# Electronic Supplementary Material (ESI) for Dalton Transactions.
# This journal is © The Royal Society of Chemistry 2021

####################################################################### 
# 
# This file contains crystal structure data downloaded from the 
# Cambridge Structural Database (CSD) hosted by the Cambridge 
# Crystallographic Data Centre (CCDC).
# 
# Full information about CCDC data access policies and citation 
# guidelines are available at http://www.ccdc.cam.ac.uk/access/V1 
# 
# Audit and citation data items may have been added by the CCDC. 
# Please retain this information to preserve the provenance of 
# this file and to allow appropriate attribution of the data. 
# 
#######################################################################

data_md_4276_mada
_database_code_depnum_ccdc_archive 'CCDC 1982348'
loop_
_audit_author_name
_audit_author_address
'Dascalu Mihaela'
;Petru Poni Institute of Macromolecular Chemistry, Iasi
Romania
;
_audit_update_record             
;
2021-08-01 deposited with the CCDC.	2021-08-20 downloaded from the CCDC.
;
_audit_creation_date             2021-07-30
_audit_creation_method           
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_shelx_SHELXL_version_number     2018/3
_chemical_name_common            ?
_chemical_name_systematic        ?
_chemical_formula_moiety         '2(C24 H30 Cl4 N2 Ni O3 Si2)'
_chemical_formula_sum            'C48 H60 Cl8 N4 Ni2 O6 Si4'
_chemical_formula_weight         1302.38
_chemical_melting_point          ?
_chemical_oxdiff_formula         C30H30N2Cl2Si2Ni2
_chemical_oxdiff_usercomment     DS-109
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'
Ni Ni 0.3393 1.1124 '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'
Si Si 0.0817 0.0704 '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      monoclinic
_space_group_IT_number           14
_space_group_name_H-M_alt        'P 1 21/c 1'
_space_group_name_Hall           '-P 2ybc'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, y+1/2, -z+1/2'
'-x, -y, -z'
'x, -y-1/2, z-1/2'

_cell_length_a                   15.2553(12)
_cell_length_b                   23.7162(17)
_cell_length_c                   17.6798(13)
_cell_angle_alpha                90
_cell_angle_beta                 108.105(9)
_cell_angle_gamma                90
_cell_volume                     6079.8(8)
_cell_formula_units_Z            4
_cell_measurement_reflns_used    5287
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      23.6640
_cell_measurement_theta_min      1.7840
_shelx_estimated_absorpt_T_max   0.811
_shelx_estimated_absorpt_T_min   0.610
_exptl_absorpt_coefficient_mu    1.097
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.76476
_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            'clear light brown'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   light
_exptl_crystal_colour_primary    brown
_exptl_crystal_density_diffrn    1.423
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       prism
_exptl_crystal_F_000             2688
_exptl_crystal_size_max          0.5
_exptl_crystal_size_mid          0.4
_exptl_crystal_size_min          0.2
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0686
_diffrn_reflns_av_unetI/netI     0.0978
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 1.000
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       22
_diffrn_reflns_limit_k_min       -28
_diffrn_reflns_limit_l_max       14
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            31505
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 1.000
_diffrn_reflns_theta_full        25.025
_diffrn_reflns_theta_max         25.025
_diffrn_reflns_theta_min         1.485
_diffrn_ambient_temperature      293(2)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 8.0797
_diffrn_detector_type            Eos
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 1.000
_diffrn_measurement_details      
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  tₑₓₚ   ω     θ     κ     φ   Frames
#--------------------------------------------------------------------------
  1  ω     33.00  65.00   1.00    6.00    --   17.79-178.00 -60.00   32
  2  ω     10.00  74.00   1.00    6.00    --   17.79  57.00  30.00   64
  3  ω      3.00  84.00   1.00    6.00    --   17.79  57.00 -60.00   81
  4  ω     60.00  85.00   1.00    6.00    --   17.79  77.00-120.00   25
  5  ω     35.00  89.00   1.00    6.00    --   17.79 178.00-120.00   54
  6  ω     38.00  75.00   1.00    6.00    --   17.79 178.00 150.00   37
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'Xcalibur, Eos'
_diffrn_measurement_method       'ω scans'
_diffrn_orient_matrix_type       
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      0.0254650000
_diffrn_orient_matrix_UB_12      0.0017191000
_diffrn_orient_matrix_UB_13      0.0409817000
_diffrn_orient_matrix_UB_21      0.0382884000
_diffrn_orient_matrix_UB_22      -0.0128383000
_diffrn_orient_matrix_UB_23      -0.0077308000
_diffrn_orient_matrix_UB_31      0.0166871000
_diffrn_orient_matrix_UB_32      0.0269889000
_diffrn_orient_matrix_UB_33      -0.0063007000
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_source                   'fine-focus sealed X-ray tube'
_diffrn_source_type              'Enhance (Mo) X-ray Source'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                6217
_reflns_number_total             10737
_reflns_odcompleteness_completeness 99.94
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     26.32
_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    'olex2.solve (Bourhis et al., 2015)'
_refine_diff_density_max         0.459
_refine_diff_density_min         -0.375
_refine_diff_density_rms         0.079
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.043
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     658
_refine_ls_number_reflns         10737
_refine_ls_number_restraints     9
_refine_ls_R_factor_all          0.1354
_refine_ls_R_factor_gt           0.0727
_refine_ls_restrained_S_all      1.043
_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)+(0.0359P)²+5.0777P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1202
_refine_ls_wR_factor_ref         0.1474
_refine_special_details          ?
_olex2_refinement_description    
;
1. Others
 Fixed Uiso: H3A(0.082) H5A(0.06) H7A(0.065) H8AA(0.067) H8AB(0.067)
 H9AA(0.065) H9AB(0.065) H10E(0.076) H10F(0.076) H11D(0.173) H11E(0.173)
 H11F(0.173) H12D(0.145) H12E(0.145) H12F(0.145) H13D(0.149) H13E(0.149)
 H13F(0.149) H14D(0.165) H14E(0.165) H14F(0.165) H15C(0.074) H15D(0.074)
 H16C(0.074) H16D(0.074) H17C(0.067) H17D(0.067) H18A(0.065) H20A(0.083)
 H22A(0.091) H3B(0.093) H5B(0.085) H7B(0.077) H8BA(0.08) H8BB(0.08) H8BC(0.08)
 H8BD(0.08) H9BA(0.084) H9BB(0.084) H9XA(0.084) H9XB(0.084) H10A(0.084)
 H10B(0.084) H10C(0.084) H10D(0.084) H11A(0.218) H11B(0.218) H11C(0.218)
 H12A(0.165) H12B(0.165) H12C(0.165) H13A(0.201) H13B(0.201) H13C(0.201)
 H14A(0.196) H14B(0.196) H14C(0.196) H15A(0.082) H15B(0.082) H16A(0.074)
 H16B(0.074) H17A(0.069) H17B(0.069) H18B(0.063) H20B(0.064) H22B(0.086)
 Fixed X: H3A(0.339772) H5A(0.405547) H7A(0.441648) H8AA(0.457399)
 H8AB(0.375437) H9AA(0.46877) H9AB(0.507339) H10E(0.576818) H10F(0.61937)
 H11D(0.772648) H11E(0.803764) H11F(0.818504) H12D(0.716249) H12E(0.702123)
 H12F(0.616788) H13D(0.746022) H13E(0.680426) H13F(0.676296) H14D(0.556177)
 H14E(0.594257) H14F(0.662745) H15C(0.435245) H15D(0.464206) H16C(0.485186)
 H16D(0.492377) H17C(0.331915) H17D(0.35264) H18A(0.240376) H20A(0.124793)
 H22A(0.09675) H3B(0.579634) H5B(0.407105) H7B(0.25326) H8BA(0.118892)
 H8BB(0.114666) H8BC(0.130684) H8BD(0.090877) H9BA(-0.00655) H9BB(0.076508)
 H9XA(0.033135) H9XB(-0.023016) H10A(0.015751) H10B(0.080557) H10C(0.078757)
 H10D(0.012728) H11A(-0.032162) H11B(-0.112195) H11C(-0.134123) H12A(-0.231573)
 H12B(-0.193663) H12C(-0.173586) H13A(0.029959) H13B(-0.076665) H13C(-0.022894)
 H14A(-0.154962) H14B(-0.207249) H14C(-0.171216) H15A(0.036975) H15B(0.04096)
 H16A(0.148702) H16B(0.155661) H17A(0.214816) H17B(0.277853) H18B(0.172418)
 H20B(0.140624) H22B(0.078566)
 Fixed Y: H3A(0.555071) H5A(0.398483) H7A(0.378638) H8AA(0.344191)
 H8AB(0.357374) H9AA(0.42748) H9AB(0.366395) H10E(0.439845) H10F(0.381296)
 H11D(0.488152) H11E(0.427212) H11F(0.477629) H12D(0.423475) H12E(0.368934)
 H12F(0.399348) H13D(0.603349) H13E(0.65414) H13F(0.624821) H14D(0.540797)
 H14E(0.602637) H14F(0.551667) H15C(0.5631) H15D(0.626428) H16C(0.566496)
 H16D(0.631975) H17C(0.635772) H17D(0.612148) H18A(0.589622) H20A(0.557137)
 H22A(0.391217) H3B(0.237422) H5B(0.281733) H7B(0.308138) H8BA(0.342374)
 H8BB(0.394907) H8BC(0.366538) H8BD(0.385329) H9BA(0.316185) H9BB(0.274191)
 H9XA(0.338102) H9XB(0.348446) H10A(0.312502) H10B(0.260931) H10C(0.248838)
 H10D(0.259171) H11A(0.144625) H11B(0.169831) H11C(0.14197) H12A(0.253622)
 H12B(0.280632) H12C(0.309354) H13A(0.137737) H13B(0.127549) H13C(0.151958)
 H14A(0.253921) H14B(0.225154) H14C(0.287182) H15A(0.308039) H15B(0.277464)
 H16A(0.244646) H16B(0.218443) H17A(0.303579) H17B(0.28063) H18B(0.387194)
 H20B(0.485233) H22B(0.584725)
 Fixed Z: H3A(0.369384) H5A(0.451674) H7A(0.592177) H8AA(0.702741)
 H8AB(0.735946) H9AA(0.82017) H9AB(0.841628) H10E(0.749619) H10F(0.782454)
 H11D(0.830584) H11E(0.86192) H11F(0.921929) H12D(1.019886) H12E(0.967361)
 H12F(0.980531) H13D(0.93572) H13E(0.936189) H13F(0.855683) H14D(1.034656)
 H14E(1.047287) H14F(1.059938) H15C(0.872626) H15D(0.886448) H16C(0.756799)
 H16D(0.768314) H17C(0.749793) H17D(0.674082) H18A(0.791935) H20A(0.842711)
 H22A(0.874624) H3B(0.467583) H5B(0.256065) H7B(0.241686) H8BA(0.207445)
 H8BB(0.260014) H8BC(0.212024) H8BD(0.280186) H9BA(0.20044) H9BB(0.216721)
 H9XA(0.328689) H9XB(0.239151) H10A(0.342413) H10B(0.345045) H10C(0.291321)
 H10D(0.205059) H11A(0.25164) H11B(0.18108) H11C(0.253572) H12A(0.259251)
 H12B(0.194697) H12C(0.278227) H13A(0.507778) H13B(0.484542) H13C(0.56857)
 H14A(0.535519) H14B(0.454161) H14C(0.455702) H15A(0.501959) H15B(0.581217)
 H16A(0.485956) H16B(0.568887) H17A(0.631837) H17B(0.583459) H18B(0.615351)
 H20B(0.626512) H22B(0.434074)
;
_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
Ni1A Ni 0.34309(4) 0.48514(3) 0.69322(4) 0.0475(2) Uani 1 1 d . . . . .
Cl1A Cl 0.33898(16) 0.61721(8) 0.50104(11) 0.1091(7) Uani 1 1 d . . . . .
Cl2A Cl 0.35947(15) 0.45071(9) 0.30261(10) 0.1027(7) Uani 1 1 d . . . . .
Cl3A Cl 0.22045(14) 0.34037(8) 0.80887(12) 0.0983(6) Uani 1 1 d . . . . .
Cl4A Cl 0.01805(14) 0.49028(11) 0.91032(14) 0.1241(8) Uani 1 1 d . . . . .
Si1A Si 0.66406(11) 0.44892(8) 0.88417(10) 0.0670(5) Uani 1 1 d . . . . .
Si2A Si 0.59766(11) 0.56923(8) 0.92380(10) 0.0634(5) Uani 1 1 d . . . . .
O1A O 0.3747(3) 0.52770(16) 0.6190(2) 0.0613(11) Uani 1 1 d . . . . .
O2A O 0.2916(2) 0.43868(16) 0.7517(2) 0.0567(10) Uani 1 1 d . . . . .
O3A O 0.6157(3) 0.50771(17) 0.8927(3) 0.0806(13) Uani 1 1 d . . . . .
N1A N 0.3968(3) 0.41875(19) 0.6652(3) 0.0509(12) Uani 1 1 d . . . . .
N2A N 0.3095(3) 0.55247(19) 0.7349(2) 0.0488(11) Uani 1 1 d . . . . .
C1A C 0.3736(3) 0.5097(2) 0.5502(3) 0.0483(14) Uani 1 1 d . . . . .
C2A C 0.3565(4) 0.5468(3) 0.4852(4) 0.0613(16) Uani 1 1 d . . . . .
C3A C 0.3525(4) 0.5295(3) 0.4113(4) 0.0686(18) Uani 1 1 d . . . . .
H3A H 0.339772 0.555071 0.369384 0.082 Uiso 1 1 calc R U . . .
C4A C 0.3679(4) 0.4725(3) 0.3986(4) 0.0644(17) Uani 1 1 d . . . . .
C5A C 0.3903(3) 0.4354(2) 0.4599(3) 0.0496(14) Uani 1 1 d . . . . .
H5A H 0.405547 0.398483 0.451674 0.060 Uiso 1 1 calc R U . . .
C6A C 0.3906(3) 0.4523(2) 0.5342(4) 0.0519(15) Uani 1 1 d . . . . .
C7A C 0.4131(3) 0.4120(2) 0.5992(4) 0.0545(15) Uani 1 1 d . . . . .
H7A H 0.441648 0.378638 0.592177 0.065 Uiso 1 1 calc R U . . .
C8A C 0.4282(4) 0.3737(2) 0.7245(3) 0.0557(15) Uani 1 1 d . . . . .
H8AA H 0.457399 0.344191 0.702741 0.067 Uiso 1 1 calc R U . . .
H8AB H 0.375437 0.357374 0.735946 0.067 Uiso 1 1 calc R U . . .
C9A C 0.4966(3) 0.3957(2) 0.8016(3) 0.0545(15) Uani 1 1 d . . . . .
H9AA H 0.468770 0.427480 0.820170 0.065 Uiso 1 1 calc R U . . .
H9AB H 0.507339 0.366395 0.841628 0.065 Uiso 1 1 calc R U . . .
C10A C 0.5878(4) 0.4141(3) 0.7942(3) 0.0631(17) Uani 1 1 d . . . . .
H10E H 0.576818 0.439845 0.749619 0.076 Uiso 1 1 calc R U . . .
H10F H 0.619370 0.381296 0.782454 0.076 Uiso 1 1 calc R U . . .
C11A C 0.7784(4) 0.4620(4) 0.8734(5) 0.116(3) Uani 1 1 d . . . . .
H11D H 0.772648 0.488152 0.830584 0.173 Uiso 1 1 calc R U . . .
H11E H 0.803764 0.427212 0.861920 0.173 Uiso 1 1 calc R U . . .
H11F H 0.818504 0.477629 0.921929 0.173 Uiso 1 1 calc R U . . .
C12A C 0.6763(5) 0.4048(3) 0.9738(4) 0.096(2) Uani 1 1 d . . . . .
H12D H 0.716249 0.423475 1.019886 0.145 Uiso 1 1 calc R U . . .
H12E H 0.702123 0.368934 0.967361 0.145 Uiso 1 1 calc R U . . .
H12F H 0.616788 0.399348 0.980531 0.145 Uiso 1 1 calc R U . . .
C13A C 0.6857(4) 0.6189(3) 0.9114(4) 0.099(2) Uani 1 1 d . . . . .
H13D H 0.746022 0.603349 0.935720 0.149 Uiso 1 1 calc R U . . .
H13E H 0.680426 0.654140 0.936189 0.149 Uiso 1 1 calc R U . . .
H13F H 0.676296 0.624821 0.855683 0.149 Uiso 1 1 calc R U . . .
C14A C 0.6034(5) 0.5657(3) 1.0290(4) 0.110(3) Uani 1 1 d . . . . .
H14D H 0.556177 0.540797 1.034656 0.165 Uiso 1 1 calc R U . . .
H14E H 0.594257 0.602637 1.047287 0.165 Uiso 1 1 calc R U . . .
H14F H 0.662745 0.551667 1.059938 0.165 Uiso 1 1 calc R U . . .
C15A C 0.4780(4) 0.5911(3) 0.8648(3) 0.0620(16) Uani 1 1 d . . . . .
H15C H 0.435245 0.563100 0.872626 0.074 Uiso 1 1 calc R U . . .
H15D H 0.464206 0.626428 0.886448 0.074 Uiso 1 1 calc R U . . .
C16A C 0.4599(4) 0.5986(2) 0.7769(3) 0.0618(16) Uani 1 1 d . . . . .
H16C H 0.485186 0.566496 0.756799 0.074 Uiso 1 1 calc R U . . .
H16D H 0.492377 0.631975 0.768314 0.074 Uiso 1 1 calc R U . . .
C17A C 0.3587(3) 0.6044(2) 0.7294(3) 0.0562(15) Uani 1 1 d . . . . .
H17C H 0.331915 0.635772 0.749793 0.067 Uiso 1 1 calc R U . . .
H17D H 0.352640 0.612148 0.674082 0.067 Uiso 1 1 calc R U . . .
C18A C 0.2527(4) 0.5541(2) 0.7754(3) 0.0544(15) Uani 1 1 d . . . . .
H18A H 0.240376 0.589622 0.791935 0.065 Uiso 1 1 calc R U . . .
C19A C 0.2066(3) 0.5083(3) 0.7979(3) 0.0527(15) Uani 1 1 d . . . . .
C20A C 0.1412(4) 0.5201(3) 0.8363(3) 0.0692(19) Uani 1 1 d . . . . .
H20A H 0.124793 0.557137 0.842711 0.083 Uiso 1 1 calc R U . . .
C21A C 0.1012(4) 0.4758(4) 0.8645(4) 0.075(2) Uani 1 1 d . . . . .
C22A C 0.1245(4) 0.4204(3) 0.8552(4) 0.076(2) Uani 1 1 d . . . . .
H22A H 0.096750 0.391217 0.874624 0.091 Uiso 1 1 calc R U . . .
C23A C 0.1878(4) 0.4086(3) 0.8178(3) 0.0589(16) Uani 1 1 d . . . . .
C24A C 0.2303(3) 0.4525(3) 0.7862(3) 0.0509(15) Uani 1 1 d . . . . .
Ni1B Ni 0.21480(5) 0.34700(3) 0.42968(4) 0.0528(2) Uani 1 1 d . . . . .
Cl1B Cl 0.59116(12) 0.24727(8) 0.31382(14) 0.1064(7) Uani 1 1 d . . . . .
Cl2B Cl 0.47762(13) 0.25059(8) 0.57243(12) 0.1002(6) Uani 1 1 d . . . . .
Cl3B Cl 0.08906(15) 0.51403(8) 0.31185(11) 0.1058(7) Uani 1 1 d . . . . .
Cl4B Cl 0.09075(12) 0.59786(8) 0.59405(11) 0.0966(6) Uani 1 1 d . . . . .
Si1B Si -0.07508(13) 0.23240(8) 0.28821(12) 0.0753(6) Uani 1 1 d D U . . .
Si2B Si -0.04796(14) 0.22404(10) 0.47291(12) 0.0879(7) Uani 1 1 d . . . . .
O1B O 0.3055(3) 0.29265(17) 0.4634(2) 0.0687(12) Uani 1 1 d . . . . .
O2B O 0.1470(2) 0.41122(17) 0.3992(2) 0.0601(10) Uani 1 1 d . . . . .
O3B O -0.0492(3) 0.2225(2) 0.3820(3) 0.1213(19) Uani 1 1 d . . . . .
N1B N 0.2038(3) 0.3355(2) 0.3200(3) 0.0608(13) Uani 1 1 d . . . . .
N2B N 0.2046(3) 0.3488(2) 0.5335(2) 0.0485(11) Uani 1 1 d . . . . .
C1B C 0.3668(4) 0.2820(2) 0.4281(4) 0.0606(16) Uani 1 1 d . . . . .
C2B C 0.4540(5) 0.2604(3) 0.4707(4) 0.0710(18) Uani 1 1 d . . . . .
C3B C 0.5220(4) 0.2502(3) 0.4367(5) 0.078(2) Uani 1 1 d . . . . .
H3B H 0.579634 0.237422 0.467583 0.093 Uiso 1 1 calc R U . . .
C4B C 0.5038(5) 0.2591(3) 0.3559(5) 0.078(2) Uani 1 1 d . . . . .
C5B C 0.4195(5) 0.2775(3) 0.3107(4) 0.0712(18) Uani 1 1 d . . . . .
H5B H 0.407105 0.281733 0.256065 0.085 Uiso 1 1 calc R U . . .
C6B C 0.3516(4) 0.2899(3) 0.3456(4) 0.0645(17) Uani 1 1 d . . . . .
C7B C 0.2655(4) 0.3117(3) 0.2964(4) 0.0639(17) Uani 1 1 d . . . . .
H7B H 0.253260 0.308138 0.241686 0.077 Uiso 1 1 calc R U . . .
C8B C 0.1177(4) 0.3541(3) 0.2597(3) 0.0670(17) Uani 1 1 d D . . . .
H8BA H 0.118892 0.342374 0.207445 0.080 Uiso 0.788(8) 1 calc R U P A 1
H8BB H 0.114666 0.394907 0.260014 0.080 Uiso 0.788(8) 1 calc R U P A 1
H8BC H 0.130684 0.366538 0.212024 0.080 Uiso 0.212(8) 1 calc R U P A 2
H8BD H 0.090877 0.385329 0.280186 0.080 Uiso 0.212(8) 1 calc R U P A 2
C9B C 0.0501(18) 0.3042(10) 0.2400(13) 0.070(2) Uani 0.212(8) 1 d D . P A 2
H9BA H -0.006550 0.316185 0.200440 0.084 Uiso 0.212(8) 1 calc R U P A 2
H9BB H 0.076508 0.274191 0.216721 0.084 Uiso 0.212(8) 1 calc R U P A 2
C9X C 0.0310(5) 0.3299(3) 0.2744(5) 0.070(2) Uani 0.788(8) 1 d D . P A 1
H9XA H 0.033135 0.338102 0.328689 0.084 Uiso 0.788(8) 1 calc R U P A 1
H9XB H -0.023016 0.348446 0.239151 0.084 Uiso 0.788(8) 1 calc R U P A 1
C10B C 0.0271(14) 0.2810(11) 0.3117(13) 0.070(2) Uani 0.212(8) 1 d D . P A 2
H10A H 0.015751 0.312502 0.342413 0.084 Uiso 0.212(8) 1 calc R U P A 2
H10B H 0.080557 0.260931 0.345045 0.084 Uiso 0.212(8) 1 calc R U P A 2
C10X C 0.0214(5) 0.2666(3) 0.2609(5) 0.070(2) Uani 0.788(8) 1 d D U P A 1
H10C H 0.078757 0.248838 0.291321 0.084 Uiso 0.788(8) 1 calc R U P A 1
H10D H 0.012728 0.259171 0.205059 0.084 Uiso 0.788(8) 1 calc R U P A 1
C11B C -0.0902(6) 0.1641(3) 0.2376(5) 0.145(4) Uani 1 1 d . . . . .
H11A H -0.032162 0.144625 0.251640 0.218 Uiso 1 1 calc R U . . .
H11B H -0.112195 0.169831 0.181080 0.218 Uiso 1 1 calc R U . . .
H11C H -0.134123 0.141970 0.253572 0.218 Uiso 1 1 calc R U . . .
C12B C -0.1811(4) 0.2740(3) 0.2506(5) 0.110(3) Uani 1 1 d . . . . .
H12A H -0.231573 0.253622 0.259251 0.165 Uiso 1 1 calc R U . . .
H12B H -0.193663 0.280632 0.194697 0.165 Uiso 1 1 calc R U . . .
H12C H -0.173586 0.309354 0.278227 0.165 Uiso 1 1 calc R U . . .
C13B C -0.0269(6) 0.1516(3) 0.5133(5) 0.134(3) Uani 1 1 d . . . . .
H13A H 0.029959 0.137737 0.507778 0.201 Uiso 1 1 calc R U . . .
H13B H -0.076665 0.127549 0.484542 0.201 Uiso 1 1 calc R U . . .
H13C H -0.022894 0.151958 0.568570 0.201 Uiso 1 1 calc R U . . .
C14B C -0.1586(5) 0.2508(4) 0.4805(5) 0.130(3) Uani 1 1 d . . . . .
H14A H -0.154962 0.253921 0.535519 0.196 Uiso 1 1 calc R U . . .
H14B H -0.207249 0.225154 0.454161 0.196 Uiso 1 1 calc R U . . .
H14C H -0.171216 0.287182 0.455702 0.196 Uiso 1 1 calc R U . . .
C15B C 0.0465(4) 0.2717(3) 0.5286(4) 0.0684(18) Uani 1 1 d . . . . .
H15A H 0.036975 0.308039 0.501959 0.082 Uiso 1 1 calc R U . . .
H15B H 0.040960 0.277464 0.581217 0.082 Uiso 1 1 calc R U . . .
C16B C 0.1437(4) 0.2531(2) 0.5381(3) 0.0619(16) Uani 1 1 d . . . . .
H16A H 0.148702 0.244646 0.485956 0.074 Uiso 1 1 calc R U . . .
H16B H 0.155661 0.218443 0.568887 0.074 Uiso 1 1 calc R U . . .
C17B C 0.2175(4) 0.2960(2) 0.5787(3) 0.0575(15) Uani 1 1 d . . . . .
H17A H 0.214816 0.303579 0.631837 0.069 Uiso 1 1 calc R U . . .
H17B H 0.277853 0.280630 0.583459 0.069 Uiso 1 1 calc R U . . .
C18B C 0.1765(3) 0.3917(3) 0.5643(3) 0.0523(15) Uani 1 1 d . . . . .
H18B H 0.172418 0.387194 0.615351 0.063 Uiso 1 1 calc R U . . .
C19B C 0.1511(3) 0.4454(2) 0.5277(3) 0.0470(14) Uani 1 1 d . . . . .
C20B C 0.1347(3) 0.4904(2) 0.5730(3) 0.0535(15) Uani 1 1 d . . . . .
H20B H 0.140624 0.485233 0.626512 0.064 Uiso 1 1 calc R U . . .
C21B C 0.1097(4) 0.5420(3) 0.5379(4) 0.0660(18) Uani 1 1 d . . . . .
C22B C 0.0960(4) 0.5497(3) 0.4575(4) 0.0718(19) Uani 1 1 d . . . . .
H22B H 0.078566 0.584725 0.434074 0.086 Uiso 1 1 calc R U . . .
C23B C 0.1085(4) 0.5051(3) 0.4128(4) 0.0629(17) Uani 1 1 d . . . . .
C24B C 0.1374(3) 0.4514(2) 0.4459(4) 0.0517(15) 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
Ni1A O1A 1.834(4) . ?
Ni1A O2A 1.845(4) . ?
Ni1A N1A 1.910(4) . ?
Ni1A N2A 1.895(4) . ?
Cl1A C2A 1.728(6) . ?
Cl2A C4A 1.740(6) . ?
Cl3A C23A 1.716(6) . ?
Cl4A C21A 1.738(6) . ?
Si1A O3A 1.606(4) . ?
Si1A C10A 1.848(6) . ?
Si1A C11A 1.840(6) . ?
Si1A C12A 1.859(6) . ?
Si2A O3A 1.613(4) . ?
Si2A C13A 1.849(6) . ?
Si2A C14A 1.836(6) . ?
Si2A C15A 1.873(6) . ?
O1A C1A 1.285(6) . ?
O2A C24A 1.307(6) . ?
N1A C7A 1.277(6) . ?
N1A C8A 1.469(6) . ?
N2A C17A 1.462(6) . ?
N2A C18A 1.284(6) . ?
C1A C2A 1.405(7) . ?
C1A C6A 1.431(7) . ?
C2A C3A 1.354(8) . ?
C3A H3A 0.9300 . ?
C3A C4A 1.401(8) . ?
C4A C5A 1.355(8) . ?
C5A H5A 0.9300 . ?
C5A C6A 1.371(7) . ?
C6A C7A 1.451(7) . ?
C7A H7A 0.9300 . ?
C8A H8AA 0.9700 . ?
C8A H8AB 0.9700 . ?
C8A C9A 1.528(7) . ?
C9A H9AA 0.9700 . ?
C9A H9AB 0.9700 . ?
C9A C10A 1.503(7) . ?
C10A H10E 0.9700 . ?
C10A H10F 0.9700 . ?
C11A H11D 0.9600 . ?
C11A H11E 0.9600 . ?
C11A H11F 0.9600 . ?
C12A H12D 0.9600 . ?
C12A H12E 0.9600 . ?
C12A H12F 0.9600 . ?
C13A H13D 0.9600 . ?
C13A H13E 0.9600 . ?
C13A H13F 0.9600 . ?
C14A H14D 0.9600 . ?
C14A H14E 0.9600 . ?
C14A H14F 0.9600 . ?
C15A H15C 0.9700 . ?
C15A H15D 0.9700 . ?
C15A C16A 1.503(7) . ?
C16A H16C 0.9700 . ?
C16A H16D 0.9700 . ?
C16A C17A 1.518(7) . ?
C17A H17C 0.9700 . ?
C17A H17D 0.9700 . ?
C18A H18A 0.9300 . ?
C18A C19A 1.417(7) . ?
C19A C20A 1.398(7) . ?
C19A C24A 1.404(7) . ?
C20A H20A 0.9300 . ?
C20A C21A 1.383(9) . ?
C21A C22A 1.385(9) . ?
C22A H22A 0.9300 . ?
C22A C23A 1.359(7) . ?
C23A C24A 1.428(7) . ?
Ni1B O1B 1.849(4) . ?
Ni1B O2B 1.826(4) . ?
Ni1B N1B 1.914(5) . ?
Ni1B N2B 1.890(4) . ?
Cl1B C4B 1.740(7) . ?
Cl2B C2B 1.736(7) . ?
Cl3B C23B 1.729(6) . ?
Cl4B C21B 1.733(6) . ?
Si1B O3B 1.598(5) . ?
Si1B C10B 1.878(11) . ?
Si1B C10X 1.870(7) . ?
Si1B C11B 1.830(7) . ?
Si1B C12B 1.833(7) . ?
Si2B O3B 1.602(5) . ?
Si2B C13B 1.850(8) . ?
Si2B C14B 1.847(7) . ?
Si2B C15B 1.855(6) . ?
O1B C1B 1.301(6) . ?
O2B C24B 1.299(6) . ?
N1B C7B 1.274(6) . ?
N1B C8B 1.478(6) . ?
N2B C17B 1.465(6) . ?
N2B C18B 1.288(6) . ?
C1B C2B 1.405(8) . ?
C1B C6B 1.417(8) . ?
C2B C3B 1.373(8) . ?
C3B H3B 0.9300 . ?
C3B C4B 1.384(9) . ?
C4B C5B 1.357(9) . ?
C5B H5B 0.9300 . ?
C5B C6B 1.393(8) . ?
C6B C7B 1.427(8) . ?
C7B H7B 0.9300 . ?
C8B H8BA 0.9700 . ?
C8B H8BB 0.9700 . ?
C8B H8BC 0.9700 . ?
C8B H8BD 0.9700 . ?
C8B C9B 1.536(12) . ?
C8B C9X 1.537(8) . ?
C9B H9BA 0.9700 . ?
C9B H9BB 0.9700 . ?
C9B C10B 1.519(12) . ?
C9X H9XA 0.9700 . ?
C9X H9XB 0.9700 . ?
C9X C10X 1.520(9) . ?
C10B H10A 0.9700 . ?
C10B H10B 0.9700 . ?
C10X H10C 0.9700 . ?
C10X H10D 0.9700 . ?
C11B H11A 0.9600 . ?
C11B H11B 0.9600 . ?
C11B H11C 0.9600 . ?
C12B H12A 0.9600 . ?
C12B H12B 0.9600 . ?
C12B H12C 0.9600 . ?
C13B H13A 0.9600 . ?
C13B H13B 0.9600 . ?
C13B H13C 0.9600 . ?
C14B H14A 0.9600 . ?
C14B H14B 0.9600 . ?
C14B H14C 0.9600 . ?
C15B H15A 0.9700 . ?
C15B H15B 0.9700 . ?
C15B C16B 1.506(7) . ?
C16B H16A 0.9700 . ?
C16B H16B 0.9700 . ?
C16B C17B 1.523(7) . ?
C17B H17A 0.9700 . ?
C17B H17B 0.9700 . ?
C18B H18B 0.9300 . ?
C18B C19B 1.428(7) . ?
C19B C20B 1.403(7) . ?
C19B C24B 1.401(7) . ?
C20B H20B 0.9300 . ?
C20B C21B 1.371(8) . ?
C21B C22B 1.384(8) . ?
C22B H22B 0.9300 . ?
C22B C23B 1.368(8) . ?
C23B C24B 1.413(7) . ?

