#------------------------------------------------------------------------------
#$Date: 2024-10-06 11:08:04 +0300 (Sun, 06 Oct 2024) $
#$Revision: 295266 $
#$URL: file:///home/coder/svn-repositories/cod/cif/7/71/68/7716818.cif $
#------------------------------------------------------------------------------
#
# This file is available in the Crystallography Open Database (COD),
# http://www.crystallography.net/
#
# All data on this site have been placed in the public domain by the
# contributors.
#
data_7716818
loop_
_publ_author_name
'Jaswal, Vishakha'
'Pachisia, Sanya'
'Chaudhary, Jagrity'
'Rangan, Krishnan'
'Sarkar, Madhushree'
_publ_section_title
;
 Selective sensing of picric acid using a Zn(II)-metallacycle:
 experimental and theoretical validation of the sensing mechanism and
 quantitative analysis of sensitivity in contact mode detection.
;
_journal_issue                   35
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              14710
_journal_page_last               14724
_journal_paper_doi               10.1039/d4dt01771d
_journal_volume                  53
_journal_year                    2024
_chemical_formula_moiety         'C76 H52 Cl4 N12 O14 Zn2, 4(C3 H7 N O)'
_chemical_formula_sum            'C88 H80 Cl4 N16 O18 Zn2'
_chemical_formula_weight         1922.22
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2yn'
_space_group_name_H-M_alt        'P 1 21/n 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_audit_creation_date             2024-07-16
_audit_creation_method
;
Olex2 1.5
(compiled 2024.02.16 svn.r378c4104 for OlexSys, GUI svn.r6928)
;
_audit_update_record
;
2024-07-20 deposited with the CCDC.	2024-08-05 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 98.188(2)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   17.2400(3)
_cell_length_b                   11.9521(2)
_cell_length_c                   21.5421(4)
_cell_measurement_reflns_used    9972
_cell_measurement_temperature    93(2)
_cell_measurement_theta_max      78.6660
_cell_measurement_theta_min      4.1310
_cell_volume                     4393.59(14)
_computing_cell_refinement       'CrysAlisPro 1.171.41.93a (Rigaku OD, 2020)'
_computing_data_collection       'CrysAlisPro 1.171.41.93a (Rigaku OD, 2020)'
_computing_data_reduction        'CrysAlisPro 1.171.41.93a (Rigaku OD, 2020)'
_computing_molecular_graphics    'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2018/3 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT  (Sheldrick, 2015)'
_diffrn_ambient_temperature      93(2)
_diffrn_detector                 'Hybrid Pixel Array Detector'
_diffrn_detector_area_resol_mean 5.8140
_diffrn_measured_fraction_theta_full 0.995
_diffrn_measured_fraction_theta_max 0.962
_diffrn_measurement_details
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  tₑₓₚ   ω     θ     κ     φ   Frames
#--------------------------------------------------------------------------
  1  ω    -85.00 -55.00   0.50   10.00    --    0.00 -37.00-150.00   60
  2  ω    -65.00  14.00   0.50   10.00    --    0.00 -37.00 -90.00  158
  3  ω     -8.00  18.00   0.50   10.00    --    0.00 -37.00-150.00   52
  4  ω    -89.00 -50.00   0.50   10.00    --    0.00 -37.00-180.00   78
  5  ω    -23.00  28.00   0.50   10.00    --    0.00 -77.00-150.00  102
  6  ω    108.00 134.00   0.50   40.00    --  107.20 -77.00  90.00   52
  7  ω     18.00  58.00   0.50   40.00    --  107.20 -77.00  90.00   80
  8  ω     18.00 132.00   0.50   40.00    --  107.20 -61.00-150.00  228
  9  ω     54.00 106.00   0.50   40.00    --  107.20 -82.00 150.00  104
 10  ω    169.00 196.00   0.50   40.00    --  107.20  61.00 120.00   54
 11  ω     18.00 126.00   0.50   40.00    --  107.20 -30.00   0.00  216
 12  ω    100.00 144.00   0.50   40.00    --  107.20  61.00 120.00   88
 13  ω     34.00 134.00   0.50   40.00    --  107.20 -77.00-150.00  200
 14  ω    151.00 180.00   0.50   40.00    --  107.20  30.00-120.00   58
 15  ω     18.00 148.00   0.50   40.00    --  107.20   0.00-120.00  260
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'XtaLAB AFC12 (RINC): Kappa dual home/near'
_diffrn_measurement_method       'ω scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      -0.0870654000
_diffrn_orient_matrix_UB_12      -0.0198621000
_diffrn_orient_matrix_UB_13      0.0053864000
_diffrn_orient_matrix_UB_21      0.0210312000
_diffrn_orient_matrix_UB_22      -0.0144948000
_diffrn_orient_matrix_UB_23      0.0714750000
_diffrn_orient_matrix_UB_31      -0.0112828000
_diffrn_orient_matrix_UB_32      0.1265491000
_diffrn_orient_matrix_UB_33      0.0090363000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Cu K\a'
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_unetI/netI     0.0534
