(5) . . . . ?
C8A N2A C25A C30A 131.5(3) . . . . ?
C5A N2A C25A C30A -53.6(4) . . . . ?
C8A N2A C25A C26A -48.9(4) . . . . ?
C5A N2A C25A C26A 126.1(3) . . . . ?
C30A C25A C26A C27A 0.9(4) . . . . ?
N2A C25A C26A C27A -178.7(3) . . . . ?
C25A C26A C27A C28A 0.4(5) . . . . ?
C26A C27A C28A C29A -1.3(5) . . . . ?
C27A C28A C29A C30A 0.7(5) . . . . ?
C26A C25A C30A C29A -1.4(4) . . . . ?
N2A C25A C30A C29A 178.2(3) . . . . ?
C28A C29A C30A C25A 0.6(4) . . . . ?
C4B N1B C1B O1B 176.5(3) . . . . ?
C19B N1B C1B O1B 1.1(4) . . . . ?
C4B N1B C1B C2B -2.1(3) . . . . ?
C19B N1B C1B C2B -177.4(2) . . . . ?
O1B C1B C2B C3B -177.9(3) . . . . ?
N1B C1B C2B C3B 0.6(3) . . . . ?
O1B C1B C2B C9B 1.8(5) . . . . ?
N1B C1B C2B C9B -179.7(3) . . . . ?
C9B C2B C3B C6B -1.0(4) . . . . ?
C1B C2B C3B C6B 178.6(2) . . . . ?
C9B C2B C3B C4B -178.7(2) . . . . ?
C1B C2B C3B C4B 0.9(3) . . . . ?
C1B N1B C4B O2B -176.6(3) . . . . ?
C19B N1B C4B O2B -1.3(4) . . . . ?
C1B N1B C4B C3B 2.6(3) . . . . ?
C19B N1B C4B C3B 177.9(2) . . . . ?
C2B C3B C4B O2B 177.0(3) . . . . ?
C6B C3B C4B O2B -0.2(5) . . . . ?
C2B C3B C4B N1B -2.1(3) . . . . ?
C6B C3B C4B N1B -179.4(3) . . . . ?
C8B N2B C5B O3B -180.0(3) . . . . ?
C25B N2B C5B O3B 0.5(5) . . . . ?
C8B N2B C5B C6B 0.7(3) . . . . ?
C25B N2B C5B C6B -178.9(3) . . . . ?
C2B C3B C6B C7B 0.5(4) . . . . ?
C4B C3B C6B C7B 177.5(3) . . . . ?
C2B C3B C6B C5B -177.5(3) . . . . ?
C4B C3B C6B C5B -0.5(5) . . . . ?
O3B C5B C6B C7B 178.1(3) . . . . ?
N2B C5B C6B C7B -2.6(3) . . . . ?
O3B C5B C6B C3B -3.7(5) . . . . ?
N2B C5B C6B C3B 175.6(3) . . . . ?
C3B C6B C7B C18B 1.4(4) . . . . ?
C5B C6B C7B C18B 179.9(2) . . . . ?
C3B C6B C7B C8B -175.0(2) . . . . ?
C5B C6B C7B C8B 3.4(3) . . . . ?
C5B N2B C8B O4B -177.9(3) . . . . ?
C25B N2B C8B O4B 1.7(5) . . . . ?
C5B N2B C8B C7B 1.3(3) . . . . ?
C25B N2B C8B C7B -179.2(3) . . . . ?
C6B C7B C8B O4B 176.2(3) . . . . ?
C18B C7B C8B O4B -0.1(5) . . . . ?
C6B C7B C8B N2B -3.0(3) . . . . ?
C18B C7B C8B N2B -179.3(3) . . . . ?
C3B C2B C9B C10B 179.4(3) . . . . ?
C1B C2B C9B C10B -0.1(4) . . . . ?
C3B C2B C9B C18B -0.3(4) . . . . ?
C1B C2B C9B C18B -179.9(3) . . . . ?
C2B C9B C10B C11B 178.6(3) . . . . ?
C18B C9B C10B C11B -1.6(4) . . . . ?