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
O1A Ni1A O2A 168.96(16) . . ?
O1A Ni1A N1A 92.25(19) . . ?
O1A Ni1A N2A 88.71(19) . . ?
O2A Ni1A N1A 86.80(19) . . ?
O2A Ni1A N2A 94.09(19) . . ?
N2A Ni1A N1A 170.17(17) . . ?
O3A Si1A C10A 106.5(2) . . ?
O3A Si1A C11A 109.9(3) . . ?
O3A Si1A C12A 109.6(3) . . ?
C10A Si1A C12A 110.6(3) . . ?
C11A Si1A C10A 110.5(3) . . ?
C11A Si1A C12A 109.7(3) . . ?
O3A Si2A C13A 109.1(3) . . ?
O3A Si2A C14A 110.1(3) . . ?
O3A Si2A C15A 107.5(2) . . ?
C13A Si2A C15A 112.1(3) . . ?
C14A Si2A C13A 110.0(3) . . ?
C14A Si2A C15A 107.9(3) . . ?
C1A O1A Ni1A 124.5(4) . . ?
C24A O2A Ni1A 127.0(4) . . ?
Si1A O3A Si2A 161.7(3) . . ?
C7A N1A Ni1A 124.1(4) . . ?
C7A N1A C8A 116.6(5) . . ?
C8A N1A Ni1A 119.1(4) . . ?
C17A N2A Ni1A 118.5(3) . . ?
C18A N2A Ni1A 123.6(4) . . ?
C18A N2A C17A 117.5(5) . . ?
O1A C1A C2A 120.8(5) . . ?
O1A C1A C6A 123.5(5) . . ?
C2A C1A C6A 115.7(5) . . ?
C1A C2A Cl1A 118.1(5) . . ?
C3A C2A Cl1A 119.2(5) . . ?
C3A C2A C1A 122.8(6) . . ?
C2A C3A H3A 120.4 . . ?
C2A C3A C4A 119.2(6) . . ?
C4A C3A H3A 120.4 . . ?
C3A C4A Cl2A 118.5(5) . . ?
C5A C4A Cl2A 120.8(5) . . ?
C5A C4A C3A 120.7(6) . . ?
C4A C5A H5A 119.9 . . ?
C4A C5A C6A 120.2(6) . . ?
C6A C5A H5A 119.9 . . ?
C1A C6A C7A 118.9(5) . . ?
C5A C6A C1A 121.3(5) . . ?
C5A C6A C7A 119.7(6) . . ?
N1A C7A C6A 125.2(6) . . ?
N1A C7A H7A 117.4 . . ?
C6A C7A H7A 117.4 . . ?
N1A C8A H8AA 109.3 . . ?
N1A C8A H8AB 109.3 . . ?
N1A C8A C9A 111.6(4) . . ?
H8AA C8A H8AB 108.0 . . ?
C9A C8A H8AA 109.3 . . ?
C9A C8A H8AB 109.3 . . ?
C8A C9A H9AA 108.6 . . ?
C8A C9A H9AB 108.6 . . ?
H9AA C9A H9AB 107.6 . . ?
C10A C9A C8A 114.5(5) . . ?
C10A C9A H9AA 108.6 . . ?
C10A C9A H9AB 108.6 . . ?
Si1A C10A H10E 108.7 . . ?
Si1A C10A H10F 108.7 . . ?
C9A C10A Si1A 114.0(4) . . ?
C9A C10A H10E 108.7 . . ?
C9A C10A H10F 108.7 . . ?
H10E C10A H10F 107.6 . . ?
Si1A C11A H11D 109.5 . . ?
Si1A C11A H11E 109.5 . . ?
Si1A C11A H11F 109.5 . . ?
H11D C11A H11E 109.5 . . ?
H11D C11A H11F 109.5 . . ?
H11E C11A H11F 109.5 . . ?
Si1A C12A H12D 109.5 . . ?
Si1A C12A H12E 109.5 . . ?
Si1A C12A H12F 109.5 . . ?
H12D C12A H12E 109.5 . . ?
H12D C12A H12F 109.5 . . ?
H12E C12A H12F 109.5 . . ?
Si2A C13A H13D 109.5 . . ?
Si2A C13A H13E 109.5 . . ?
Si2A C13A H13F 109.5 . . ?
H13D C13A H13E 109.5 . . ?
H13D C13A H13F 109.5 . . ?
H13E C13A H13F 109.5 . . ?
Si2A C14A H14D 109.5 . . ?
Si2A C14A H14E 109.5 . . ?
Si2A C14A H14F 109.5 . . ?
H14D C14A H14E 109.5 . . ?
H14D C14A H14F 109.5 . . ?
H14E C14A H14F 109.5 . . ?
Si2A C15A H15C 108.2 . . ?
Si2A C15A H15D 108.2 . . ?
H15C C15A H15D 107.4 . . ?
C16A C15A Si2A 116.2(4) . . ?
C16A C15A H15C 108.2 . . ?
C16A C15A H15D 108.2 . . ?
C15A C16A H16C 108.7 . . ?
C15A C16A H16D 108.7 . . ?
C15A C16A C17A 114.3(5) . . ?
H16C C16A H16D 107.6 . . ?
C17A C16A H16C 108.7 . . ?
C17A C16A H16D 108.7 . . ?
N2A C17A C16A 110.0(4) . . ?
N2A C17A H17C 109.7 . . ?
N2A C17A H17D 109.7 . . ?
C16A C17A H17C 109.7 . . ?
C16A C17A H17D 109.7 . . ?
H17C C17A H17D 108.2 . . ?
N2A C18A H18A 116.1 . . ?
N2A C18A C19A 127.8(6) . . ?
C19A C18A H18A 116.1 . . ?
C20A C19A C18A 118.3(6) . . ?
C20A C19A C24A 121.0(6) . . ?
C24A C19A C18A 120.5(5) . . ?
C19A C20A H20A 120.5 . . ?
C21A C20A C19A 119.0(7) . . ?
C21A C20A H20A 120.5 . . ?
C20A C21A Cl4A 119.1(6) . . ?
C20A C21A C22A 121.4(6) . . ?
C22A C21A Cl4A 119.6(6) . . ?
C21A C22A H22A 120.0 . . ?
C23A C22A C21A 120.0(6) . . ?
C23A C22A H22A 120.0 . . ?
C22A C23A Cl3A 120.6(5) . . ?
C22A C23A C24A 121.3(6) . . ?
C24A C23A Cl3A 118.1(5) . . ?
O2A C24A C19A 124.0(5) . . ?
O2A C24A C23A 118.5(6) . . ?
C19A C24A C23A 117.4(5) . . ?
O1B Ni1B N1B 92.82(19) . . ?
O1B Ni1B N2B 88.94(18) . . ?
O2B Ni1B O1B 167.26(18) . . ?
O2B Ni1B N1B 87.51(19) . . ?
O2B Ni1B N2B 93.28(18) . . ?
N2B Ni1B N1B 168.44(19) . . ?
O3B Si1B C10B 86.6(7) . . ?
O3B Si1B C10X 111.8(3) . . ?
O3B Si1B C11B 109.3(4) . . ?
O3B Si1B C12B 111.1(3) . . ?
C11B Si1B C10B 128.4(10) . . ?
C11B Si1B C10X 104.3(4) . . ?
C11B Si1B C12B 109.6(4) . . ?
C12B Si1B C10B 109.2(10) . . ?
C12B Si1B C10X 110.5(4) . . ?
O3B Si2B C13B 108.2(4) . . ?
O3B Si2B C14B 110.8(3) . . ?
O3B Si2B C15B 108.1(3) . . ?
C13B Si2B C15B 110.4(3) . . ?
C14B Si2B C13B 110.1(4) . . ?
C14B Si2B C15B 109.2(3) . . ?
C1B O1B Ni1B 123.9(4) . . ?
C24B O2B Ni1B 126.1(3) . . ?
Si1B O3B Si2B 163.7(4) . . ?
C7B N1B Ni1B 123.6(4) . . ?
C7B N1B C8B 118.5(5) . . ?
C8B N1B Ni1B 117.8(4) . . ?
C17B N2B Ni1B 118.2(4) . . ?
C18B N2B Ni1B 124.6(4) . . ?
C18B N2B C17B 116.7(5) . . ?
O1B C1B C2B 121.0(6) . . ?
O1B C1B C6B 123.8(5) . . ?
C2B C1B C6B 115.2(6) . . ?
C1B C2B Cl2B 117.5(5) . . ?
C3B C2B Cl2B 119.2(6) . . ?
C3B C2B C1B 123.2(6) . . ?
C2B C3B H3B 120.4 . . ?
C2B C3B C4B 119.2(6) . . ?
C4B C3B H3B 120.4 . . ?
C3B C4B Cl1B 118.8(6) . . ?
C5B C4B Cl1B 120.7(7) . . ?
C5B C4B C3B 120.5(6) . . ?
C4B C5B H5B 119.8 . . ?
C4B C5B C6B 120.4(7) . . ?
C6B C5B H5B 119.8 . . ?
C1B C6B C7B 120.1(6) . . ?
C5B C6B C1B 121.4(6) . . ?
C5B C6B C7B 118.5(6) . . ?
N1B C7B C6B 126.5(6) . . ?
N1B C7B H7B 116.8 . . ?
C6B C7B H7B 116.8 . . ?
N1B C8B H8BA 109.0 . . ?
N1B C8B H8BB 109.0 . . ?
N1B C8B H8BC 110.0 . . ?
N1B C8B H8BD 110.0 . . ?
N1B C8B C9B 108.5(13) . . ?
N1B C8B C9X 112.7(5) . . ?
H8BA C8B H8BB 107.8 . . ?
H8BC C8B H8BD 108.4 . . ?
C9B C8B H8BC 110.0 . . ?
C9B C8B H8BD 110.0 . . ?
C9X C8B H8BA 109.0 . . ?
C9X C8B H8BB 109.0 . . ?
C8B C9B H9BA 108.8 . . ?
C8B C9B H9BB 108.8 . . ?
H9BA C9B H9BB 107.7 . . ?
C10B C9B C8B 113.7(12) . . ?
C10B C9B H9BA 108.8 . . ?
C10B C9B H9BB 108.8 . . ?
C8B C9X H9XA 109.0 . . ?
C8B C9X H9XB 109.0 . . ?
H9XA C9X H9XB 107.8 . . ?
C10X C9X C8B 112.8(6) . . ?
C10X C9X H9XA 109.0 . . ?
C10X C9X H9XB 109.0 . . ?
Si1B C10B H10A 108.4 . . ?
Si1B C10B H10B 108.4 . . ?
C9B C10B Si1B 115.4(11) . . ?
C9B C10B H10A 108.4 . . ?
C9B C10B H10B 108.4 . . ?
H10A C10B H10B 107.5 . . ?
Si1B C10X H10C 108.4 . . ?
Si1B C10X H10D 108.4 . . ?
C9X C10X Si1B 115.6(5) . . ?
C9X C10X H10C 108.4 . . ?
C9X C10X H10D 108.4 . . ?
H10C C10X H10D 107.4 . . ?
Si1B C11B H11A 109.5 . . ?
Si1B C11B H11B 109.5 . . ?
Si1B C11B H11C 109.5 . . ?
H11A C11B H11B 109.5 . . ?
H11A C11B H11C 109.5 . . ?
H11B C11B H11C 109.5 . . ?
Si1B C12B H12A 109.5 . . ?
Si1B C12B H12B 109.5 . . ?
Si1B C12B H12C 109.5 . . ?
H12A C12B H12B 109.5 . . ?
H12A C12B H12C 109.5 . . ?
H12B C12B H12C 109.5 . . ?
Si2B C13B H13A 109.5 . . ?
Si2B C13B H13B 109.5 . . ?
Si2B C13B H13C 109.5 . . ?
H13A C13B H13B 109.5 . . ?
H13A C13B H13C 109.5 . . ?
H13B C13B H13C 109.5 . . ?
Si2B C14B H14A 109.5 . . ?
Si2B C14B H14B 109.5 . . ?
Si2B C14B H14C 109.5 . . ?
H14A C14B H14B 109.5 . . ?
H14A C14B H14C 109.5 . . ?
H14B C14B H14C 109.5 . . ?
Si2B C15B H15A 108.0 . . ?
Si2B C15B H15B 108.0 . . ?
H15A C15B H15B 107.3 . . ?
C16B C15B Si2B 117.1(4) . . ?
C16B C15B H15A 108.0 . . ?
C16B C15B H15B 108.0 . . ?
C15B C16B H16A 108.6 . . ?
C15B C16B H16B 108.6 . . ?
C15B C16B C17B 114.5(5) . . ?
H16A C16B H16B 107.6 . . ?
C17B C16B H16A 108.6 . . ?
C17B C16B H16B 108.6 . . ?
N2B C17B C16B 111.2(4) . . ?
N2B C17B H17A 109.4 . . ?
N2B C17B H17B 109.4 . . ?
C16B C17B H17A 109.4 . . ?
C16B C17B H17B 109.4 . . ?
H17A C17B H17B 108.0 . . ?
N2B C18B H18B 116.9 . . ?
N2B C18B C19B 126.3(5) . . ?
C19B C18B H18B 116.9 . . ?
C20B C19B C18B 119.4(5) . . ?
C24B C19B C18B 119.4(5) . . ?
C24B C19B C20B 121.1(5) . . ?
C19B C20B H20B 120.2 . . ?
C21B C20B C19B 119.6(6) . . ?
C21B C20B H20B 120.2 . . ?
C20B C21B Cl4B 119.7(5) . . ?
C20B C21B C22B 121.0(6) . . ?
C22B C21B Cl4B 119.2(5) . . ?
C21B C22B H22B 120.4 . . ?
C23B C22B C21B 119.2(6) . . ?
C23B C22B H22B 120.4 . . ?
C22B C23B Cl3B 119.4(5) . . ?
C22B C23B C24B 122.6(6) . . ?
C24B C23B Cl3B 118.0(5) . . ?
O2B C24B C19B 124.9(5) . . ?
O2B C24B C23B 118.6(6) . . ?
C19B C24B C23B 116.5(6) . . ?