_diffrn_reflns_Laue_measured_fraction_full 0.995
_diffrn_reflns_Laue_measured_fraction_max 0.962
_diffrn_reflns_limit_h_max       21
_diffrn_reflns_limit_h_min       -21
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       27
_diffrn_reflns_limit_l_min       -27
_diffrn_reflns_number            15886
_diffrn_reflns_point_group_measured_fraction_full 0.995
_diffrn_reflns_point_group_measured_fraction_max 0.962
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         79.676
_diffrn_reflns_theta_min         4.147
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'Rigaku (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    2.446
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.79954
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.41.93a (Rigaku Oxford Diffraction, 2020)
Empirical absorption correction using spherical harmonics,
implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            colourless
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.453
_exptl_crystal_description       block
_exptl_crystal_F_000             1984
_exptl_crystal_size_max          0.17
_exptl_crystal_size_mid          0.06
_exptl_crystal_size_min          0.04
_refine_diff_density_max         0.887
_refine_diff_density_min         -0.877
_refine_diff_density_rms         0.090
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.987
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     582
_refine_ls_number_reflns         11452
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.987
_refine_ls_R_factor_all          0.0848
_refine_ls_R_factor_gt           0.0614
_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)+(0.1061P)²] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1553
_refine_ls_wR_factor_ref         0.1672
_reflns_Friedel_coverage         0.000
_reflns_number_gt                11452
_reflns_number_total             11452
_reflns_threshold_expression     'I > 2σ(I)'
_twin_special_details
;
Component 2 rotated by 179.9997° 
around [0.51 -0.00 0.86] (reciprocal) or [0.71 0.00 0.71] (direct)
;
_cod_data_source_file            d4dt01771d2.cif
_cod_data_source_block           exp921_twinmodel_20211208_twin1_hklf4
_cod_depositor_comments          'Adding full bibliography for 7716818.cif.'
_cod_database_code               7716818
_shelx_shelxl_version_number     2018/3
_chemical_oxdiff_formula         'C44 H40 Cl2 N8 O9 Zn'
_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.
;
_shelx_estimated_absorpt_t_max   0.908
_shelx_estimated_absorpt_t_min   0.681
_olex2_refinement_description
;
1. Twinned data refinement
 Scales: 0.7433(8)
 0.2567(8)
2. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All N(H) groups
 At 1.5 times of:
  All C(H,H,H) groups
3.a Aromatic/amide H refined with riding coordinates:
 N1(H1), N2(H2), N3(H3), C2(H2A), C4(H4), C6(H6), C10(H10), C12(H12), C13(H13),
  C14(H14), C15(H15), C17(H17), C18(H18), C19(H19), C20(H20), C22(H22),
 C23(H23), C24(H24), C27(H27), C28(H28), C30(H30), C31(H31), C34(H34), C35(H35),
  C37(H37), C38(H38), C39(H39), C42(H42)
3.b Idealised Me refined as rotating group:
 C40(H40A,H40B,H40C), C41(H41A,H41B,H41C), C43(H43A,H43B,H43C), C44(H44A,H44B,
 H44C)
;
_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 1.647
_oxdiff_exptl_absorpt_empirical_full_min 0.710
_oxdiff_twin_integration_method  simultaneous
_oxdiff_twin_items               2
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x+1/2, y+1/2, -z+1/2'
'-x, -y, -z'
'x-1/2, -y-1/2, z-1/2'
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
Zn1 Zn 0.32964(3) 0.06741(4) 0.51488(2) 0.02427(13) Uani 1 1 d . . . . .
Cl1 Cl 0.37197(14) -0.61806(10) 0.61361(9) 0.1062(8) Uani 1 1 d . . . . .
Cl2 Cl 0.54971(6) 0.15728(9) 0.18630(5) 0.0438(2) Uani 1 1 d . . . . .
O1 O 0.08814(18) 0.5505(2) 0.49596(16) 0.0439(8) Uani 1 1 d . . . . .
O2 O 0.34534(17) 0.6910(2) 0.30732(14) 0.0390(7) Uani 1 1 d . . . . .
O3 O 0.02474(17) 0.9305(2) 0.41973(19) 0.0509(9) Uani 1 1 d . . . . .
O4 O 0.34968(18) -0.0958(2) 0.49978(13) 0.0352(6) Uani 1 1 d . . . . .
O5 O 0.27104(18) -0.0812(2) 0.57096(15) 0.0422(7) Uani 1 1 d . . . . .
O6 O 0.39043(16) 0.1258(2) 0.45052(12) 0.0334(6) Uani 1 1 d . . . . .
O7 O 0.28403(16) 0.0918(2) 0.38141(14) 0.0339(6) Uani 1 1 d . . . . .
N1 N 0.19382(18) 0.4561(2) 0.47151(14) 0.0257(6) Uani 1 1 d . . . . .
H1 H 0.235239 0.462194 0.452126 0.031 Uiso 1 1 calc R U . . .
N2 N 0.38318(17) 0.8318(2) 0.37739(14) 0.0264(6) Uani 1 1 d . . . . .
H2 H 0.366523 0.875313 0.405709 0.032 Uiso 1 1 calc R U . . .
N3 N 0.12355(17) 1.0433(2) 0.39819(14) 0.0260(6) Uani 1 1 d . . . . .
H3 H 0.173669 1.044412 0.394312 0.031 Uiso 1 1 calc R U . . .
N4 N 0.23747(17) 0.1693(2) 0.52059(13) 0.0245(6) Uani 1 1 d . . . . .