C9B C10B C11B C12B -179.7(3) . . . . ?
C9B C10B C11B C16B 0.2(4) . . . . ?
C10B C11B C12B C13B 179.1(3) . . . . ?
C16B C11B C12B C13B -0.8(4) . . . . ?
C11B C12B C13B C14B 0.2(4) . . . . ?
C12B C13B C14B C15B 0.2(4) . . . . ?
C13B C14B C15B C16B -0.1(4) . . . . ?
C14B C15B C16B C17B 179.5(3) . . . . ?
C14B C15B C16B C11B -0.5(4) . . . . ?
C10B C11B C16B C17B 1.1(4) . . . . ?
C12B C11B C16B C17B -179.1(2) . . . . ?
C10B C11B C16B C15B -179.0(2) . . . . ?
C12B C11B C16B C15B 0.9(4) . . . . ?
C15B C16B C17B C18B 179.2(3) . . . . ?
C11B C16B C17B C18B -0.8(4) . . . . ?
C16B C17B C18B C7B 178.9(3) . . . . ?
C16B C17B C18B C9B -0.6(4) . . . . ?
C6B C7B C18B C17B 177.7(3) . . . . ?
C8B C7B C18B C17B -6.5(4) . . . . ?
C6B C7B C18B C9B -2.7(4) . . . . ?
C8B C7B C18B C9B 173.0(3) . . . . ?
C10B C9B C18B C17B 1.8(4) . . . . ?
C2B C9B C18B C17B -178.4(2) . . . . ?
C10B C9B C18B C7B -177.7(2) . . . . ?
C2B C9B C18B C7B 2.1(4) . . . . ?
C1B N1B C19B C24B 119.7(3) . . . . ?
C4B N1B C19B C24B -55.1(4) . . . . ?
C1B N1B C19B C20B -59.3(4) . . . . ?
C4B N1B C19B C20B 125.9(3) . . . . ?
C24B C19B C20B C21B -1.3(4) . . . . ?
N1B C19B C20B C21B 177.7(3) . . . . ?
C19B C20B C21B C22B 0.5(5) . . . . ?
C20B C21B C22B C23B 1.0(5) . . . . ?
C21B C22B C23B C24B -1.7(5) . . . . ?
C22B C23B C24B C19B 0.9(5) . . . . ?
C20B C19B C24B C23B 0.6(4) . . . . ?
N1B C19B C24B C23B -178.4(3) . . . . ?
C8B N2B C25B C26B -53.0(4) . . . . ?
C5B N2B C25B C26B 126.5(3) . . . . ?
C8B N2B C25B C30B 126.7(3) . . . . ?
C5B N2B C25B C30B -53.9(4) . . . . ?
C30B C25B C26B C27B 0.0(5) . . . . ?
N2B C25B C26B C27B 179.7(3) . . . . ?
C25B C26B C27B C28B 1.1(5) . . . . ?
C26B C27B C28B C29B -0.7(5) . . . . ?
C27B C28B C29B C30B -0.8(5) . . . . ?
C28B C29B C30B C25B 1.9(5) . . . . ?
C26B C25B C30B C29B -1.5(5) . . . . ?
N2B C25B C30B C29B 178.8(3) . . . . ?
 
_refine_diff_density_max    0.332
_refine_diff_density_min   -0.727
_refine_diff_density_rms    0.064


# start Validation Reply Form
_vrf_PLAT340_23051z
;
PROBLEM: Low Bond Precision on C-C Bonds ............... 0.0042 Ang.
RESPONSE: ... Relatively small crystalline specimen with Cl as heavy atom.
 VGY
;
_vrf_PLAT906_23051z
;
PROBLEM: Large K Value in the Analysis of Variance ...... 12.303 Check
RESPONSE: ... Relatively small crystalline specimen with long frame times
 and weak diffraction data. VGY
;
_vrf_PLAT911_23051z
;
PROBLEM: Missing FCF Refl Between Thmin & STh/L= 0.600 9 Report
RESPONSE: ... Acknowledged. VGY
;
# end Validation Reply Form