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
Ni1A O1A C1A C2A 150.5(4) . . . . ?
Ni1A O1A C1A C6A -30.6(7) . . . . ?
Ni1A O2A C24A C19A -13.5(7) . . . . ?
Ni1A O2A C24A C23A 170.0(3) . . . . ?
Ni1A N1A C7A C6A -2.5(7) . . . . ?
Ni1A N1A C8A C9A -55.2(5) . . . . ?
Ni1A N2A C17A C16A -62.9(5) . . . . ?
Ni1A N2A C18A C19A 1.3(7) . . . . ?
Cl1A C2A C3A C4A 179.1(4) . . . . ?
Cl2A C4A C5A C6A -175.5(4) . . . . ?
Cl3A C23A C24A O2A 0.2(6) . . . . ?
Cl3A C23A C24A C19A -176.5(4) . . . . ?
Cl4A C21A C22A C23A 178.5(4) . . . . ?
Si2A C15A C16A C17A 168.0(4) . . . . ?
O1A Ni1A O2A C24A -86.0(10) . . . . ?
O1A Ni1A N2A C17A -30.7(4) . . . . ?
O1A Ni1A N2A C18A 157.1(4) . . . . ?
O1A C1A C2A Cl1A 1.1(7) . . . . ?
O1A C1A C2A C3A -178.4(5) . . . . ?
O1A C1A C6A C5A -178.8(5) . . . . ?
O1A C1A C6A C7A -1.9(7) . . . . ?
O2A Ni1A O1A C1A -48.2(11) . . . . ?
O2A Ni1A N2A C17A 160.0(4) . . . . ?
O2A Ni1A N2A C18A -12.2(4) . . . . ?
O3A Si1A C10A C9A -67.3(5) . . . . ?
O3A Si2A C15A C16A -63.4(5) . . . . ?
N1A Ni1A O1A C1A 36.6(4) . . . . ?
N1A Ni1A O2A C24A -171.3(4) . . . . ?
N1A C8A C9A C10A -67.9(6) . . . . ?
N2A Ni1A O1A C1A -153.1(4) . . . . ?
N2A Ni1A O2A C24A 18.5(4) . . . . ?
N2A C18A C19A C20A -174.4(5) . . . . ?
N2A C18A C19A C24A 9.3(8) . . . . ?
C1A C2A C3A C4A -1.4(9) . . . . ?
C1A C6A C7A N1A 19.0(8) . . . . ?
C2A C1A C6A C5A 0.3(7) . . . . ?
C2A C1A C6A C7A 177.1(5) . . . . ?
C2A C3A C4A Cl2A 178.2(4) . . . . ?
C2A C3A C4A C5A -2.7(9) . . . . ?
C3A C4A C5A C6A 5.5(8) . . . . ?
C4A C5A C6A C1A -4.2(8) . . . . ?
C4A C5A C6A C7A 178.9(5) . . . . ?
C5A C6A C7A N1A -164.1(5) . . . . ?
C6A C1A C2A Cl1A -178.0(4) . . . . ?
C6A C1A C2A C3A 2.5(8) . . . . ?
C7A N1A C8A C9A 120.4(5) . . . . ?
C8A N1A C7A C6A -177.8(5) . . . . ?
C8A C9A C10A Si1A 172.7(4) . . . . ?
C10A Si1A O3A Si2A -173.7(10) . . . . ?
C11A Si1A O3A Si2A -54.0(11) . . . . ?
C11A Si1A C10A C9A 173.3(5) . . . . ?
C12A Si1A O3A Si2A 66.6(11) . . . . ?
C12A Si1A C10A C9A 51.7(5) . . . . ?
C13A Si2A O3A Si1A 61.4(11) . . . . ?
C13A Si2A C15A C16A 56.5(5) . . . . ?
C14A Si2A O3A Si1A -59.4(11) . . . . ?
C14A Si2A C15A C16A 177.8(5) . . . . ?
C15A Si2A O3A Si1A -176.8(10) . . . . ?
C15A C16A C17A N2A -63.9(6) . . . . ?
C17A N2A C18A C19A -171.0(5) . . . . ?
C18A N2A C17A C16A 109.8(5) . . . . ?
C18A C19A C20A C21A -174.7(5) . . . . ?
C18A C19A C24A O2A -2.9(8) . . . . ?
C18A C19A C24A C23A 173.6(5) . . . . ?
C19A C20A C21A Cl4A -178.7(4) . . . . ?
C19A C20A C21A C22A -0.2(9) . . . . ?
C20A C19A C24A O2A -179.1(5) . . . . ?
C20A C19A C24A C23A -2.6(7) . . . . ?
C20A C21A C22A C23A 0.0(9) . . . . ?
C21A C22A C23A Cl3A 177.7(5) . . . . ?
C21A C22A C23A C24A -1.2(9) . . . . ?
C22A C23A C24A O2A 179.1(5) . . . . ?
C22A C23A C24A C19A 2.4(8) . . . . ?
C24A C19A C20A C21A 1.6(8) . . . . ?
Ni1B O1B C1B C2B 152.0(5) . . . . ?
Ni1B O1B C1B C6B -29.2(8) . . . . ?
Ni1B O2B C24B C19B -21.8(7) . . . . ?
Ni1B O2B C24B C23B 160.0(4) . . . . ?
Ni1B N1B C7B C6B -0.1(9) . . . . ?
Ni1B N1B C8B C9B -92.2(11) . . . . ?
Ni1B N1B C8B C9X -53.1(6) . . . . ?
Ni1B N2B C17B C16B -63.2(5) . . . . ?
Ni1B N2B C18B C19B -2.1(7) . . . . ?
Cl1B C4B C5B C6B -176.4(5) . . . . ?
Cl2B C2B C3B C4B -178.7(5) . . . . ?
Cl3B C23B C24B O2B -0.7(7) . . . . ?
Cl3B C23B C24B C19B -179.1(4) . . . . ?
Cl4B C21B C22B C23B -178.2(4) . . . . ?
Si2B C15B C16B C17B 175.5(4) . . . . ?
O1B Ni1B O2B C24B -74.3(9) . . . . ?
O1B Ni1B N2B C17B -34.8(4) . . . . ?
O1B Ni1B N2B C18B 153.7(4) . . . . ?
O1B C1B C2B Cl2B -1.9(8) . . . . ?
O1B C1B C2B C3B -177.9(6) . . . . ?
O1B C1B C6B C5B -179.6(6) . . . . ?
O1B C1B C6B C7B 1.2(9) . . . . ?
O2B Ni1B O1B C1B -57.8(10) . . . . ?
O2B Ni1B N2B C17B 157.7(4) . . . . ?
O2B Ni1B N2B C18B -13.8(4) . . . . ?
O3B Si1B C10B C9B 175(2) . . . . ?
O3B Si1B C10X C9X -79.0(6) . . . . ?
O3B Si2B C15B C16B -67.0(5) . . . . ?
N1B Ni1B O1B C1B 33.4(5) . . . . ?
N1B Ni1B O2B C24B -166.1(4) . . . . ?
N1B Ni1B N2B C17B 64.1(11) . . . . ?
N1B Ni1B N2B C18B -107.4(11) . . . . ?
N1B C8B C9B C10B 59(3) . . . . ?
N1B C8B C9X C10X -68.6(8) . . . . ?
N2B Ni1B O1B C1B -158.0(5) . . . . ?
N2B Ni1B O2B C24B 25.5(4) . . . . ?
N2B C18B C19B C20B -170.9(5) . . . . ?
N2B C18B C19B C24B 13.2(8) . . . . ?
C1B C2B C3B C4B -2.8(10) . . . . ?
C1B C6B C7B N1B 14.2(10) . . . . ?
C2B C1B C6B C5B -0.7(9) . . . . ?
C2B C1B C6B C7B -179.9(5) . . . . ?
C2B C3B C4B Cl1B 178.8(5) . . . . ?
C2B C3B C4B C5B -0.4(10) . . . . ?
C3B C4B C5B C6B 2.8(10) . . . . ?
C4B C5B C6B C1B -2.3(9) . . . . ?
C4B C5B C6B C7B 177.0(6) . . . . ?
C5B C6B C7B N1B -165.0(6) . . . . ?
C6B C1B C2B Cl2B 179.2(4) . . . . ?
C6B C1B C2B C3B 3.2(9) . . . . ?
C7B N1B C8B C9B 86.2(11) . . . . ?
C7B N1B C8B C9X 125.3(6) . . . . ?
C8B N1B C7B C6B -178.4(6) . . . . ?
C8B C9B C10B Si1B 166.0(17) . . . . ?
C8B C9X C10X Si1B 173.5(5) . . . . ?
C10B Si1B O3B Si2B 104.7(17) . . . . ?
C10X Si1B O3B Si2B 119.4(14) . . . . ?
C11B Si1B O3B Si2B -125.7(14) . . . . ?
C11B Si1B C10B C9B 62(3) . . . . ?
C11B Si1B C10X C9X 163.0(6) . . . . ?
C12B Si1B O3B Si2B -4.6(15) . . . . ?
C12B Si1B C10B C9B -74(2) . . . . ?
C12B Si1B C10X C9X 45.3(7) . . . . ?
C13B Si2B O3B Si1B 136.9(14) . . . . ?
C13B Si2B C15B C16B 51.2(6) . . . . ?
C14B Si2B O3B Si1B 16.0(15) . . . . ?
C14B Si2B C15B C16B 172.5(5) . . . . ?
C15B Si2B O3B Si1B -103.6(14) . . . . ?
C15B C16B C17B N2B -60.1(6) . . . . ?
C17B N2B C18B C19B -173.7(5) . . . . ?
C18B N2B C17B C16B 109.0(5) . . . . ?
C18B C19B C20B C21B -179.6(5) . . . . ?
C18B C19B C24B O2B -0.9(8) . . . . ?
C18B C19B C24B C23B 177.4(5) . . . . ?
C19B C20B C21B Cl4B -179.2(4) . . . . ?
C19B C20B C21B C22B 3.3(8) . . . . ?
C20B C19B C24B O2B -176.7(5) . . . . ?
C20B C19B C24B C23B 1.5(7) . . . . ?
C20B C21B C22B C23B -0.6(9) . . . . ?
C21B C22B C23B Cl3B 178.6(4) . . . . ?
C21B C22B C23B C24B -1.7(9) . . . . ?
C22B C23B C24B O2B 179.6(5) . . . . ?
C22B C23B C24B C19B 1.2(8) . . . . ?
C24B C19B C20B C21B -3.8(8) . . . . ?