N5 N 0.59146(17) 0.8975(2) 0.40688(13) 0.0248(6) Uani 1 1 d . . . . .
N6 N 0.0863(2) 1.3337(3) 0.34997(16) 0.0416(8) Uani 1 1 d . . . . .
C1 C 0.1703(2) 0.6484(3) 0.43590(16) 0.0242(7) Uani 1 1 d . . . . .
C2 C 0.2366(2) 0.6506(3) 0.40510(16) 0.0242(7) Uani 1 1 d . . . . .
H2A H 0.266592 0.584546 0.402408 0.029 Uiso 1 1 calc R U . . .
C3 C 0.2585(2) 0.7495(3) 0.37854(16) 0.0235(7) Uani 1 1 d . . . . .
C4 C 0.2138(2) 0.8458(3) 0.38116(17) 0.0256(7) Uani 1 1 d . . . . .
H4 H 0.229814 0.913825 0.364009 0.031 Uiso 1 1 calc R U . . .
C5 C 0.1455(2) 0.8427(3) 0.40891(16) 0.0249(7) Uani 1 1 d . . . . .
C6 C 0.1249(2) 0.7441(3) 0.43655(16) 0.0249(7) Uani 1 1 d . . . . .
H6 H 0.079021 0.742236 0.456238 0.030 Uiso 1 1 calc R U . . .
C7 C 0.1461(2) 0.5474(3) 0.47007(17) 0.0263(7) Uani 1 1 d . . . . .
C8 C 0.3324(2) 0.7531(3) 0.34956(17) 0.0256(7) Uani 1 1 d . . . . .
C9 C 0.0921(2) 0.9422(3) 0.40987(18) 0.0281(7) Uani 1 1 d . . . . .
C10 C 0.2400(2) 0.2716(3) 0.49515(16) 0.0245(7) Uani 1 1 d . . . . .
H10 H 0.281829 0.289220 0.472466 0.029 Uiso 1 1 calc R U . . .
C11 C 0.1834(2) 0.3530(3) 0.50091(15) 0.0234(6) Uani 1 1 d . . . . .
C12 C 0.1221(2) 0.3275(3) 0.53348(17) 0.0280(7) Uani 1 1 d . . . . .
H12 H 0.082557 0.381068 0.538100 0.034 Uiso 1 1 calc R U . . .
C13 C 0.1201(2) 0.2205(3) 0.55936(18) 0.0292(7) Uani 1 1 d . . . . .
H13 H 0.078646 0.200457 0.581876 0.035 Uiso 1 1 calc R U . . .
C14 C 0.1777(2) 0.1443(3) 0.55246(16) 0.0269(7) Uani 1 1 d . . . . .
H14 H 0.175449 0.072084 0.570536 0.032 Uiso 1 1 calc R U . . .
C15 C 0.51640(19) 0.8783(3) 0.41419(16) 0.0234(6) Uani 1 1 d . . . . .
H15 H 0.501546 0.884880 0.454837 0.028 Uiso 1 1 calc R U . . .
C16 C 0.4602(2) 0.8492(3) 0.36448(16) 0.0244(7) Uani 1 1 d . . . . .
C17 C 0.4817(2) 0.8407(3) 0.30453(16) 0.0287(7) Uani 1 1 d . . . . .
H17 H 0.444246 0.822072 0.269328 0.034 Uiso 1 1 calc R U . . .
C18 C 0.5592(2) 0.8603(3) 0.29796(17) 0.0295(7) Uani 1 1 d . . . . .
H18 H 0.575795 0.854482 0.257883 0.035 Uiso 1 1 calc R U . . .
C19 C 0.6122(2) 0.8883(3) 0.34956(17) 0.0266(7) Uani 1 1 d . . . . .
H19 H 0.665223 0.901409 0.344328 0.032 Uiso 1 1 calc R U . . .
C20 C 0.1157(3) 1.2296(3) 0.35848(18) 0.0349(8) Uani 1 1 d . . . . .
H20 H 0.161547 1.211909 0.340673 0.042 Uiso 1 1 calc R U . . .
C21 C 0.0832(2) 1.1466(3) 0.39173(16) 0.0270(7) Uani 1 1 d . . . . .
C22 C 0.0154(2) 1.1697(3) 0.41702(19) 0.0355(8) Uani 1 1 d . . . . .
H22 H -0.008456 1.114702 0.439952 0.043 Uiso 1 1 calc R U . . .
C23 C -0.0166(3) 1.2766(4) 0.4076(2) 0.0423(10) Uani 1 1 d . . . . .
H23 H -0.063202 1.295826 0.423869 0.051 Uiso 1 1 calc R U . . .
C24 C 0.0205(3) 1.3544(4) 0.37422(19) 0.0437(10) Uani 1 1 d . . . . .
H24 H -0.002155 1.426772 0.368212 0.052 Uiso 1 1 calc R U . . .
C25 C 0.3128(2) -0.1394(3) 0.54182(17) 0.0297(8) Uani 1 1 d . . . . .
C26 C 0.3248(2) -0.2611(3) 0.55602(17) 0.0295(8) Uani 1 1 d . . . . .
C27 C 0.3817(3) -0.3213(4) 0.5311(2) 0.0406(10) Uani 1 1 d . . . . .