_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 1.204
_oxdiff_exptl_absorpt_empirical_full_min 0.878
####################################################################### 
# 
# This file contains crystal structure data downloaded from the 
# Cambridge Structural Database (CSD) hosted by the Cambridge 
# Crystallographic Data Centre (CCDC).
# 
# Full information about CCDC data access policies and citation 
# guidelines are available at http://www.ccdc.cam.ac.uk/access/V1 
# 
# Audit and citation data items may have been added by the CCDC. 
# Please retain this information to preserve the provenance of 
# this file and to allow appropriate attribution of the data. 
# 
#######################################################################

data_md_4271_mada
_database_code_depnum_ccdc_archive 'CCDC 1982363'
loop_
_audit_author_name
_audit_author_address
'Dascalu Mihaela'
;Petru Poni Institute of Macromolecular Chemistry, Iasi
Romania
;
_audit_update_record             
;
2021-08-01 deposited with the CCDC.	2021-08-20 downloaded from the CCDC.
;
_audit_creation_date             2020-02-06
_audit_creation_method           
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_shelx_SHELXL_version_number     2018/3
_chemical_name_common            ?
_chemical_name_systematic        ?
_chemical_formula_moiety         '2(C24 H30 Br4 N2 Ni O3 Si2)'
_chemical_formula_sum            'C48 H60 Br8 N4 Ni2 O6 Si4'
_chemical_formula_weight         1658.06
_chemical_melting_point          ?
_chemical_oxdiff_formula         C30H30N2Br2Si2Ni1
_chemical_oxdiff_usercomment     DS-108
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'
Br Br -0.2901 2.4595 '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'
Ni Ni 0.3393 1.1124 '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'
Si Si 0.0817 0.0704 '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      monoclinic
_space_group_IT_number           14
_space_group_name_H-M_alt        'P 1 21/c 1'
_space_group_name_Hall           '-P 2ybc'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, y+1/2, -z+1/2'
'-x, -y, -z'
'x, -y-1/2, z-1/2'

_cell_length_a                   15.4499(13)
_cell_length_b                   23.9712(14)
_cell_length_c                   17.9196(12)
_cell_angle_alpha                90
_cell_angle_beta                 109.483(8)
_cell_angle_gamma                90
_cell_volume                     6256.6(8)
_cell_formula_units_Z            4
_cell_measurement_reflns_used    5698
_cell_measurement_temperature    180.00(10)
_cell_measurement_theta_max      24.9660
_cell_measurement_theta_min      1.7290
_shelx_estimated_absorpt_T_max   0.759
_shelx_estimated_absorpt_T_min   0.388
_exptl_absorpt_coefficient_mu    5.833
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.64862
_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            'clear light brown'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   light
_exptl_crystal_colour_primary    brown
_exptl_crystal_density_diffrn    1.760
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       prism
_exptl_crystal_F_000             3264
_exptl_crystal_size_max          0.2
_exptl_crystal_size_mid          0.15
_exptl_crystal_size_min          0.05
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0666
_diffrn_reflns_av_unetI/netI     0.1490
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 1.000
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_h_min       -18
_diffrn_reflns_limit_k_max       24
_diffrn_reflns_limit_k_min       -28
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            30414
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 1.000
_diffrn_reflns_theta_full        25.027
_diffrn_reflns_theta_max         25.027
_diffrn_reflns_theta_min         1.699
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      180.00(10)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 8.0797
_diffrn_detector_type            Eos
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 1.000
_diffrn_measurement_details      
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  tₑₓₚ   ω     θ     κ     φ   Frames
#--------------------------------------------------------------------------
  1  ω    -10.00  48.00   1.00  100.00    --   17.79 -99.00 120.00   58
  2  ω    -25.00  30.00   1.00  100.00    --   17.79 -99.00  60.00   55
  3  ω    -17.00  20.00   1.00  100.00    --   17.79 -99.00 -30.00   37
  4  ω    -25.00  46.00   1.00  100.00    --   17.79 -99.00 -60.00   71
  5  ω      2.00  47.00   1.00  100.00    --   17.79  57.00-150.00   45
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'Xcalibur, Eos'
_diffrn_measurement_method       'ω scans'
_diffrn_orient_matrix_type       
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      0.0095734000
_diffrn_orient_matrix_UB_12      -0.0119678000
_diffrn_orient_matrix_UB_13      -0.0325780000
_diffrn_orient_matrix_UB_21      0.0162635000
_diffrn_orient_matrix_UB_22      -0.0245336000
_diffrn_orient_matrix_UB_23      0.0224825000
_diffrn_orient_matrix_UB_31      -0.0448846000
_diffrn_orient_matrix_UB_32      -0.0114470000
_diffrn_orient_matrix_UB_33      -0.0140180000
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_source                   'fine-focus sealed X-ray tube'
_diffrn_source_type              'Enhance (Mo) X-ray Source'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                6054
_reflns_number_total             11048
_reflns_odcompleteness_completeness 99.97
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     26.32
_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    'olex2.solve (Bourhis et al., 2015)'
_refine_diff_density_max         0.874
_refine_diff_density_min         -1.169
_refine_diff_density_rms         0.111
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.888
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     652
_refine_ls_number_reflns         11048
_refine_ls_number_restraints     3
_refine_ls_R_factor_all          0.1203
_refine_ls_R_factor_gt           0.0514
_refine_ls_restrained_S_all      0.889
_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)] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0656
_refine_ls_wR_factor_ref         0.0843
_refine_special_details          ?
_olex2_refinement_description    
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups, All C(H,H,H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Restrained distances
 C17A-C16A \\sim C17A-C16X
 with sigma of 0.01
 C16A-C15A \\sim C16X-C15X
 with sigma of 0.01
 Si2A-C15A \\sim Si2A-C15X
 with sigma of 0.01
3. Uiso/Uaniso restraints and constraints
Uiso(C15A) = Uiso(C15X) = Uiso(C16X) = Uiso(C16A)
4. Others
 Fixed Sof: H17C(0.5) H17D(0.5) H17A(0.5) H17B(0.5) C16A(0.5) H16A(0.5)
 H16B(0.5) C16X(0.5) H16C(0.5) H16D(0.5) C15A(0.5) H15A(0.5) H15B(0.5)
 C15X(0.5) H15C(0.5) H15D(0.5)
5.a Secondary CH2 refined with riding coordinates:
 C8A(H8AA,H8AB), C9A(H9AA,H9AB), C10A(H10A,H10B), C17A(H17C,H17D), C17A(H17A,
 H17B), C16A(H16A,H16B), C16X(H16C,H16D), C15A(H15A,H15B), C15X(H15C,H15D),
 C8B(H8BA,H8BB), C9B(H9BA,H9BB), C10B(H10C,H10D), C15B(H15E,H15F), C16B(H16E,
 H16F), C17B(H17E,H17F)
5.b Aromatic/amide H refined with riding coordinates:
 C18A(H18A), C3A(H3A), C5A(H5A), C7A(H7A), C20A(H20A), C22A(H22A), C3B(H3B),
 C5B(H5B), C7B(H7B), C18B(H18B), C20B(H20B), C22B(H22B)
5.c Idealised Me refined as rotating group:
 C11A(H11A,H11B,H11C), C12A(H12A,H12B,H12C), C13A(H13A,H13B,H13C), C14A(H14A,
 H14B,H14C), C11B(H11D,H11E,H11F), C12B(H12D,H12E,H12F), C13B(H13D,H13E,H13F),
 C14B(H14D,H14E,H14F)
;
_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
Br1A Br 0.08669(5) 0.59760(4) 0.59899(4) 0.0584(3) Uani 1 1 d . . . . .
Br2A Br 0.09591(6) 0.51540(4) 0.30621(4) 0.0609(3) Uani 1 1 d . . . . .
Br3A Br 0.59657(5) 0.24929(4) 0.31041(4) 0.0505(2) Uani 1 1 d . . . . .
Br4A Br 0.48668(5) 0.24972(4) 0.58133(4) 0.0498(2) Uani 1 1 d . . . . .
Ni1A Ni 0.21879(6) 0.34690(4) 0.43019(4) 0.0315(2) Uani 1 1 d . . . . .
Si1A Si -0.04091(16) 0.22436(12) 0.47483(12) 0.0574(7) Uani 1 1 d . . . . .
Si2A Si -0.07132(15) 0.23491(10) 0.29029(12) 0.0469(6) Uani 1 1 d D . . . .
O1A O 0.1523(3) 0.4110(2) 0.4006(2) 0.0394(13) Uani 1 1 d . . . . .
O3A O -0.0456(4) 0.2248(3) 0.3834(3) 0.099(3) Uani 1 1 d . . . . .
O2A O 0.3106(3) 0.2934(2) 0.4636(2) 0.0372(13) Uani 1 1 d . . . . .
N1A N 0.2102(3) 0.3483(2) 0.5336(3) 0.0316(15) Uani 1 1 d . . . . .
N2A N 0.2041(4) 0.3361(3) 0.3217(3) 0.0393(16) Uani 1 1 d . . . . .
C18A C 0.2653(5) 0.3140(3) 0.2976(4) 0.040(2) Uani 1 1 d . . . . .
H18A H 0.252376 0.312506 0.243135 0.049 Uiso 1 1 calc R . . . .
C1A C 0.1421(4) 0.4507(3) 0.4459(4) 0.0332(18) Uani 1 1 d . . . . .
C19A C 0.3523(4) 0.2911(3) 0.3459(4) 0.0335(18) Uani 1 1 d . . . . .
C2A C 0.1145(5) 0.5044(3) 0.4150(4) 0.043(2) Uani 1 1 d . . . . .
C3A C 0.0989(4) 0.5470(3) 0.4596(4) 0.044(2) Uani 1 1 d . . . . .
H3A H 0.080423 0.581754 0.436853 0.052 Uiso 1 1 calc R . . . .
C4A C 0.1109(4) 0.5381(3) 0.5396(4) 0.040(2) Uani 1 1 d . . . . .
C5A C 0.1361(4) 0.4862(3) 0.5723(4) 0.0359(19) Uani 1 1 d . . . . .
H5A H 0.141237 0.480017 0.624807 0.043 Uiso 1 1 calc R . . . .
C6A C 0.1542(4) 0.4429(3) 0.5279(4) 0.0297(17) Uani 1 1 d . . . . .
C7A C 0.1812(4) 0.3901(3) 0.5638(3) 0.0277(17) Uani 1 1 d . . . . .
H7A H 0.177661 0.385135 0.614127 0.033 Uiso 1 1 calc R . . . .
C8A C 0.2246(4) 0.2951(3) 0.5770(3) 0.0318(18) Uani 1 1 d . . . . .
H8AA H 0.225192 0.301830 0.630551 0.038 Uiso 1 1 calc R . . . .
H8AB H 0.284027 0.279969 0.580259 0.038 Uiso 1 1 calc R . . . .
C9A C 0.1504(4) 0.2524(3) 0.5375(3) 0.0372(19) Uani 1 1 d . . . . .
H9AA H 0.164577 0.217858 0.567215 0.045 Uiso 1 1 calc R . . . .
H9AB H 0.151570 0.244966 0.484680 0.045 Uiso 1 1 calc R . . . .
C10A C 0.0533(4) 0.2708(3) 0.5315(4) 0.041(2) Uani 1 1 d . . . . .
H10A H 0.042327 0.307456 0.507340 0.049 Uiso 1 1 calc R . . . .
H10B H 0.050934 0.274368 0.584663 0.049 Uiso 1 1 calc R . . . .
C11A C -0.0185(6) 0.1517(4) 0.5119(5) 0.098(4) Uani 1 1 d . . . . .
H11A H 0.036224 0.138145 0.503944 0.147 Uiso 1 1 calc GR . . . .
H11B H -0.069496 0.128483 0.483655 0.147 Uiso 1 1 calc GR . . . .
H11C H -0.010598 0.150938 0.567370 0.147 Uiso 1 1 calc GR . . . .
C12A C -0.1514(5) 0.2494(4) 0.4821(4) 0.085(3) Uani 1 1 d . . . . .
H12A H -0.149363 0.247373 0.536145 0.127 Uiso 1 1 calc GR . . . .
H12B H -0.200531 0.226373 0.449775 0.127 Uiso 1 1 calc GR . . . .
H12C H -0.161556 0.287289 0.464053 0.127 Uiso 1 1 calc GR . . . .
C13A C -0.1794(4) 0.2747(3) 0.2516(4) 0.067(3) Uani 1 1 d . . . . .
H13A H -0.229376 0.252324 0.255390 0.101 Uiso 1 1 calc GR . . . .
H13B H -0.190236 0.284182 0.197182 0.101 Uiso 1 1 calc GR . . . .
H13C H -0.174958 0.308147 0.282022 0.101 Uiso 1 1 calc GR . . . .
C14A C -0.0834(6) 0.1680(4) 0.2392(5) 0.126(5) Uani 1 1 d . . . . .
H14A H -0.023645 0.153481 0.244737 0.189 Uiso 1 1 calc GR . . . .
H14B H -0.117671 0.173067 0.184143 0.189 Uiso 1 1 calc GR . . . .
H14C H -0.115124 0.142245 0.262006 0.189 Uiso 1 1 calc GR . . . .
C17A C 0.1187(4) 0.3554(3) 0.2604(3) 0.040(2) Uani 1 1 d D . . . .
H17C H 0.131366 0.365172 0.212571 0.048 Uiso 0.5 1 calc R . P A 2
H17D H 0.095534 0.388340 0.278996 0.048 Uiso 0.5 1 calc R . P A 2
H17A H 0.118800 0.343718 0.208655 0.048 Uiso 0.5 1 calc R . P B 1
H17B H 0.116130 0.395841 0.260929 0.048 Uiso 0.5 1 calc R . P B 1
C16A C 0.0321(7) 0.3308(5) 0.2760(7) 0.034(2) Uiso 0.5 1 d D . P C 1
H16A H 0.038188 0.336907 0.331033 0.041 Uiso 0.5 1 calc R . P C 1
H16B H -0.022018 0.350734 0.243661 0.041 Uiso 0.5 1 calc R . P C 1
C16X C 0.0459(8) 0.3082(5) 0.2425(6) 0.034(2) Uiso 0.5 1 d D . P C 2
H16C H -0.011266 0.322979 0.206546 0.041 Uiso 0.5 1 calc R . P C 2
H16D H 0.065551 0.278716 0.214792 0.041 Uiso 0.5 1 calc R . P C 2
C15A C 0.0186(8) 0.2698(5) 0.2583(7) 0.034(2) Uiso 0.5 1 d D . P C 1
H15A H 0.076630 0.251004 0.283523 0.041 Uiso 0.5 1 calc R . P C 1
H15B H 0.002981 0.264746 0.201586 0.041 Uiso 0.5 1 calc R . P C 1
C15X C 0.0272(7) 0.2837(5) 0.3088(6) 0.034(2) Uiso 0.5 1 d D . P C 2
H15C H 0.017858 0.313952 0.341266 0.041 Uiso 0.5 1 calc R . P C 2
H15D H 0.082013 0.263960 0.340172 0.041 Uiso 0.5 1 calc R . P C 2
C20A C 0.4198(5) 0.2803(3) 0.3106(4) 0.0379(19) Uani 1 1 d . . . . .
H20A H 0.407652 0.286689 0.256910 0.045 Uiso 1 1 calc R . . . .
C21A C 0.5041(5) 0.2600(3) 0.3572(4) 0.0404(19) Uani 1 1 d . . . . .
C22A C 0.5228(5) 0.2511(3) 0.4373(4) 0.047(2) Uani 1 1 d . . . . .
H22A H 0.580172 0.238074 0.468418 0.056 Uiso 1 1 calc R . . . .
C23A C 0.4564(5) 0.2615(3) 0.4705(4) 0.0360(18) Uani 1 1 d . . . . .
C24A C 0.3693(5) 0.2832(3) 0.4284(4) 0.0334(18) Uani 1 1 d . . . . .
Br1B Br 0.01465(5) 0.48849(5) 0.90955(4) 0.0629(3) Uani 1 1 d . . . . .
Br2B Br 0.23145(6) 0.33308(4) 0.81302(4) 0.0552(2) Uani 1 1 d . . . . .
Br3B Br 0.33665(7) 0.62227(4) 0.50524(5) 0.0716(3) Uani 1 1 d . . . . .
Br4B Br 0.36309(6) 0.44987(4) 0.29973(4) 0.0613(3) Uani 1 1 d . . . . .
Ni1B Ni 0.34309(6) 0.48343(4) 0.69426(4) 0.0291(2) Uani 1 1 d . . . . .
Si1B Si 0.59527(14) 0.56696(10) 0.92731(11) 0.0393(6) Uani 1 1 d . . . . .
Si2B Si 0.66233(14) 0.44796(10) 0.88863(11) 0.0402(6) Uani 1 1 d . . . . .
O1B O 0.2933(3) 0.4369(2) 0.7518(2) 0.0335(12) Uani 1 1 d . . . . .
O3B O 0.6129(3) 0.5063(2) 0.8945(2) 0.0494(14) Uani 1 1 d . . . . .
O2B O 0.3721(3) 0.52669(19) 0.6217(2) 0.0368(12) Uani 1 1 d . . . . .
N1B N 0.3092(3) 0.5495(2) 0.7348(3) 0.0313(15) Uani 1 1 d . . . . .
N2B N 0.3970(3) 0.4185(2) 0.6669(3) 0.0302(14) Uani 1 1 d . . . . .
C1B C 0.2326(4) 0.4500(3) 0.7860(3) 0.0302(18) Uani 1 1 d . . . . .
C2B C 0.1916(5) 0.4068(3) 0.8178(3) 0.0354(19) Uani 1 1 d . . . . .
C3B C 0.1292(5) 0.4175(4) 0.8549(4) 0.044(2) Uani 1 1 d . . . . .
H3B H 0.103589 0.388593 0.875086 0.052 Uiso 1 1 calc R . . . .
C4B C 0.1046(5) 0.4730(4) 0.8618(3) 0.040(2) Uani 1 1 d . . . . .
C5B C 0.1426(4) 0.5174(3) 0.8332(3) 0.0343(19) Uani 1 1 d . . . . .
H5B H 0.125876 0.554044 0.838686 0.041 Uiso 1 1 calc R . . . .
C6B C 0.2070(4) 0.5049(3) 0.7957(3) 0.0313(18) Uani 1 1 d . . . . .
C7B C 0.2527(4) 0.5514(3) 0.7739(3) 0.0304(18) Uani 1 1 d . . . . .
H7B H 0.240204 0.586489 0.789868 0.037 Uiso 1 1 calc R . . . .
C8B C 0.3562(4) 0.6027(3) 0.7302(4) 0.0296(17) Uani 1 1 d . . . . .
H8BA H 0.328672 0.633044 0.750135 0.036 Uiso 1 1 calc R . . . .
H8BB H 0.349875 0.610702 0.675535 0.036 Uiso 1 1 calc R . . . .
C9B C 0.4580(4) 0.5973(3) 0.7797(3) 0.0360(18) Uani 1 1 d . . . . .
H9BA H 0.483802 0.566142 0.759760 0.043 Uiso 1 1 calc R . . . .
H9BB H 0.489631 0.630801 0.772655 0.043 Uiso 1 1 calc R . . . .
C10B C 0.4768(4) 0.5886(3) 0.8683(3) 0.0364(19) Uani 1 1 d . . . . .
H10C H 0.434524 0.560561 0.874666 0.044 Uiso 1 1 calc R . . . .
H10D H 0.463159 0.623173 0.890335 0.044 Uiso 1 1 calc R . . . .
C11B C 0.6030(5) 0.5604(4) 1.0320(3) 0.070(3) Uani 1 1 d . . . . .
H11D H 0.555220 0.536156 1.035855 0.105 Uiso 1 1 calc GR . . . .
H11E H 0.596058 0.596555 1.052459 0.105 Uiso 1 1 calc GR . . . .
H11F H 0.661694 0.545175 1.062207 0.105 Uiso 1 1 calc GR . . . .
C12B C 0.6833(4) 0.6163(3) 0.9181(4) 0.056(2) Uani 1 1 d . . . . .
H12D H 0.743286 0.602227 0.947145 0.084 Uiso 1 1 calc GR . . . .
H12E H 0.674772 0.651918 0.939002 0.084 Uiso 1 1 calc GR . . . .
H12F H 0.677470 0.620197 0.863306 0.084 Uiso 1 1 calc GR . . . .
C13B C 0.6749(5) 0.4050(3) 0.9782(3) 0.060(2) Uani 1 1 d . . . . .
H13D H 0.712833 0.424484 1.024359 0.090 Uiso 1 1 calc GR . . . .
H13E H 0.702938 0.370009 0.973781 0.090 Uiso 1 1 calc GR . . . .
H13F H 0.615526 0.398506 0.982589 0.090 Uiso 1 1 calc GR . . . .
C14B C 0.7780(4) 0.4617(4) 0.8827(4) 0.069(3) Uani 1 1 d . . . . .
H14D H 0.772700 0.486184 0.838983 0.104 Uiso 1 1 calc GR . . . .
H14E H 0.805448 0.427192 0.875185 0.104 Uiso 1 1 calc GR . . . .
H14F H 0.815813 0.478960 0.930955 0.104 Uiso 1 1 calc GR . . . .
C15B C 0.5882(4) 0.4127(3) 0.7977(3) 0.0315(17) Uani 1 1 d . . . . .
H15E H 0.577744 0.437834 0.753133 0.038 Uiso 1 1 calc R . . . .
H15F H 0.620199 0.380163 0.787795 0.038 Uiso 1 1 calc R . . . .
C16B C 0.4957(4) 0.3944(3) 0.8027(3) 0.0301(17) Uani 1 1 d . . . . .
H16E H 0.468409 0.425889 0.820636 0.036 Uiso 1 1 calc R . . . .
H16F H 0.506408 0.365402 0.842506 0.036 Uiso 1 1 calc R . . . .
C17B C 0.4266(4) 0.3726(3) 0.7253(3) 0.0330(18) Uani 1 1 d . . . . .
H17E H 0.454676 0.343128 0.704025 0.040 Uiso 1 1 calc R . . . .
H17F H 0.373655 0.357100 0.735503 0.040 Uiso 1 1 calc R . . . .
C18B C 0.4126(4) 0.4125(3) 0.6010(3) 0.0321(17) Uani 1 1 d . . . . .
H18B H 0.440062 0.379356 0.593587 0.039 Uiso 1 1 calc R . . . .
C19B C 0.3907(4) 0.4529(3) 0.5378(4) 0.0289(17) Uani 1 1 d . . . . .
C20B C 0.3915(4) 0.4356(3) 0.4648(3) 0.0276(17) Uani 1 1 d . . . . .
H20B H 0.405956 0.398840 0.457178 0.033 Uiso 1 1 calc R . . . .
C21B C 0.3705(5) 0.4734(3) 0.4027(4) 0.038(2) Uani 1 1 d . . . . .
C22B C 0.3539(5) 0.5291(4) 0.4144(4) 0.045(2) Uani 1 1 d . . . . .
H22B H 0.340737 0.554512 0.372918 0.055 Uiso 1 1 calc R . . . .
C23B C 0.3573(5) 0.5456(3) 0.4883(4) 0.0402(19) Uani 1 1 d . . . . .
C24B C 0.3732(4) 0.5085(3) 0.5535(4) 0.0346(18) 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
Br1A C4A 1.889(7) . ?
Br2A C2A 1.892(7) . ?
Br3A C21A 1.900(7) . ?
Br4A C23A 1.903(6) . ?
Ni1A O1A 1.827(5) . ?
Ni1A O2A 1.856(4) . ?
Ni1A N1A 1.901(5) . ?
Ni1A N2A 1.897(5) . ?
Si1A O3A 1.616(5) . ?
Si1A C10A 1.844(7) . ?
Si1A C11A 1.855(9) . ?
Si1A C12A 1.854(7) . ?
Si2A O3A 1.599(5) . ?
Si2A C13A 1.846(7) . ?
Si2A C14A 1.825(9) . ?
Si2A C15A 1.869(9) . ?
Si2A C15X 1.859(9) . ?
O1A C1A 1.293(8) . ?
O2A C24A 1.290(7) . ?
N1A C7A 1.288(8) . ?
N1A C8A 1.471(8) . ?
N2A C18A 1.279(8) . ?
N2A C17A 1.481(7) . ?
C18A C19A 1.442(8) . ?
C1A C2A 1.410(9) . ?
C1A C6A 1.431(8) . ?
C19A C20A 1.412(8) . ?
C19A C24A 1.425(8) . ?
C2A C3A 1.367(9) . ?
C3A C4A 1.399(9) . ?
C4A C5A 1.375(9) . ?
C5A C6A 1.392(9) . ?
C6A C7A 1.418(9) . ?
C8A C9A 1.523(8) . ?
C9A C10A 1.531(8) . ?
C17A C16A 1.570(10) . ?
C17A C16X 1.551(10) . ?
C16A C15A 1.495(11) . ?
C16X C15X 1.438(11) . ?
C20A C21A 1.380(8) . ?
C21A C22A 1.382(8) . ?
C22A C23A 1.369(9) . ?
C23A C24A 1.406(8) . ?
Br1B C4B 1.896(7) . ?
Br2B C2B 1.883(7) . ?
Br3B C23B 1.907(7) . ?
Br4B C21B 1.896(6) . ?
Ni1B O1B 1.852(4) . ?
Ni1B O2B 1.832(4) . ?
Ni1B N1B 1.889(6) . ?
Ni1B N2B 1.905(6) . ?
Si1B O3B 1.625(5) . ?
Si1B C10B 1.857(6) . ?
Si1B C11B 1.847(6) . ?
Si1B C12B 1.850(7) . ?
Si2B O3B 1.614(5) . ?
Si2B C13B 1.861(7) . ?
Si2B C14B 1.855(7) . ?
Si2B C15B 1.854(6) . ?
O1B C1B 1.317(7) . ?
O2B C24B 1.302(7) . ?
N1B C7B 1.290(7) . ?
N1B C8B 1.482(8) . ?
N2B C17B 1.482(7) . ?
N2B C18B 1.289(7) . ?
C1B C2B 1.428(9) . ?
C1B C6B 1.403(9) . ?
C2B C3B 1.365(9) . ?
C3B C4B 1.401(10) . ?
C4B C5B 1.392(10) . ?
C5B C6B 1.406(8) . ?
C6B C7B 1.440(9) . ?
C8B C9B 1.532(7) . ?
C9B C10B 1.530(7) . ?
C15B C16B 1.526(7) . ?
C16B C17B 1.534(7) . ?
C18B C19B 1.443(8) . ?
C19B C20B 1.376(8) . ?
C19B C24B 1.408(9) . ?
C20B C21B 1.388(9) . ?
C21B C22B 1.388(10) . ?
C22B C23B 1.367(8) . ?
C23B C24B 1.423(9) . ?

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
O1A Ni1A O2A 165.9(2) . . ?
O1A Ni1A N1A 93.1(2) . . ?
O1A Ni1A N2A 87.3(2) . . ?
O2A Ni1A N1A 89.5(2) . . ?
O2A Ni1A N2A 93.1(2) . . ?
N2A Ni1A N1A 167.7(2) . . ?
O3A Si1A C10A 108.3(3) . . ?
O3A Si1A C11A 108.0(4) . . ?
O3A Si1A C12A 109.8(3) . . ?
C10A Si1A C11A 110.5(3) . . ?
C10A Si1A C12A 110.0(4) . . ?
C12A Si1A C11A 110.2(4) . . ?
O3A Si2A C13A 110.5(3) . . ?
O3A Si2A C14A 109.7(4) . . ?
O3A Si2A C15A 115.9(4) . . ?
O3A Si2A C15X 90.3(4) . . ?
C13A Si2A C15A 109.0(5) . . ?
C13A Si2A C15X 109.0(5) . . ?
C14A Si2A C13A 109.7(4) . . ?
C14A Si2A C15A 101.6(5) . . ?
C14A Si2A C15X 125.7(6) . . ?
C1A O1A Ni1A 127.6(4) . . ?
Si2A O3A Si1A 166.0(5) . . ?
C24A O2A Ni1A 124.1(4) . . ?
C7A N1A Ni1A 124.7(5) . . ?
C7A N1A C8A 117.7(5) . . ?
C8A N1A Ni1A 116.9(4) . . ?
C18A N2A Ni1A 123.6(5) . . ?
C18A N2A C17A 117.1(6) . . ?
C17A N2A Ni1A 119.4(4) . . ?
N2A C18A C19A 127.0(6) . . ?
O1A C1A C2A 120.6(6) . . ?
O1A C1A C6A 123.2(7) . . ?
C2A C1A C6A 116.2(7) . . ?
C20A C19A C18A 118.7(6) . . ?
C20A C19A C24A 122.1(6) . . ?
C24A C19A C18A 119.0(6) . . ?
C1A C2A Br2A 117.0(6) . . ?
C3A C2A Br2A 120.1(6) . . ?
C3A C2A C1A 122.8(6) . . ?
C2A C3A C4A 119.8(7) . . ?
C3A C4A Br1A 118.7(6) . . ?
C5A C4A Br1A 121.6(6) . . ?
C5A C4A C3A 119.7(7) . . ?
C4A C5A C6A 121.0(6) . . ?
C5A C6A C1A 120.5(6) . . ?
C5A C6A C7A 119.5(6) . . ?
C7A C6A C1A 120.0(6) . . ?
N1A C7A C6A 126.6(6) . . ?
N1A C8A C9A 112.2(5) . . ?
C8A C9A C10A 114.1(6) . . ?
C9A C10A Si1A 116.2(5) . . ?
N2A C17A C16A 110.6(7) . . ?
N2A C17A C16X 109.3(7) . . ?
C15A C16A C17A 113.3(8) . . ?
C15X C16X C17A 117.3(8) . . ?
C16A C15A Si2A 115.9(7) . . ?
C16X C15X Si2A 119.2(7) . . ?
C21A C20A C19A 118.8(6) . . ?
C20A C21A Br3A 118.5(5) . . ?
C20A C21A C22A 120.7(7) . . ?
C22A C21A Br3A 120.7(6) . . ?
C23A C22A C21A 119.7(7) . . ?
C22A C23A Br4A 117.9(5) . . ?
C22A C23A C24A 123.8(6) . . ?
C24A C23A Br4A 118.2(5) . . ?
O2A C24A C19A 124.5(6) . . ?
O2A C24A C23A 120.8(6) . . ?
C23A C24A C19A 114.7(6) . . ?
O1B Ni1B N1B 94.1(2) . . ?
O1B Ni1B N2B 87.2(2) . . ?
O2B Ni1B O1B 169.03(18) . . ?
O2B Ni1B N1B 87.9(2) . . ?
O2B Ni1B N2B 92.8(2) . . ?
N1B Ni1B N2B 170.3(2) . . ?
O3B Si1B C10B 107.2(3) . . ?
O3B Si1B C11B 109.3(3) . . ?
O3B Si1B C12B 108.8(3) . . ?
C11B Si1B C10B 108.6(3) . . ?
C11B Si1B C12B 110.2(3) . . ?
C12B Si1B C10B 112.7(3) . . ?
O3B Si2B C13B 109.8(3) . . ?
O3B Si2B C14B 109.6(4) . . ?
O3B Si2B C15B 106.6(3) . . ?
C14B Si2B C13B 108.8(3) . . ?
C15B Si2B C13B 111.2(3) . . ?
C15B Si2B C14B 110.8(3) . . ?
C1B O1B Ni1B 127.4(5) . . ?
Si2B O3B Si1B 159.9(3) . . ?
C24B O2B Ni1B 124.0(5) . . ?
C7B N1B Ni1B 124.2(5) . . ?
C7B N1B C8B 115.8(6) . . ?
C8B N1B Ni1B 119.7(4) . . ?
C17B N2B Ni1B 118.9(4) . . ?
C18B N2B Ni1B 124.0(5) . . ?
C18B N2B C17B 117.1(6) . . ?
O1B C1B C2B 119.5(7) . . ?
O1B C1B C6B 123.7(7) . . ?
C6B C1B C2B 116.8(7) . . ?
C1B C2B Br2B 117.8(5) . . ?
C3B C2B Br2B 119.6(6) . . ?
C3B C2B C1B 122.5(7) . . ?
C2B C3B C4B 118.6(8) . . ?
C3B C4B Br1B 119.2(6) . . ?
C5B C4B Br1B 118.6(6) . . ?
C5B C4B C3B 122.2(7) . . ?
C4B C5B C6B 117.8(7) . . ?
C1B C6B C5B 122.2(7) . . ?
C1B C6B C7B 120.5(6) . . ?
C5B C6B C7B 117.1(7) . . ?
N1B C7B C6B 127.1(7) . . ?
N1B C8B C9B 108.8(5) . . ?
C10B C9B C8B 114.6(5) . . ?
C9B C10B Si1B 116.0(4) . . ?
C16B C15B Si2B 113.2(4) . . ?
C15B C16B C17B 115.3(5) . . ?
N2B C17B C16B 110.1(5) . . ?
N2B C18B C19B 125.2(7) . . ?
C20B C19B C18B 118.0(7) . . ?
C20B C19B C24B 122.7(6) . . ?
C24B C19B C18B 119.3(6) . . ?
C19B C20B C21B 119.5(7) . . ?
C20B C21B Br4B 120.6(6) . . ?
C20B C21B C22B 120.8(6) . . ?
C22B C21B Br4B 118.6(6) . . ?
C23B C22B C21B 118.4(7) . . ?
C22B C23B Br3B 118.6(6) . . ?
C22B C23B C24B 123.7(7) . . ?
C24B C23B Br3B 117.6(5) . . ?
O2B C24B C19B 124.6(6) . . ?
O2B C24B C23B 120.6(7) . . ?
C19B C24B C23B 114.8(6) . . ?