H27 H 0.411575 -0.286477 0.502666 0.049 Uiso 1 1 calc R U . . .
C28 C 0.3949(3) -0.4326(4) 0.5477(2) 0.0543(14) Uani 1 1 d . . . . .
H28 H 0.432977 -0.474973 0.530127 0.065 Uiso 1 1 calc R U . . .
C29 C 0.3525(4) -0.4807(4) 0.5896(2) 0.0593(15) Uani 1 1 d . . . . .
C30 C 0.2938(4) -0.4236(4) 0.6135(2) 0.0584(15) Uani 1 1 d . . . . .
H30 H 0.263065 -0.459698 0.640781 0.070 Uiso 1 1 calc R U . . .
C31 C 0.2807(3) -0.3121(4) 0.5967(2) 0.0436(10) Uani 1 1 d . . . . .
H31 H 0.241229 -0.270935 0.613279 0.052 Uiso 1 1 calc R U . . .
C32 C 0.3543(2) 0.1157(3) 0.39393(17) 0.0252(7) Uani 1 1 d . . . . .
C33 C 0.4035(2) 0.1319(3) 0.34293(16) 0.0241(7) Uani 1 1 d . . . . .
C34 C 0.4829(2) 0.1539(3) 0.35594(17) 0.0293(7) Uani 1 1 d . . . . .
H34 H 0.506479 0.162825 0.398261 0.035 Uiso 1 1 calc R U . . .
C35 C 0.5285(2) 0.1630(3) 0.30834(17) 0.0312(8) Uani 1 1 d . . . . .
H35 H 0.582941 0.178879 0.317652 0.037 Uiso 1 1 calc R U . . .
C36 C 0.4937(2) 0.1486(3) 0.24698(17) 0.0298(7) Uani 1 1 d . . . . .
C37 C 0.4144(2) 0.1267(4) 0.23285(18) 0.0370(9) Uani 1 1 d . . . . .
H37 H 0.391213 0.116167 0.190543 0.044 Uiso 1 1 calc R U . . .
C38 C 0.3693(2) 0.1201(3) 0.28064(17) 0.0318(8) Uani 1 1 d . . . . .
H38 H 0.314485 0.107460 0.271057 0.038 Uiso 1 1 calc R U . . .
O8 O 0.34385(19) 0.4221(2) 0.41800(15) 0.0427(7) Uani 1 1 d . . . . .
N7 N 0.3652(3) 0.4244(3) 0.31678(17) 0.0448(9) Uani 1 1 d . . . . .
C39 C 0.3869(2) 0.4322(3) 0.37740(19) 0.0357(8) Uani 1 1 d . . . . .
H39 H 0.440719 0.446851 0.391295 0.043 Uiso 1 1 calc R U . . .
C40 C 0.4186(5) 0.4458(5) 0.2722(3) 0.075(2) Uani 1 1 d . . . . .
H40A H 0.401110 0.511997 0.247258 0.112 Uiso 1 1 calc R U . . .
H40B H 0.419473 0.380990 0.244460 0.112 Uiso 1 1 calc R U . . .
H40C H 0.471285 0.458836 0.294738 0.112 Uiso 1 1 calc R U . . .
C41 C 0.2845(4) 0.4020(5) 0.2913(3) 0.0747(19) Uani 1 1 d . . . . .
H41A H 0.281335 0.331040 0.268268 0.112 Uiso 1 1 calc R U . . .
H41B H 0.264521 0.462614 0.262846 0.112 Uiso 1 1 calc R U . . .
H41C H 0.252896 0.397005 0.325622 0.112 Uiso 1 1 calc R U . . .
O9 O 0.2291(3) 0.6538(4) 0.7473(3) 0.0920(16) Uani 1 1 d . . . . .
N8 N 0.3056(3) 0.5028(4) 0.7777(2) 0.0630(12) Uani 1 1 d . . . . .
C42 C 0.2927(4) 0.6129(5) 0.7692(3) 0.0673(17) Uani 1 1 d . . . . .
H42 H 0.335381 0.662432 0.780905 0.081 Uiso 1 1 calc R U . . .
C43 C 0.2405(4) 0.4270(5) 0.7617(3) 0.0716(17) Uani 1 1 d . . . . .
H43A H 0.197343 0.466455 0.736319 0.107 Uiso 1 1 calc R U . . .
H43B H 0.222955 0.399355 0.800240 0.107 Uiso 1 1 calc R U . . .
H43C H 0.257158 0.363771 0.737844 0.107 Uiso 1 1 calc R U . . .
C44 C 0.3768(6) 0.4545(11) 0.8054(5) 0.145(5) Uani 1 1 d . . . . .
H44A H 0.371382 0.427941 0.847641 0.218 Uiso 1 1 calc R U . . .
H44B H 0.418593 0.510653 0.808141 0.218 Uiso 1 1 calc R U . . .
H44C H 0.389958 0.391420 0.779817 0.218 Uiso 1 1 calc R U . . .
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'
Cl Cl 0.3639 0.7018 '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'
O O 0.0492 0.0322 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Zn Zn -1.5491 0.6778 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
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
O4 Zn1 O5 57.94(10) . . ?
O4 Zn1 N4 138.40(12) . . ?