_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 1.339
_oxdiff_exptl_absorpt_empirical_full_min 0.754
####################################################################### 
# 
# This file contains crystal structure data downloaded from the 
# Cambridge Structural Database (CSD) hosted by the Cambridge 
# Crystallographic Data Centre (CCDC).
# 
# Full information about CCDC data access policies and citation 
# guidelines are available at http://www.ccdc.cam.ac.uk/access/V1 
# 
# Audit and citation data items may have been added by the CCDC. 
# Please retain this information to preserve the provenance of 
# this file and to allow appropriate attribution of the data. 
# 
#######################################################################

data_md_4171_mada
_database_code_depnum_ccdc_archive 'CCDC 1982359'
loop_
_audit_author_name
_audit_author_address
'Dascalu Mihaela'
;Petru Poni Institute of Macromolecular Chemistry, Iasi
Romania
;
_audit_update_record             
;
2021-08-01 deposited with the CCDC.	2021-08-20 downloaded from the CCDC.
;
_audit_creation_date             2020-02-06
_audit_creation_method           
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_shelx_SHELXL_version_number     2018/3
_chemical_name_common            ?
_chemical_name_systematic        ?
_chemical_formula_moiety         '2(C24 H30 Cl4 Cu N2 O3 Si2), C H2 Cl2'
_chemical_formula_sum            'C49 H62 Cl10 Cu2 N4 O6 Si4'
_chemical_formula_weight         1396.96
_chemical_melting_point          ?
_chemical_oxdiff_formula         C17H34N4O3Cl2Si2Mn1
_chemical_oxdiff_usercomment     DS22
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'
Cu Cu 0.3201 1.2651 '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'
Si Si 0.0817 0.0704 '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      monoclinic
_space_group_IT_number           14
_space_group_name_H-M_alt        'P 1 21/c 1'
_space_group_name_Hall           '-P 2ybc'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, y+1/2, -z+1/2'
'-x, -y, -z'
'x, -y-1/2, z-1/2'

_cell_length_a                   20.1918(12)
_cell_length_b                   12.5700(9)
_cell_length_c                   26.0592(14)
_cell_angle_alpha                90
_cell_angle_beta                 103.639(6)
_cell_angle_gamma                90
_cell_volume                     6427.6(7)
_cell_formula_units_Z            4
_cell_measurement_reflns_used    6121
_cell_measurement_temperature    180.05(10)
_cell_measurement_theta_max      26.9810
_cell_measurement_theta_min      1.9860
_shelx_estimated_absorpt_T_max   0.943
_shelx_estimated_absorpt_T_min   0.533
_exptl_absorpt_coefficient_mu    1.198
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.51934
_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            'clear light brown'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   light
_exptl_crystal_colour_primary    brown
_exptl_crystal_density_diffrn    1.444
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       prism
_exptl_crystal_F_000             2864
_exptl_crystal_size_max          0.6
_exptl_crystal_size_mid          0.15
_exptl_crystal_size_min          0.05
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0558
_diffrn_reflns_av_unetI/netI     0.1009
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_limit_h_max       24
_diffrn_reflns_limit_h_min       -22
_diffrn_reflns_limit_k_max       10
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       29
_diffrn_reflns_limit_l_min       -31
_diffrn_reflns_number            31162
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_theta_full        25.027
_diffrn_reflns_theta_max         25.027
_diffrn_reflns_theta_min         1.608
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      180.05(10)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 8.0797
_diffrn_detector_type            Eos
_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      0.00  89.00   1.00  150.00    --   17.79  19.00   0.00   89
  2  ω      5.00  74.00   1.00  150.00    --   17.79  57.00 -90.00   69
  3  ω      1.00  36.00   1.00  150.00    --   17.79  57.00-150.00   35
  4  ω    -18.00  10.00   1.00  150.00    --  -15.60 -99.00 -60.00   28
  5  ω     65.00  90.00   1.00  150.00    --   17.79-178.00-180.00   25
  6  ω     61.00  90.00   1.00  150.00    --   17.79-178.00 -30.00   29
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'Xcalibur, Eos'
_diffrn_measurement_method       'ω scans'
_diffrn_orient_matrix_type       
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      -0.0333977000
_diffrn_orient_matrix_UB_12      -0.0200923000
_diffrn_orient_matrix_UB_13      -0.0099513000
_diffrn_orient_matrix_UB_21      0.0131014000
_diffrn_orient_matrix_UB_22      -0.0525501000
_diffrn_orient_matrix_UB_23      0.0016261000
_diffrn_orient_matrix_UB_31      -0.0044084000
_diffrn_orient_matrix_UB_32      -0.0043479000
_diffrn_orient_matrix_UB_33      0.0261304000
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_source                   'fine-focus sealed X-ray tube'
_diffrn_source_type              'Enhance (Mo) X-ray Source'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                7496
_reflns_number_total             11343
_reflns_odcompleteness_completeness 99.96
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     26.32
_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    'olex2.solve (Bourhis et al., 2015)'
_refine_diff_density_max         0.770
_refine_diff_density_min         -0.887
_refine_diff_density_rms         0.081
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.039
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     686
_refine_ls_number_reflns         11343
_refine_ls_number_restraints     2
_refine_ls_R_factor_all          0.1042
_refine_ls_R_factor_gt           0.0598
_refine_ls_restrained_S_all      1.039
_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)+(0.0381P)²] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1066
_refine_ls_wR_factor_ref         0.1239
_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
 Cl2-C1X \\sim Cl2-C1
 with sigma of 0.01
 Cl1X-C1X \\sim Cl1-C1
 with sigma of 0.01
3. Uiso/Uaniso restraints and constraints
Uanis(Cl1) = Uanis(Cl1X)
Uiso(C1X) = Uiso(C1)
4. Others
 Sof(Cl1X)=Sof(C1X)=Sof(H1XA)=Sof(H1XB)=1-FVAR(1)
 Sof(Cl1)=Sof(C1)=Sof(H1A)=Sof(H1B)=FVAR(1)
5.a Secondary CH2 refined with riding coordinates:
 C8A(H8AA,H8AB), C9A(H9AA,H9AB), C10A(H10A,H10B), C15A(H15A,H15B), C16A(H16A,
 H16B), C17A(H17A,H17B), C8B(H8BA,H8BB), C9B(H9BA,H9BB), C10B(H10C,H10D),
 C15B(H15C,H15D), C16B(H16C,H16D), C17B(H17C,H17D), C1(H1A,H1B), C1X(H1XA,H1XB)
5.b Aromatic/amide H refined with riding coordinates:
 C3A(H3A), C5A(H5A), C7A(H7A), C18A(H18A), C20A(H20A), C22A(H22A), C3B(H3B),
 C5B(H5B), C7B(H7B), C18B(H18B), C20B(H20B), C22B(H22B)
5.c Idealised Me refined as rotating group:
 C11A(H11A,H11B,H11C), C12A(H12A,H12B,H12C), C13A(H13A,H13B,H13C), C14A(H14A,
 H14B,H14C), C11B(H11D,H11E,H11F), C12B(H12D,H12E,H12F), C13B(H13D,H13E,H13F),
 C14B(H14D,H14E,H14F)
;
_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
Cu1A Cu 0.78884(3) 0.63237(5) 0.54072(2) 0.03060(17) Uani 1 1 d . . . . .
Cl1A Cl 0.66514(6) 0.80328(12) 0.65003(5) 0.0441(4) Uani 1 1 d . . . . .
Cl2A Cl 0.88445(8) 1.03857(14) 0.74020(5) 0.0652(5) Uani 1 1 d . . . . .
Cl3A Cl 0.89198(7) 0.58236(14) 0.39660(5) 0.0558(4) Uani 1 1 d . . . . .
Cl4A Cl 0.64693(7) 0.50243(12) 0.26750(4) 0.0457(4) Uani 1 1 d . . . . .
Si1A Si 0.91564(7) 0.33380(13) 0.66111(5) 0.0370(4) Uani 1 1 d . . . . .
Si2A Si 0.76113(7) 0.25955(13) 0.61739(5) 0.0378(4) Uani 1 1 d . . . . .
O1A O 0.75540(15) 0.7074(3) 0.59233(12) 0.0373(9) Uani 1 1 d . . . . .
O2A O 0.81627(14) 0.5948(3) 0.47837(11) 0.0347(9) Uani 1 1 d . . . . .
O3A O 0.83510(16) 0.3170(3) 0.63641(14) 0.0513(10) Uani 1 1 d . . . . .
N1A N 0.88392(18) 0.6646(3) 0.57586(14) 0.0321(10) Uani 1 1 d . . . . .
N2A N 0.69897(17) 0.5679(3) 0.51542(13) 0.0261(9) Uani 1 1 d . . . . .
C1A C 0.7863(2) 0.7783(4) 0.62488(17) 0.0297(12) Uani 1 1 d . . . . .
C2A C 0.7496(2) 0.8375(4) 0.65521(16) 0.0304(12) Uani 1 1 d . . . . .
C3A C 0.7788(3) 0.9175(4) 0.68903(18) 0.0404(14) Uani 1 1 d . . . . .
H3A H 0.752509 0.956814 0.707096 0.049 Uiso 1 1 calc R . . . .
C4A C 0.8478(3) 0.9391(4) 0.69602(17) 0.0386(14) Uani 1 1 d . . . . .
C5A C 0.8865(3) 0.8820(4) 0.66928(17) 0.0369(13) Uani 1 1 d . . . . .
H5A H 0.932695 0.896763 0.674486 0.044 Uiso 1 1 calc R . . . .
C6A C 0.8570(2) 0.8008(4) 0.63390(17) 0.0330(13) Uani 1 1 d . . . . .
C7A C 0.9016(2) 0.7353(4) 0.61137(17) 0.0335(13) Uani 1 1 d . . . . .
H7A H 0.948157 0.745993 0.624139 0.040 Uiso 1 1 calc R . . . .
C8A C 0.9374(2) 0.5965(4) 0.56354(18) 0.0366(14) Uani 1 1 d . . . . .
H8AA H 0.981825 0.622113 0.582216 0.044 Uiso 1 1 calc R . . . .
H8AB H 0.935091 0.599273 0.525964 0.044 Uiso 1 1 calc R . . . .
C9A C 0.9278(2) 0.4830(4) 0.57975(18) 0.0351(13) Uani 1 1 d . . . . .
H9AA H 0.959731 0.437840 0.567385 0.042 Uiso 1 1 calc R . . . .
H9AB H 0.882157 0.459992 0.562293 0.042 Uiso 1 1 calc R . . . .
C10A C 0.9379(2) 0.4667(4) 0.63974(17) 0.0385(14) Uani 1 1 d . . . . .
H10A H 0.910642 0.519247 0.652731 0.046 Uiso 1 1 calc R . . . .
H10B H 0.985251 0.480751 0.656505 0.046 Uiso 1 1 calc R . . . .
C11A C 0.9332(3) 0.3330(6) 0.73450(19) 0.075(2) Uani 1 1 d . . . . .
H11A H 0.915794 0.268571 0.746114 0.113 Uiso 1 1 calc GR . . . .
H11B H 0.911289 0.393072 0.746238 0.113 Uiso 1 1 calc GR . . . .
H11C H 0.981428 0.337120 0.748991 0.113 Uiso 1 1 calc GR . . . .
C12A C 0.9638(3) 0.2272(5) 0.6371(2) 0.0663(19) Uani 1 1 d . . . . .
H12A H 0.953314 0.228088 0.599203 0.099 Uiso 1 1 calc GR . . . .
H12B H 0.951387 0.159515 0.649078 0.099 Uiso 1 1 calc GR . . . .
H12C H 1.011791 0.238699 0.650557 0.099 Uiso 1 1 calc GR . . . .
C13A C 0.7260(3) 0.2343(5) 0.6762(2) 0.0582(18) Uani 1 1 d . . . . .
H13A H 0.716374 0.300897 0.690981 0.087 Uiso 1 1 calc GR . . . .
H13B H 0.758665 0.195326 0.702126 0.087 Uiso 1 1 calc GR . . . .
H13C H 0.684715 0.193637 0.665861 0.087 Uiso 1 1 calc GR . . . .
C14A C 0.7694(3) 0.1333(5) 0.5825(2) 0.0548(16) Uani 1 1 d . . . . .
H14A H 0.801319 0.087501 0.605375 0.082 Uiso 1 1 calc GR . . . .
H14B H 0.785369 0.148345 0.551340 0.082 Uiso 1 1 calc GR . . . .
H14C H 0.725819 0.098865 0.572687 0.082 Uiso 1 1 calc GR . . . .
C15A C 0.7067(2) 0.3533(4) 0.57117(18) 0.0342(13) Uani 1 1 d . . . . .
H15A H 0.726526 0.363727 0.541093 0.041 Uiso 1 1 calc R . . . .
H15B H 0.662283 0.320771 0.558240 0.041 Uiso 1 1 calc R . . . .
C16A C 0.6967(2) 0.4616(4) 0.59421(17) 0.0327(13) Uani 1 1 d . . . . .
H16A H 0.741059 0.490939 0.610511 0.039 Uiso 1 1 calc R . . . .
H16B H 0.672260 0.451927 0.621788 0.039 Uiso 1 1 calc R . . . .
C17A C 0.6579(2) 0.5420(4) 0.55441(17) 0.0311(12) Uani 1 1 d . . . . .
H17A H 0.614289 0.512475 0.536294 0.037 Uiso 1 1 calc R . . . .
H17B H 0.649630 0.606148 0.572577 0.037 Uiso 1 1 calc R . . . .
C18A C 0.6726(2) 0.5446(4) 0.46693(17) 0.0262(11) Uani 1 1 d . . . . .
H18A H 0.628022 0.519686 0.458757 0.031 Uiso 1 1 calc R . . . .
C19A C 0.7063(2) 0.5539(4) 0.42384(16) 0.0232(11) Uani 1 1 d . . . . .
C20A C 0.6667(2) 0.5350(4) 0.37259(16) 0.0295(12) Uani 1 1 d . . . . .
H20A H 0.619980 0.524761 0.367149 0.035 Uiso 1 1 calc R . . . .
C21A C 0.6966(2) 0.5315(4) 0.33073(17) 0.0320(12) Uani 1 1 d . . . . .
C22A C 0.7661(2) 0.5464(4) 0.33762(18) 0.0354(13) Uani 1 1 d . . . . .
H22A H 0.786256 0.542781 0.309033 0.043 Uiso 1 1 calc R . . . .
C23A C 0.8047(2) 0.5667(4) 0.38750(18) 0.0329(13) Uani 1 1 d . . . . .
C24A C 0.7763(2) 0.5737(4) 0.43238(18) 0.0296(12) Uani 1 1 d . . . . .
Cu1B Cu 0.59765(3) 0.04237(5) 0.38219(2) 0.02788(16) Uani 1 1 d . . . . .
Cl1B Cl 0.50645(7) 0.30918(11) 0.47363(5) 0.0464(4) Uani 1 1 d . . . . .
Cl2B Cl 0.55107(7) 0.06997(14) 0.64957(4) 0.0537(4) Uani 1 1 d . . . . .
Cl3B Cl 0.57533(7) -0.23838(11) 0.25978(5) 0.0486(4) Uani 1 1 d . . . . .
Cl4B Cl 0.51300(6) 0.04052(12) 0.09826(4) 0.0406(4) Uani 1 1 d . . . . .
Si1B Si 0.85576(7) -0.03723(14) 0.46319(6) 0.0417(4) Uani 1 1 d . . . . .
Si2B Si 0.84009(8) 0.19510(14) 0.41463(5) 0.0420(4) Uani 1 1 d . . . . .
O1B O 0.56443(15) 0.1310(3) 0.42941(11) 0.0318(8) Uani 1 1 d . . . . .
O2B O 0.60188(16) -0.0494(3) 0.32491(11) 0.0329(8) Uani 1 1 d . . . . .
O3B O 0.83109(17) 0.0806(3) 0.44117(13) 0.0486(10) Uani 1 1 d . . . . .
N1B N 0.62323(18) -0.0724(3) 0.43469(14) 0.0269(9) Uani 1 1 d . . . . .
N2B N 0.60585(18) 0.1692(3) 0.33966(13) 0.0274(9) Uani 1 1 d . . . . .
C1B C 0.5639(2) 0.1142(4) 0.47838(17) 0.0261(11) Uani 1 1 d . . . . .
C2B C 0.5365(2) 0.1934(4) 0.50658(17) 0.0297(12) Uani 1 1 d . . . . .
C3B C 0.5341(2) 0.1805(4) 0.55854(17) 0.0347(13) Uani 1 1 d . . . . .
H3B H 0.516994 0.234514 0.576149 0.042 Uiso 1 1 calc R . . . .
C4B C 0.5573(2) 0.0866(5) 0.58445(17) 0.0344(14) Uani 1 1 d . . . . .
C5B C 0.5834(2) 0.0069(4) 0.55932(18) 0.0367(14) Uani 1 1 d . . . . .
H5B H 0.598770 -0.055670 0.577261 0.044 Uiso 1 1 calc R . . . .
C6B C 0.5872(2) 0.0194(4) 0.50635(17) 0.0268(12) Uani 1 1 d . . . . .
C7B C 0.6151(2) -0.0675(4) 0.48230(18) 0.0304(12) Uani 1 1 d . . . . .
H7B H 0.628780 -0.126866 0.503447 0.036 Uiso 1 1 calc R . . . .
C8B C 0.6577(2) -0.1676(4) 0.4201(2) 0.0367(13) Uani 1 1 d . . . . .
H8BA H 0.632094 -0.195106 0.386488 0.044 Uiso 1 1 calc R . . . .
H8BB H 0.659698 -0.222590 0.446574 0.044 Uiso 1 1 calc R . . . .
C9B C 0.7293(2) -0.1386(4) 0.41622(18) 0.0364(13) Uani 1 1 d . . . . .
H9BA H 0.726598 -0.079022 0.392138 0.044 Uiso 1 1 calc R . . . .
H9BB H 0.748567 -0.198299 0.401187 0.044 Uiso 1 1 calc R . . . .
C10B C 0.7778(2) -0.1088(4) 0.46930(18) 0.0378(13) Uani 1 1 d . . . . .
H10C H 0.791097 -0.173348 0.489477 0.045 Uiso 1 1 calc R . . . .
H10D H 0.753176 -0.064620 0.489081 0.045 Uiso 1 1 calc R . . . .
C11B C 0.9160(3) -0.0247(5) 0.5284(2) 0.065(2) Uani 1 1 d . . . . .
H11D H 0.949747 0.028101 0.526512 0.097 Uiso 1 1 calc GR . . . .
H11E H 0.937978 -0.091844 0.538254 0.097 Uiso 1 1 calc GR . . . .
H11F H 0.891675 -0.003760 0.554250 0.097 Uiso 1 1 calc GR . . . .
C12B C 0.8971(3) -0.1054(6) 0.4160(2) 0.078(2) Uani 1 1 d . . . . .
H12D H 0.865834 -0.109149 0.382019 0.117 Uiso 1 1 calc GR . . . .
H12E H 0.910118 -0.175973 0.428426 0.117 Uiso 1 1 calc GR . . . .
H12F H 0.936922 -0.066259 0.413054 0.117 Uiso 1 1 calc GR . . . .
C13B C 0.9031(3) 0.1824(6) 0.3728(2) 0.070(2) Uani 1 1 d . . . . .
H13D H 0.947007 0.164801 0.394649 0.105 Uiso 1 1 calc GR . . . .
H13E H 0.906004 0.248684 0.355086 0.105 Uiso 1 1 calc GR . . . .
H13F H 0.888710 0.127347 0.347042 0.105 Uiso 1 1 calc GR . . . .
C14B C 0.8707(3) 0.2921(5) 0.4682(2) 0.0680(19) Uani 1 1 d . . . . .
H14D H 0.838644 0.296428 0.490069 0.102 Uiso 1 1 calc GR . . . .
H14E H 0.875318 0.360716 0.453240 0.102 Uiso 1 1 calc GR . . . .
H14F H 0.914173 0.269569 0.489149 0.102 Uiso 1 1 calc GR . . . .
C15B C 0.7559(2) 0.2336(4) 0.37364(17) 0.0406(14) Uani 1 1 d . . . . .
H15C H 0.761477 0.297804 0.354399 0.049 Uiso 1 1 calc R . . . .
H15D H 0.740406 0.177961 0.347841 0.049 Uiso 1 1 calc R . . . .
C16B C 0.7005(2) 0.2535(4) 0.40339(17) 0.0376(13) Uani 1 1 d . . . . .
H16C H 0.699626 0.194015 0.426914 0.045 Uiso 1 1 calc R . . . .
H16D H 0.712330 0.316644 0.425023 0.045 Uiso 1 1 calc R . . . .
C17B C 0.6293(2) 0.2682(4) 0.36817(17) 0.0355(13) Uani 1 1 d . . . . .
H17C H 0.598019 0.288319 0.389576 0.043 Uiso 1 1 calc R . . . .
H17D H 0.629956 0.324916 0.343039 0.043 Uiso 1 1 calc R . . . .
C18B C 0.5933(2) 0.1697(4) 0.28907(17) 0.0293(12) Uani 1 1 d . . . . .
H18B H 0.596282 0.234893 0.272886 0.035 Uiso 1 1 calc R . . . .
C19B C 0.5751(2) 0.0794(4) 0.25513(17) 0.0265(11) Uani 1 1 d . . . . .
C20B C 0.5540(2) 0.0986(4) 0.20061(17) 0.0311(12) Uani 1 1 d . . . . .
H20B H 0.549843 0.167918 0.187825 0.037 Uiso 1 1 calc R . . . .
C21B C 0.5394(2) 0.0144(4) 0.16639(17) 0.0295(12) Uani 1 1 d . . . . .
C22B C 0.5450(2) -0.0895(4) 0.18362(18) 0.0329(13) Uani 1 1 d . . . . .
H22B H 0.535004 -0.145488 0.159739 0.039 Uiso 1 1 calc R . . . .
C23B C 0.5659(2) -0.1086(4) 0.23741(18) 0.0306(12) Uani 1 1 d . . . . .
C24B C 0.5813(2) -0.0255(4) 0.27499(18) 0.0270(12) Uani 1 1 d . . . . .
Cl1 Cl 0.8574(4) -0.1464(6) 0.2540(3) 0.1388(19) Uani 0.462(4) 1 d D . P A 1
Cl1X Cl 0.8228(3) -0.2037(5) 0.2780(2) 0.1388(19) Uani 0.538(4) 1 d D . P A 2
Cl2 Cl 0.75729(13) 0.0012(2) 0.26502(11) 0.1451(10) Uani 1 1 d D . . . .
C1 C 0.7730(7) -0.1035(11) 0.2350(5) 0.089(4) Uiso 0.462(4) 1 d D . P A 1
H1A H 0.761842 -0.089591 0.197358 0.106 Uiso 0.462(4) 1 calc R . P A 1
H1B H 0.743548 -0.160351 0.241508 0.106 Uiso 0.462(4) 1 calc R . P A 1
C1X C 0.7491(6) -0.1276(9) 0.2642(5) 0.089(4) Uiso 0.538(4) 1 d D . P A 2
H1XA H 0.722601 -0.147917 0.229493 0.106 Uiso 0.538(4) 1 calc R . P A 2
H1XB H 0.722646 -0.146613 0.289405 0.106 Uiso 0.538(4) 1 calc R . P A 2