O4 Zn1 N5 102.80(11) . 3_666 ?
O6 Zn1 O4 96.21(11) . . ?
O6 Zn1 O5 154.00(11) . . ?
O6 Zn1 N4 109.24(11) . . ?
O6 Zn1 N5 98.51(11) . 3_666 ?
N4 Zn1 O5 91.37(11) . . ?
N4 Zn1 N5 105.19(12) . 3_666 ?
N5 Zn1 O5 90.85(11) 3_666 . ?
C25 O4 Zn1 99.5(2) . . ?
C25 O5 Zn1 81.2(2) . . ?
C32 O6 Zn1 113.2(2) . . ?
C7 N1 H1 116.7 . . ?
C7 N1 C11 126.5(3) . . ?
C11 N1 H1 116.7 . . ?
C8 N2 H2 117.3 . . ?
C8 N2 C16 125.3(3) . . ?
C16 N2 H2 117.3 . . ?
C9 N3 H3 117.0 . . ?
C9 N3 C21 126.1(3) . . ?
C21 N3 H3 117.0 . . ?
C10 N4 Zn1 116.9(2) . . ?
C10 N4 C14 118.7(3) . . ?
C14 N4 Zn1 124.2(2) . . ?
C15 N5 Zn1 118.3(2) . 3_666 ?
C19 N5 Zn1 122.8(2) . 3_666 ?
C19 N5 C15 118.8(3) . . ?
C24 N6 C20 116.3(4) . . ?
C2 C1 C7 123.3(3) . . ?
C6 C1 C2 119.2(3) . . ?
C6 C1 C7 117.5(3) . . ?
C1 C2 H2A 120.0 . . ?
C3 C2 C1 119.9(3) . . ?
C3 C2 H2A 120.0 . . ?
C2 C3 C4 120.2(3) . . ?
C2 C3 C8 119.6(3) . . ?
C4 C3 C8 120.2(3) . . ?
C3 C4 H4 119.9 . . ?
C3 C4 C5 120.1(3) . . ?
C5 C4 H4 119.9 . . ?
C4 C5 C9 122.7(3) . . ?
C6 C5 C4 119.3(3) . . ?
C6 C5 C9 118.0(3) . . ?
C1 C6 C5 121.1(3) . . ?
C1 C6 H6 119.4 . . ?
C5 C6 H6 119.4 . . ?
O1 C7 N1 123.2(3) . . ?
O1 C7 C1 120.4(3) . . ?
N1 C7 C1 116.4(3) . . ?
O2 C8 N2 125.0(3) . . ?
O2 C8 C3 123.5(3) . . ?
N2 C8 C3 111.6(3) . . ?
O3 C9 N3 123.3(3) . . ?
O3 C9 C5 120.8(3) . . ?
N3 C9 C5 115.9(3) . . ?
N4 C10 H10 118.9 . . ?
N4 C10 C11 122.3(3) . . ?
C11 C10 H10 118.9 . . ?
C10 C11 N1 115.7(3) . . ?
C12 C11 N1 125.1(3) . . ?
C12 C11 C10 119.1(3) . . ?
C11 C12 H12 121.1 . . ?
C11 C12 C13 117.8(3) . . ?
C13 C12 H12 121.1 . . ?
C12 C13 H13 119.8 . . ?
C14 C13 C12 120.4(3) . . ?
C14 C13 H13 119.8 . . ?
N4 C14 C13 121.7(3) . . ?
N4 C14 H14 119.2 . . ?
C13 C14 H14 119.2 . . ?
N5 C15 H15 118.9 . . ?
N5 C15 C16 122.1(3) . . ?
C16 C15 H15 118.9 . . ?
C15 C16 N2 117.4(3) . . ?
C15 C16 C17 119.0(3) . . ?
C17 C16 N2 123.6(3) . . ?
C16 C17 H17 121.0 . . ?
C18 C17 C16 118.0(3) . . ?
C18 C17 H17 121.0 . . ?
C17 C18 H18 120.1 . . ?
C19 C18 C17 119.9(3) . . ?
C19 C18 H18 120.1 . . ?
N5 C19 C18 122.1(3) . . ?
N5 C19 H19 118.9 . . ?
C18 C19 H19 118.9 . . ?
N6 C20 H20 118.0 . . ?
N6 C20 C21 123.9(4) . . ?
C21 C20 H20 118.0 . . ?
C20 C21 N3 116.4(3) . . ?
C22 C21 N3 124.5(3) . . ?
C22 C21 C20 119.1(3) . . ?
C21 C22 H22 121.2 . . ?
C21 C22 C23 117.6(4) . . ?
C23 C22 H22 121.2 . . ?
C22 C23 H23 120.4 . . ?
C24 C23 C22 119.3(4) . . ?
C24 C23 H23 120.4 . . ?
N6 C24 C23 123.8(4) . . ?
N6 C24 H24 118.1 . . ?
C23 C24 H24 118.1 . . ?
O4 C25 C26 118.0(3) . . ?
O5 C25 O4 120.8(3) . . ?
O5 C25 C26 121.2(4) . . ?
C27 C26 C25 120.7(4) . . ?
C31 C26 C25 119.1(4) . . ?
C31 C26 C27 120.1(4) . . ?
C26 C27 H27 120.1 . . ?