_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
Cu1A O1A 1.893(3) . ?
Cu1A O2A 1.896(3) . ?
Cu1A N1A 1.965(4) . ?
Cu1A N2A 1.955(4) . ?
Cl1A C2A 1.733(5) . ?
Cl2A C4A 1.742(5) . ?
Cl3A C23A 1.734(5) . ?
Cl4A C21A 1.754(5) . ?
Si1A O3A 1.616(3) . ?
Si1A C10A 1.849(5) . ?
Si1A C11A 1.861(5) . ?
Si1A C12A 1.849(5) . ?
Si2A O3A 1.627(4) . ?
Si2A C13A 1.862(5) . ?
Si2A C14A 1.856(6) . ?
Si2A C15A 1.850(5) . ?
O1A C1A 1.285(5) . ?
O2A C24A 1.305(5) . ?
N1A C7A 1.272(6) . ?
N1A C8A 1.471(6) . ?
N2A C17A 1.490(5) . ?
N2A C18A 1.283(5) . ?
C1A C2A 1.415(6) . ?
C1A C6A 1.420(6) . ?
C2A C3A 1.375(7) . ?
C3A C4A 1.389(7) . ?
C4A C5A 1.367(6) . ?
C5A C6A 1.409(6) . ?
C6A C7A 1.444(6) . ?
C8A C9A 1.513(7) . ?
C9A C10A 1.542(6) . ?
C15A C16A 1.520(7) . ?
C16A C17A 1.525(6) . ?
C18A C19A 1.448(5) . ?
C19A C20A 1.406(6) . ?
C19A C24A 1.400(6) . ?
C20A C21A 1.366(6) . ?
C21A C22A 1.385(6) . ?
C22A C23A 1.372(6) . ?
C23A C24A 1.421(6) . ?
Cu1B O1B 1.896(3) . ?
Cu1B O2B 1.905(3) . ?
Cu1B N1B 1.971(4) . ?
Cu1B N2B 1.971(4) . ?
Cl1B C2B 1.726(5) . ?
Cl2B C4B 1.743(4) . ?
Cl3B C23B 1.728(5) . ?
Cl4B C21B 1.760(4) . ?
Si1B O3B 1.623(4) . ?
Si1B C10B 1.853(5) . ?
Si1B C11B 1.849(5) . ?
Si1B C12B 1.852(5) . ?
Si2B O3B 1.626(4) . ?
Si2B C13B 1.868(5) . ?
Si2B C14B 1.847(6) . ?
Si2B C15B 1.846(5) . ?
O1B C1B 1.296(5) . ?
O2B C24B 1.304(5) . ?
N1B C7B 1.291(5) . ?
N1B C8B 1.478(6) . ?
N2B C17B 1.470(6) . ?
N2B C18B 1.282(5) . ?
C1B C2B 1.423(6) . ?
C1B C6B 1.418(6) . ?
C2B C3B 1.376(6) . ?
C3B C4B 1.386(7) . ?
C4B C5B 1.369(7) . ?
C5B C6B 1.409(6) . ?
C6B C7B 1.439(6) . ?
C8B C9B 1.518(6) . ?
C9B C10B 1.540(6) . ?
C15B C16B 1.525(6) . ?
C16B C17B 1.523(6) . ?
C18B C19B 1.432(6) . ?
C19B C20B 1.404(6) . ?
C19B C24B 1.412(6) . ?
C20B C21B 1.370(6) . ?
C21B C22B 1.377(7) . ?
C22B C23B 1.386(6) . ?
C23B C24B 1.414(6) . ?
Cl1 C1 1.744(11) . ?
Cl1X C1X 1.733(10) . ?
Cl2 C1 1.600(11) . ?
Cl2 C1X 1.627(11) . ?

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
O1A Cu1A O2A 163.43(15) . . ?
O1A Cu1A N1A 92.25(15) . . ?
O1A Cu1A N2A 89.30(14) . . ?
O2A Cu1A N1A 90.01(14) . . ?
O2A Cu1A N2A 92.47(13) . . ?
N2A Cu1A N1A 165.97(17) . . ?
O3A Si1A C10A 106.9(2) . . ?
O3A Si1A C11A 109.8(2) . . ?
O3A Si1A C12A 109.3(3) . . ?
C10A Si1A C11A 108.3(3) . . ?
C10A Si1A C12A 111.6(2) . . ?
C12A Si1A C11A 110.9(3) . . ?
O3A Si2A C13A 109.0(2) . . ?
O3A Si2A C14A 110.3(2) . . ?
O3A Si2A C15A 106.1(2) . . ?
C14A Si2A C13A 110.7(3) . . ?
C15A Si2A C13A 111.1(2) . . ?
C15A Si2A C14A 109.5(2) . . ?
C1A O1A Cu1A 128.0(3) . . ?
C24A O2A Cu1A 126.6(3) . . ?
Si1A O3A Si2A 160.9(3) . . ?
C7A N1A Cu1A 124.0(3) . . ?
C7A N1A C8A 118.1(4) . . ?
C8A N1A Cu1A 117.7(3) . . ?
C17A N2A Cu1A 118.8(3) . . ?
C18A N2A Cu1A 124.2(3) . . ?
C18A N2A C17A 117.0(4) . . ?
O1A C1A C2A 119.8(4) . . ?
O1A C1A C6A 124.0(4) . . ?
C2A C1A C6A 116.1(4) . . ?
C1A C2A Cl1A 117.4(4) . . ?
C3A C2A Cl1A 119.8(4) . . ?
C3A C2A C1A 122.8(5) . . ?
C2A C3A C4A 119.5(5) . . ?
C3A C4A Cl2A 118.9(4) . . ?
C5A C4A Cl2A 120.6(4) . . ?
C5A C4A C3A 120.4(5) . . ?
C4A C5A C6A 120.7(5) . . ?
C1A C6A C7A 121.2(5) . . ?
C5A C6A C1A 120.4(4) . . ?
C5A C6A C7A 118.1(4) . . ?
N1A C7A C6A 126.8(4) . . ?
N1A C8A C9A 109.8(4) . . ?
C8A C9A C10A 114.4(4) . . ?
C9A C10A Si1A 116.2(4) . . ?
C16A C15A Si2A 115.3(3) . . ?
C15A C16A C17A 114.8(4) . . ?
N2A C17A C16A 109.3(3) . . ?
N2A C18A C19A 125.7(4) . . ?
C20A C19A C18A 117.2(4) . . ?
C24A C19A C18A 122.2(4) . . ?
C24A C19A C20A 120.5(4) . . ?
C21A C20A C19A 120.3(4) . . ?
C20A C21A Cl4A 119.6(4) . . ?
C20A C21A C22A 121.1(4) . . ?
C22A C21A Cl4A 119.2(3) . . ?
C23A C22A C21A 118.6(4) . . ?
C22A C23A Cl3A 118.8(3) . . ?
C22A C23A C24A 122.8(4) . . ?
C24A C23A Cl3A 118.3(4) . . ?
O2A C24A C19A 124.4(4) . . ?
O2A C24A C23A 119.1(4) . . ?
C19A C24A C23A 116.5(4) . . ?
O1B Cu1B O2B 162.33(13) . . ?
O1B Cu1B N1B 93.12(14) . . ?
O1B Cu1B N2B 88.82(14) . . ?
O2B Cu1B N1B 92.73(15) . . ?
O2B Cu1B N2B 91.38(14) . . ?
N2B Cu1B N1B 159.92(15) . . ?
O3B Si1B C10B 106.1(2) . . ?
O3B Si1B C11B 109.1(3) . . ?
O3B Si1B C12B 109.6(3) . . ?
C11B Si1B C10B 110.6(2) . . ?
C11B Si1B C12B 110.3(3) . . ?
C12B Si1B C10B 111.0(3) . . ?
O3B Si2B C13B 109.4(3) . . ?
O3B Si2B C14B 108.3(2) . . ?
O3B Si2B C15B 107.4(2) . . ?
C14B Si2B C13B 110.2(3) . . ?
C15B Si2B C13B 110.2(2) . . ?
C15B Si2B C14B 111.3(3) . . ?
C1B O1B Cu1B 129.1(3) . . ?
C24B O2B Cu1B 125.4(3) . . ?
Si1B O3B Si2B 154.5(2) . . ?
C7B N1B Cu1B 124.1(3) . . ?
C7B N1B C8B 117.4(4) . . ?
C8B N1B Cu1B 118.5(3) . . ?
C17B N2B Cu1B 117.4(3) . . ?
C18B N2B Cu1B 124.0(3) . . ?
C18B N2B C17B 118.5(4) . . ?
O1B C1B C2B 119.3(5) . . ?
O1B C1B C6B 124.3(4) . . ?
C6B C1B C2B 116.4(4) . . ?
C1B C2B Cl1B 117.8(3) . . ?
C3B C2B Cl1B 119.9(4) . . ?
C3B C2B C1B 122.3(5) . . ?
C2B C3B C4B 119.5(5) . . ?
C3B C4B Cl2B 118.9(4) . . ?
C5B C4B Cl2B 120.2(4) . . ?
C5B C4B C3B 121.0(4) . . ?
C4B C5B C6B 120.2(5) . . ?
C1B C6B C7B 122.1(4) . . ?
C5B C6B C1B 120.6(5) . . ?
C5B C6B C7B 117.3(5) . . ?
N1B C7B C6B 127.3(5) . . ?
N1B C8B C9B 109.6(4) . . ?
C8B C9B C10B 114.3(4) . . ?
C9B C10B Si1B 114.4(3) . . ?
C16B C15B Si2B 115.8(3) . . ?
C17B C16B C15B 114.5(4) . . ?
N2B C17B C16B 110.4(4) . . ?
N2B C18B C19B 126.2(5) . . ?
C20B C19B C18B 117.5(5) . . ?
C20B C19B C24B 120.7(5) . . ?
C24B C19B C18B 121.8(4) . . ?
C21B C20B C19B 119.6(5) . . ?
C20B C21B Cl4B 118.7(4) . . ?
C20B C21B C22B 122.1(4) . . ?
C22B C21B Cl4B 119.2(4) . . ?
C21B C22B C23B 118.4(5) . . ?
C22B C23B Cl3B 119.2(4) . . ?
C22B C23B C24B 122.5(5) . . ?
C24B C23B Cl3B 118.3(4) . . ?
O2B C24B C19B 124.1(4) . . ?
O2B C24B C23B 119.1(5) . . ?
C19B C24B C23B 116.7(4) . . ?
Cl2 C1 Cl1 114.2(8) . . ?
Cl2 C1X Cl1X 117.9(7) . . ?