C26 C27 C28 119.7(5) . . ?
C28 C27 H27 120.1 . . ?
C27 C28 H28 120.3 . . ?
C29 C28 C27 119.4(5) . . ?
C29 C28 H28 120.3 . . ?
C28 C29 Cl1 119.7(5) . . ?
C28 C29 C30 121.9(4) . . ?
C30 C29 Cl1 118.4(5) . . ?
C29 C30 H30 120.7 . . ?
C29 C30 C31 118.6(5) . . ?
C31 C30 H30 120.7 . . ?
C26 C31 C30 120.3(5) . . ?
C26 C31 H31 119.9 . . ?
C30 C31 H31 119.9 . . ?
O6 C32 C33 115.7(3) . . ?
O7 C32 O6 123.6(3) . . ?
O7 C32 C33 120.7(3) . . ?
C34 C33 C32 121.7(3) . . ?
C34 C33 C38 119.0(3) . . ?
C38 C33 C32 119.2(3) . . ?
C33 C34 H34 119.5 . . ?
C35 C34 C33 121.1(3) . . ?
C35 C34 H34 119.5 . . ?
C34 C35 H35 120.5 . . ?
C36 C35 C34 118.9(3) . . ?
C36 C35 H35 120.5 . . ?
C35 C36 Cl2 120.0(3) . . ?
C37 C36 Cl2 119.0(3) . . ?
C37 C36 C35 121.0(3) . . ?
C36 C37 H37 120.3 . . ?
C38 C37 C36 119.5(4) . . ?
C38 C37 H37 120.3 . . ?
C33 C38 H38 119.8 . . ?
C37 C38 C33 120.5(4) . . ?
C37 C38 H38 119.8 . . ?
C39 N7 C40 122.1(5) . . ?
C39 N7 C41 120.9(5) . . ?
C40 N7 C41 116.8(5) . . ?
O8 C39 N7 125.9(4) . . ?
O8 C39 H39 117.0 . . ?
N7 C39 H39 117.0 . . ?
N7 C40 H40A 109.5 . . ?
N7 C40 H40B 109.5 . . ?
N7 C40 H40C 109.5 . . ?
H40A C40 H40B 109.5 . . ?
H40A C40 H40C 109.5 . . ?
H40B C40 H40C 109.5 . . ?
N7 C41 H41A 109.5 . . ?
N7 C41 H41B 109.5 . . ?
N7 C41 H41C 109.5 . . ?
H41A C41 H41B 109.5 . . ?
H41A C41 H41C 109.5 . . ?
H41B C41 H41C 109.5 . . ?
C42 N8 C43 118.3(5) . . ?
C42 N8 C44 125.1(7) . . ?
C44 N8 C43 116.3(7) . . ?
O9 C42 N8 124.2(6) . . ?
O9 C42 H42 117.9 . . ?
N8 C42 H42 117.9 . . ?
N8 C43 H43A 109.5 . . ?
N8 C43 H43B 109.5 . . ?
N8 C43 H43C 109.5 . . ?
H43A C43 H43B 109.5 . . ?
H43A C43 H43C 109.5 . . ?
H43B C43 H43C 109.5 . . ?
N8 C44 H44A 109.5 . . ?
N8 C44 H44B 109.5 . . ?
N8 C44 H44C 109.5 . . ?
H44A C44 H44B 109.5 . . ?
H44A C44 H44C 109.5 . . ?
H44B C44 H44C 109.5 . . ?
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
Zn1 O4 2.015(3) . ?
Zn1 O5 2.446(3) . ?
Zn1 O6 1.980(3) . ?
Zn1 N4 2.020(3) . ?
Zn1 N5 2.053(3) 3_666 ?
Cl1 C29 1.739(5) . ?
Cl2 C36 1.736(4) . ?
O1 C7 1.212(4) . ?
O2 C8 1.219(4) . ?
O3 C9 1.218(5) . ?
O4 C25 1.289(5) . ?
O5 C25 1.234(5) . ?
O6 C32 1.293(4) . ?
O7 C32 1.236(4) . ?
N1 H1 0.8800 . ?
N1 C7 1.365(4) . ?
N1 C11 1.408(4) . ?
N2 H2 0.8800 . ?
N2 C8 1.365(4) . ?
N2 C16 1.410(4) . ?
N3 H3 0.8800 . ?
N3 C9 1.363(4) . ?
N3 C21 1.415(4) . ?
N4 C10 1.344(4) . ?
N4 C14 1.351(4) . ?
N5 C15 1.345(4) . ?
N5 C19 1.338(4) . ?
N6 C20 1.346(5) . ?
N6 C24 1.337(6) . ?
C1 C2 1.402(5) . ?
C1 C6 1.387(5) . ?
C1 C7 1.503(5) . ?
C2 H2A 0.9500 . ?
C2 C3 1.389(4) . ?
C3 C4 1.390(5) . ?
C3 C8 1.496(5) . ?
C4 H4 0.9500 . ?
C4 C5 1.395(5) . ?
C5 C6 1.389(5) . ?
C5 C9 1.506(5) . ?
C6 H6 0.9500 . ?
C10 H10 0.9500 . ?
C10 C11 1.395(5) . ?
C11 C12 1.384(5) . ?
C12 H12 0.9500 . ?
C12 C13 1.398(5) . ?
C13 H13 0.9500 . ?
C13 C14 1.370(5) . ?
C14 H14 0.9500 . ?
C15 H15 0.9500 . ?
C15 C16 1.382(5) . ?
C16 C17 1.397(5) . ?
C17 H17 0.9500 . ?
C17 C18 1.383(5) . ?
C18 H18 0.9500 . ?
C18 C19 1.376(5) . ?
C19 H19 0.9500 . ?
C20 H20 0.9500 . ?
C20 C21 1.388(5) . ?
C21 C22 1.386(5) . ?
C22 H22 0.9500 . ?
C22 C23 1.395(5) . ?
C23 H23 0.9500 . ?
C23 C24 1.386(7) . ?
C24 H24 0.9500 . ?
C25 C26 1.495(5) . ?
C26 C27 1.385(6) . ?
C26 C31 1.381(6) . ?
C27 H27 0.9500 . ?
C27 C28 1.389(6) . ?
C28 H28 0.9500 . ?
C28 C29 1.365(8) . ?
C29 C30 1.379(9) . ?
C30 H30 0.9500 . ?
C30 C31 1.391(6) . ?
C31 H31 0.9500 . ?
C32 C33 1.493(5) . ?
C33 C34 1.383(5) . ?
C33 C38 1.394(5) . ?
C34 H34 0.9500 . ?
C34 C35 1.383(5) . ?
C35 H35 0.9500 . ?
C35 C36 1.383(5) . ?
C36 C37 1.383(6) . ?
C37 H37 0.9500 . ?
C37 C38 1.378(5) . ?
C38 H38 0.9500 . ?
O8 C39 1.231(5) . ?
N7 C39 1.309(5) . ?
N7 C40 1.443(6) . ?
N7 C41 1.446(7) . ?
C39 H39 0.9500 . ?
C40 H40A 0.9800 . ?
C40 H40B 0.9800 . ?
C40 H40C 0.9800 . ?
C41 H41A 0.9800 . ?
C41 H41B 0.9800 . ?
C41 H41C 0.9800 . ?
O9 C42 1.231(8) . ?
N8 C42 1.343(8) . ?
N8 C43 1.444(8) . ?
N8 C44 1.411(9) . ?
C42 H42 0.9500 . ?
C43 H43A 0.9800 . ?
C43 H43B 0.9800 . ?
C43 H43C 0.9800 . ?
C44 H44A 0.9800 . ?
C44 H44B 0.9800 . ?
C44 H44C 0.9800 . ?
loop_
_geom_hbond_atom_site_label_D
_geom_hbond_atom_site_label_H
_geom_hbond_atom_site_label_A
_geom_hbond_distance_DH
_geom_hbond_distance_HA
_geom_hbond_distance_DA
_geom_hbond_angle_DHA
_geom_hbond_site_symmetry_A
_geom_hbond_publ_flag
N3 H3 O7 0.88 2.04 2.900(4) 164.5 1_565 yes
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
Zn1 O4 C25 O5 8.9(4) . . . . ?
Zn1 O4 C25 C26 -168.5(3) . . . . ?
Zn1 O5 C25 O4 -7.3(3) . . . . ?
Zn1 O5 C25 C26 170.0(3) . . . . ?
Zn1 O6 C32 O7 12.7(4) . . . . ?
Zn1 O6 C32 C33 -165.7(2) . . . . ?
Zn1 N4 C10 C11 -174.2(3) . . . . ?
Zn1 N4 C14 C13 174.2(3) . . . . ?
Zn1 N5 C15 C16 -177.1(2) 3_666 . . . ?
Zn1 N5 C19 C18 177.4(3) 3_666 . . . ?
Cl1 C29 C30 C31 176.9(4) . . . . ?
Cl2 C36 C37 C38 -179.7(3) . . . . ?
O4 C25 C26 C27 8.6(5) . . . . ?
O4 C25 C26 C31 -174.2(4) . . . . ?
O5 C25 C26 C27 -168.8(4) . . . . ?
O5 C25 C26 C31 8.3(5) . . . . ?
O6 C32 C33 C34 1.4(5) . . . . ?
O6 C32 C33 C38 178.7(3) . . . . ?
O7 C32 C33 C34 -177.2(3) . . . . ?
O7 C32 C33 C38 0.1(5) . . . . ?
N1 C11 C12 C13 179.3(3) . . . . ?
N2 C16 C17 C18 179.7(3) . . . . ?
N3 C21 C22 C23 178.7(4) . . . . ?
N4 C10 C11 N1 -179.8(3) . . . . ?
N4 C10 C11 C12 -0.5(5) . . . . ?
N5 C15 C16 N2 -179.5(3) . . . . ?
N5 C15 C16 C17 -0.7(5) . . . . ?
N6 C20 C21 N3 -177.6(4) . . . . ?
N6 C20 C21 C22 1.3(6) . . . . ?
C1 C2 C3 C4 -1.5(5) . . . . ?
C1 C2 C3 C8 175.9(3) . . . . ?
C2 C1 C6 C5 -2.0(5) . . . . ?
C2 C1 C7 O1 179.8(4) . . . . ?
C2 C1 C7 N1 1.8(5) . . . . ?
C2 C3 C4 C5 -1.8(5) . . . . ?
C2 C3 C8 O2 57.2(5) . . . . ?
C2 C3 C8 N2 -121.3(3) . . . . ?
C3 C4 C5 C6 3.2(5) . . . . ?
C3 C4 C5 C9 -176.3(3) . . . . ?
C4 C3 C8 O2 -125.5(4) . . . . ?
C4 C3 C8 N2 56.1(4) . . . . ?
C4 C5 C6 C1 -1.3(5) . . . . ?
C4 C5 C9 O3 161.4(4) . . . . ?
C4 C5 C9 N3 -17.6(5) . . . . ?
C6 C1 C2 C3 3.3(5) . . . . ?
C6 C1 C7 O1 1.3(5) . . . . ?
C6 C1 C7 N1 -176.8(3) . . . . ?
C6 C5 C9 O3 -18.1(6) . . . . ?
C6 C5 C9 N3 162.9(3) . . . . ?
C7 N1 C11 C10 179.3(3) . . . . ?
C7 N1 C11 C12 0.1(6) . . . . ?
C7 C1 C2 C3 -175.2(3) . . . . ?
C7 C1 C6 C5 176.7(3) . . . . ?
C8 N2 C16 C15 -143.6(3) . . . . ?
C8 N2 C16 C17 37.7(5) . . . . ?
C8 C3 C4 C5 -179.2(3) . . . . ?
C9 N3 C21 C20 -157.3(4) . . . . ?
C9 N3 C21 C22 23.8(6) . . . . ?
C9 C5 C6 C1 178.2(3) . . . . ?
C10 N4 C14 C13 0.0(5) . . . . ?
C10 C11 C12 C13 0.2(5) . . . . ?
C11 N1 C7 O1 1.5(6) . . . . ?
C11 N1 C7 C1 179.5(3) . . . . ?
C11 C12 C13 C14 0.2(6) . . . . ?
C12 C13 C14 N4 -0.3(6) . . . . ?
C14 N4 C10 C11 0.4(5) . . . . ?
C15 N5 C19 C18 0.3(5) . . . . ?
C15 C16 C17 C18 1.0(5) . . . . ?
C16 N2 C8 O2 -4.1(6) . . . . ?
C16 N2 C8 C3 174.3(3) . . . . ?
C16 C17 C18 C19 -0.6(5) . . . . ?
C17 C18 C19 N5 0.0(6) . . . . ?
C19 N5 C15 C16 0.1(5) . . . . ?
C20 N6 C24 C23 1.2(6) . . . . ?
C20 C21 C22 C23 -0.1(6) . . . . ?
C21 N3 C9 O3 -4.3(6) . . . . ?
C21 N3 C9 C5 174.7(3) . . . . ?
C21 C22 C23 C24 -0.5(6) . . . . ?
C22 C23 C24 N6 -0.1(7) . . . . ?
C24 N6 C20 C21 -1.8(6) . . . . ?
C25 C26 C27 C28 176.3(4) . . . . ?
C25 C26 C31 C30 -176.3(4) . . . . ?
C26 C27 C28 C29 -1.4(6) . . . . ?
C27 C26 C31 C30 0.9(6) . . . . ?
C27 C28 C29 Cl1 -176.9(3) . . . . ?
C27 C28 C29 C30 3.5(7) . . . . ?
C28 C29 C30 C31 -3.5(7) . . . . ?
C29 C30 C31 C26 1.2(7) . . . . ?
C31 C26 C27 C28 -0.8(6) . . . . ?
C32 C33 C34 C35 176.6(3) . . . . ?
C32 C33 C38 C37 -175.3(3) . . . . ?
C33 C34 C35 C36 -0.7(6) . . . . ?
C34 C33 C38 C37 2.1(6) . . . . ?
C34 C35 C36 Cl2 -178.9(3) . . . . ?
C34 C35 C36 C37 0.7(6) . . . . ?
C35 C36 C37 C38 0.7(6) . . . . ?
C36 C37 C38 C33 -2.1(6) . . . . ?
C38 C33 C34 C35 -0.7(5) . . . . ?
C40 N7 C39 O8 175.2(4) . . . . ?
C41 N7 C39 O8 -0.1(7) . . . . ?
C43 N8 C42 O9 -1.7(9) . . . . ?
C44 N8 C42 O9 -176.8(7) . . . . ?
loop_
_twin_individual_id
_twin_individual_mass_fraction_refined
_oxdiff_twin_reflns_isolated
_oxdiff_twin_reflns_overlapped
_twin_individual_twin_lattice_type
_twin_individual_twin_matrix_11
_twin_individual_twin_matrix_12
_twin_individual_twin_matrix_13
_twin_individual_twin_matrix_21
_twin_individual_twin_matrix_22
_twin_individual_twin_matrix_23
_twin_individual_twin_matrix_31
_twin_individual_twin_matrix_32
_twin_individual_twin_matrix_33
1 0.7433(8) 16310 10602 ref 1.0000 0.0000 0.0000 0.0000 1.0000 0.0000 0.0000
0.0000 1.0000
2 0.2567(8) 16359 10602 nmt -0.2566 0.0004 0.7445 -0.0002 -1.0001 0.0001 1.2546
-0.0012 0.2558