_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 1.487
_oxdiff_exptl_absorpt_empirical_full_min 0.767
####################################################################### 
# 
# This file contains crystal structure data downloaded from the 
# Cambridge Structural Database (CSD) hosted by the Cambridge 
# Crystallographic Data Centre (CCDC).
# 
# Full information about CCDC data access policies and citation 
# guidelines are available at http://www.ccdc.cam.ac.uk/access/V1 
# 
# Audit and citation data items may have been added by the CCDC. 
# Please retain this information to preserve the provenance of 
# this file and to allow appropriate attribution of the data. 
# 
#######################################################################

data_shi_4176_mada
_database_code_depnum_ccdc_archive 'CCDC 1982362'
loop_
_audit_author_name
_audit_author_address
'Dascalu Mihaela'
;Petru Poni Institute of Macromolecular Chemistry, Iasi
Romania
;
_audit_update_record             
;
2021-08-01 deposited with the CCDC.	2021-08-20 downloaded from the CCDC.
;
_audit_creation_date             2020-02-06
_audit_creation_method           
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_shelx_SHELXL_version_number     2018/3
_chemical_name_common            ?
_chemical_name_systematic        ?
_chemical_formula_moiety         '3(C24 H30 Cl4 N2 O3 Si2 Zn), C H2 Cl2'
_chemical_formula_sum            'C73 H92 Cl14 N6 O9 Si6 Zn3'
_chemical_formula_weight         2058.47
_chemical_melting_point          ?
_chemical_oxdiff_formula         C30H30N2O4Cl2Si2Zn1
_chemical_oxdiff_usercomment     DS_39
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'
Si Si 0.0817 0.0704 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Zn Zn 0.2839 1.4301 '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                   15.6914(9)
_cell_length_b                   17.4652(7)
_cell_length_c                   19.6006(8)
_cell_angle_alpha                99.587(3)
_cell_angle_beta                 104.598(4)
_cell_angle_gamma                109.175(4)
_cell_volume                     4723.6(4)
_cell_formula_units_Z            2
_cell_measurement_reflns_used    6281
_cell_measurement_temperature    180.05(10)
_cell_measurement_theta_max      24.6710
_cell_measurement_theta_min      1.5310
_shelx_estimated_absorpt_T_max   0.905
_shelx_estimated_absorpt_T_min   0.628
_exptl_absorpt_coefficient_mu    1.280
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.76709
_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            'clear light yellow'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   light
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    1.447
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       block
_exptl_crystal_F_000             2112
_exptl_crystal_size_max          0.4
_exptl_crystal_size_mid          0.15
_exptl_crystal_size_min          0.08
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0547
_diffrn_reflns_av_unetI/netI     0.1070
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.997
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -18
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_number            35173
_diffrn_reflns_point_group_measured_fraction_full 0.997
_diffrn_reflns_point_group_measured_fraction_max 0.997
_diffrn_reflns_theta_full        25.027
_diffrn_reflns_theta_max         25.027
_diffrn_reflns_theta_min         1.514
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      180.05(10)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 8.0797
_diffrn_detector_type            Eos
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measurement_details      
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  tₑₓₚ   ω     θ     κ     φ   Frames
#--------------------------------------------------------------------------
  1  ω    -28.00  46.00   1.00   30.00    --  -15.76  57.00  30.00   74
  2  ω      2.00  79.00   1.00   30.00    --   17.94  57.00 120.00   77
  3  ω      6.00  78.00   1.00   30.00    --   17.94  57.00 -90.00   72
  4  ω     16.00  83.00   1.00   30.00    --   17.94  57.00-180.00   67
  5  ω    -23.00  23.00   1.00   30.00    --  -15.76 -99.00   0.00   46
  6  ω    -32.00  29.00   1.00   30.00    --  -15.76  57.00 -30.00   61
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'Xcalibur, Eos'
_diffrn_measurement_method       'ω scans'
_diffrn_orient_matrix_type       
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      -0.0485654000
_diffrn_orient_matrix_UB_12      -0.0092534000
_diffrn_orient_matrix_UB_13      -0.0192567000
_diffrn_orient_matrix_UB_21      -0.0050116000
_diffrn_orient_matrix_UB_22      -0.0404048000
_diffrn_orient_matrix_UB_23      -0.0188917000
_diffrn_orient_matrix_UB_31      -0.0136156000
_diffrn_orient_matrix_UB_32      -0.0167111000
_diffrn_orient_matrix_UB_33      0.0279836000
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_source                   'fine-focus sealed X-ray tube'
_diffrn_source_type              'Enhance (Mo) X-ray Source'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                11272
_reflns_number_total             16648
_reflns_odcompleteness_completeness 99.97
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     26.32
_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    'olex2.solve (Bourhis et al., 2015)'
_refine_diff_density_max         0.726
_refine_diff_density_min         -0.750
_refine_diff_density_rms         0.101
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.099
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1019
_refine_ls_number_reflns         16648
_refine_ls_number_restraints     2
_refine_ls_R_factor_all          0.1254
_refine_ls_R_factor_gt           0.0823
_refine_ls_restrained_S_all      1.099
_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)+(0.0490P)²+12.2125P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1568
_refine_ls_wR_factor_ref         0.1753
_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
 Cl2-C1X \\sim Cl2X-C1X
 with sigma of 0.01
 Cl2X-C1X \\sim Cl2-C1
 with sigma of 0.01
 Cl1-C1X \\sim Cl1-C1
 with sigma of 0.01
3. Uiso/Uaniso restraints and constraints
Uanis(Cl2X) = Uanis(Cl2)
Uanis(C1X) = Uanis(C1)
4. Others
 Sof(Cl2X)=Sof(C1X)=Sof(H7DA)=Sof(H8DA)=1-FVAR(1)
 Sof(Cl2)=Sof(C1)=Sof(H5DA)=Sof(H6DA)=FVAR(1)
5.a Secondary CH2 refined with riding coordinates:
 C8A(HC,HD), C9A(HE,HF), C10A(HG,HH), C15A(HU,HV), C16A(HW,HX), C17A(HY,HZ),
 C8B(H8BA,H8BB), C9B(H9BA,H9BB), C10B(H10A,H10B), C15B(H15A,H15B), C16B(H16A,
 H16B), C17B(H17A,H17B), C8C(H6AA,H7AA), C9C(H8AA,H9AA), C10C(H0BA,H1BA),
 C15C(H6CA,H7CA), C16C(H8CA,H9CA), C17C(H0DA,H1DA), C1(H5DA,H6DA), C1X(H7DA,
 H8DA)
5.b Aromatic/amide H refined with riding coordinates:
 C3A(H), C5A(HA), C7A(HB), C18A(H0AA), C20A(H1AA), C22A(H2AA), C3B(H3B),
 C5B(H5B), C7B(H7B), C18B(H18B), C20B(H20B), C22B(H22B), C3C(H3AA), C5C(H4AA),
 C7C(H5AA), C18C(H2DA), C20C(H3DA), C22C(H4DA)
5.c Idealised Me refined as rotating group:
 C11A(HI,HJ,HK), C12A(HL,HM,HN), C13A(HO,HP,HQ), C14A(HR,HS,HT), C11B(H11A,
 H11B,H11C), C12B(H12A,H12B,H12C), C13B(H13A,H13B,H13C), C14B(H14A,H14B,H14C),
 C11C(H2BA,H3BA,H4BA), C12C(H5BA,H6BA,H7BA), C13C(H0CA,H1CA,H2CA), C14C(H3CA,
 H4CA,H5CA)
;
_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
Zn1A Zn 0.43510(6) 0.96095(5) 0.23923(4) 0.0333(2) Uani 1 1 d . . . . .
Cl1A Cl 0.62391(18) 1.05338(14) 0.49037(11) 0.0621(7) Uani 1 1 d . . . . .
Cl2A Cl 0.5248(2) 1.31767(15) 0.53217(12) 0.0751(8) Uani 1 1 d . . . . .
Cl3A Cl 0.45634(14) 0.60796(11) 0.00234(10) 0.0414(5) Uani 1 1 d . . . . .
Cl4A Cl 0.54941(15) 0.94108(11) 0.03871(10) 0.0427(5) Uani 1 1 d . . . . .
Si1A Si 0.04573(15) 0.92038(13) 0.14314(11) 0.0365(5) Uani 1 1 d . . . . .
Si2A Si 0.04434(15) 0.74731(13) 0.17674(12) 0.0397(5) Uani 1 1 d . . . . .
O1A O 0.5167(4) 1.0197(3) 0.3375(2) 0.0392(13) Uani 1 1 d . . . . .
O2A O 0.4820(3) 0.9351(3) 0.1615(2) 0.0352(12) Uani 1 1 d . . . . .
O3A O 0.0637(4) 0.8416(3) 0.1678(3) 0.0639(17) Uani 1 1 d . . . . .
N1A N 0.3871(4) 1.0515(3) 0.2232(3) 0.0246(13) Uani 1 1 d . . . . .
N2A N 0.3815(4) 0.8419(3) 0.2459(3) 0.0267(13) Uani 1 1 d . . . . .
C1A C 0.5120(5) 1.0848(4) 0.3776(3) 0.0278(16) Uani 1 1 d . . . . .
C2A C 0.5622(5) 1.1111(4) 0.4545(4) 0.0348(18) Uani 1 1 d . . . . .
C3A C 0.5657(6) 1.1815(5) 0.4997(4) 0.039(2) Uani 1 1 d . . . . .
H H 0.600808 1.197490 0.549278 0.047 Uiso 1 1 calc R . . . .
C4A C 0.5178(6) 1.2291(4) 0.4724(4) 0.0381(19) Uani 1 1 d . . . . .
C5A C 0.4682(5) 1.2077(4) 0.3991(4) 0.0339(17) Uani 1 1 d . . . . .
HA H 0.438049 1.241360 0.380817 0.041 Uiso 1 1 calc R . . . .
C6A C 0.4624(5) 1.1345(4) 0.3506(3) 0.0248(15) Uani 1 1 d . . . . .
C7A C 0.4083(5) 1.1180(4) 0.2748(3) 0.0254(15) Uani 1 1 d . . . . .
HB H 0.386647 1.158891 0.261853 0.031 Uiso 1 1 calc R . . . .
C8A C 0.3298(5) 1.0464(4) 0.1484(3) 0.0274(16) Uani 1 1 d . . . . .
HC H 0.360012 1.031247 0.113702 0.033 Uiso 1 1 calc R . . . .
HD H 0.328215 1.101137 0.146927 0.033 Uiso 1 1 calc R . . . .
C9A C 0.2284(5) 0.9817(4) 0.1259(4) 0.0338(18) Uani 1 1 d . . . . .
HE H 0.198001 0.972394 0.073894 0.041 Uiso 1 1 calc R . . . .
HF H 0.231163 0.928886 0.133146 0.041 Uiso 1 1 calc R . . . .
C10A C 0.1660(5) 1.0046(4) 0.1663(4) 0.0357(18) Uani 1 1 d . . . . .
HG H 0.158214 1.054632 0.155538 0.043 Uiso 1 1 calc R . . . .
HH H 0.198616 1.018591 0.218564 0.043 Uiso 1 1 calc R . . . .
C11A C -0.0234(6) 0.9548(6) 0.1955(4) 0.059(3) Uani 1 1 d . . . . .
HI H -0.081468 0.908148 0.188065 0.089 Uiso 1 1 calc GR . . . .
HJ H -0.038465 0.999104 0.179130 0.089 Uiso 1 1 calc GR . . . .
HK H 0.013629 0.975205 0.246669 0.089 Uiso 1 1 calc GR . . . .
C12A C -0.0149(6) 0.8870(6) 0.0435(4) 0.063(3) Uani 1 1 d . . . . .
HL H 0.023011 0.867122 0.019305 0.094 Uiso 1 1 calc GR . . . .
HM H -0.023044 0.933901 0.027410 0.094 Uiso 1 1 calc GR . . . .
HN H -0.076287 0.842502 0.031715 0.094 Uiso 1 1 calc GR . . . .
C13A C -0.0234(6) 0.7292(5) 0.2416(5) 0.056(2) Uani 1 1 d . . . . .
HO H 0.009250 0.774038 0.286175 0.084 Uiso 1 1 calc GR . . . .
HP H -0.028196 0.676493 0.252284 0.084 Uiso 1 1 calc GR . . . .
HQ H -0.086312 0.727555 0.220049 0.084 Uiso 1 1 calc GR . . . .
C14A C -0.0230(6) 0.6684(5) 0.0870(5) 0.061(3) Uani 1 1 d . . . . .
HR H -0.086180 0.667985 0.069768 0.091 Uiso 1 1 calc GR . . . .
HS H -0.027156 0.613694 0.091981 0.091 Uiso 1 1 calc GR . . . .
HT H 0.009269 0.682604 0.052447 0.091 Uiso 1 1 calc GR . . . .
C15A C 0.1660(5) 0.7452(5) 0.2133(4) 0.043(2) Uani 1 1 d . . . . .
HU H 0.159259 0.694115 0.228675 0.052 Uiso 1 1 calc R . . . .
HV H 0.193218 0.743022 0.174058 0.052 Uiso 1 1 calc R . . . .
C16A C 0.2357(5) 0.8213(4) 0.2781(4) 0.0343(18) Uani 1 1 d . . . . .
HW H 0.236907 0.872493 0.264566 0.041 Uiso 1 1 calc R . . . .
HX H 0.212194 0.819766 0.319301 0.041 Uiso 1 1 calc R . . . .
C17A C 0.3368(5) 0.8244(4) 0.3018(4) 0.0313(17) Uani 1 1 d . . . . .
HY H 0.374316 0.867905 0.347568 0.038 Uiso 1 1 calc R . . . .
HZ H 0.335616 0.770850 0.310136 0.038 Uiso 1 1 calc R . . . .
C18A C 0.3938(4) 0.7813(4) 0.2067(3) 0.0247(15) Uani 1 1 d . . . . .
H0AA H 0.375765 0.730055 0.218145 0.030 Uiso 1 1 calc R . . . .
C19A C 0.4323(5) 0.7848(4) 0.1473(3) 0.0262(16) Uani 1 1 d . . . . .
C20A C 0.4294(5) 0.7082(4) 0.1089(3) 0.0275(16) Uani 1 1 d . . . . .
H1AA H 0.406522 0.660071 0.124113 0.033 Uiso 1 1 calc R . . . .
C21A C 0.4594(5) 0.7032(4) 0.0499(4) 0.0277(16) Uani 1 1 d . . . . .
C22A C 0.4951(5) 0.7746(4) 0.0269(4) 0.0291(16) Uani 1 1 d . . . . .
H2AA H 0.515020 0.770817 -0.014013 0.035 Uiso 1 1 calc R . . . .
C23A C 0.5009(5) 0.8506(4) 0.0648(3) 0.0264(16) Uani 1 1 d . . . . .
C24A C 0.4711(5) 0.8604(4) 0.1269(3) 0.0269(16) Uani 1 1 d . . . . .
Zn1B Zn 0.62303(6) 0.69408(5) 0.28809(4) 0.0279(2) Uani 1 1 d . . . . .
Cl1B Cl 0.70227(15) 0.61171(13) 0.07611(10) 0.0470(5) Uani 1 1 d . . . . .
Cl2B Cl 0.76201(17) 0.91667(16) 0.02981(13) 0.0661(7) Uani 1 1 d . . . . .
Cl3B Cl 0.34630(16) 0.36366(12) 0.41288(12) 0.0521(6) Uani 1 1 d . . . . .
Cl4B Cl 0.28920(13) 0.57997(12) 0.25996(10) 0.0415(5) Uani 1 1 d . . . . .
Si1B Si 0.85809(14) 0.97284(12) 0.55069(10) 0.0311(5) Uani 1 1 d . . . . .
Si2B Si 0.91365(16) 0.81985(13) 0.58463(11) 0.0384(5) Uani 1 1 d . . . . .
O1B O 0.6634(4) 0.6793(3) 0.2036(2) 0.0347(12) Uani 1 1 d . . . . .
O2B O 0.4928(3) 0.6363(3) 0.2812(2) 0.0320(11) Uani 1 1 d . . . . .
O3B O 0.9010(4) 0.9010(3) 0.5614(3) 0.0389(12) Uani 1 1 d . . . . .
N1B N 0.6440(4) 0.8151(3) 0.2995(3) 0.0277(13) Uani 1 1 d . . . . .
N2B N 0.6807(4) 0.6337(3) 0.3507(3) 0.0236(12) Uani 1 1 d . . . . .
C1B C 0.6876(5) 0.7359(4) 0.1692(3) 0.0259(15) Uani 1 1 d . . . . .
C2B C 0.7077(5) 0.7129(5) 0.1039(4) 0.0351(18) Uani 1 1 d . . . . .
C3B C 0.7301(5) 0.7668(5) 0.0616(4) 0.040(2) Uani 1 1 d . . . . .
H3B H 0.742105 0.749308 0.018777 0.048 Uiso 1 1 calc R . . . .
C4B C 0.7345(5) 0.8491(5) 0.0845(4) 0.043(2) Uani 1 1 d . . . . .
C5B C 0.7173(5) 0.8748(5) 0.1468(4) 0.0354(18) Uani 1 1 d . . . . .
H5B H 0.721536 0.929826 0.161146 0.042 Uiso 1 1 calc R . . . .
C6B C 0.6931(5) 0.8199(4) 0.1907(4) 0.0296(16) Uani 1 1 d . . . . .
C7B C 0.6689(5) 0.8525(4) 0.2520(4) 0.0292(16) Uani 1 1 d . . . . .
H7B H 0.671578 0.907325 0.258288 0.035 Uiso 1 1 calc R . . . .
C8B C 0.6151(5) 0.8566(4) 0.3559(3) 0.0313(17) Uani 1 1 d . . . . .
H8BA H 0.550857 0.821088 0.352049 0.038 Uiso 1 1 calc R . . . .
H8BB H 0.614012 0.909412 0.347319 0.038 Uiso 1 1 calc R . . . .
C9B C 0.6833(5) 0.8739(4) 0.4340(3) 0.0286(16) Uani 1 1 d . . . . .
H9BA H 0.652777 0.887506 0.468972 0.034 Uiso 1 1 calc R . . . .
H9BB H 0.692874 0.822790 0.439042 0.034 Uiso 1 1 calc R . . . .
C10B C 0.7797(5) 0.9444(5) 0.4534(4) 0.0350(18) Uani 1 1 d . . . . .
H10A H 0.769877 0.994053 0.443538 0.042 Uiso 1 1 calc R . . . .
H10B H 0.812775 0.928266 0.421508 0.042 Uiso 1 1 calc R . . . .
C11B C 0.9606(6) 1.0737(5) 0.5736(4) 0.049(2) Uani 1 1 d . . . . .
H11A H 1.004892 1.082803 0.620973 0.074 Uiso 1 1 calc GR . . . .
H11B H 0.938478 1.118831 0.574410 0.074 Uiso 1 1 calc GR . . . .
H11C H 0.991904 1.071903 0.537496 0.074 Uiso 1 1 calc GR . . . .
C12B C 0.7868(6) 0.9802(6) 0.6127(4) 0.053(2) Uani 1 1 d . . . . .
H12A H 0.732353 0.928157 0.599209 0.079 Uiso 1 1 calc GR . . . .
H12B H 0.765547 1.025392 0.608386 0.079 Uiso 1 1 calc GR . . . .
H12C H 0.825674 0.990850 0.662384 0.079 Uiso 1 1 calc GR . . . .
C13B C 1.0406(6) 0.8356(6) 0.6049(5) 0.064(3) Uani 1 1 d . . . . .
H13A H 1.058277 0.840392 0.561875 0.097 Uiso 1 1 calc GR . . . .
H13B H 1.050012 0.788429 0.619566 0.097 Uiso 1 1 calc GR . . . .
H13C H 1.079434 0.886231 0.643790 0.097 Uiso 1 1 calc GR . . . .
C14B C 0.8789(7) 0.8099(6) 0.6668(4) 0.068(3) Uani 1 1 d . . . . .
H14A H 0.924067 0.856000 0.707938 0.102 Uiso 1 1 calc GR . . . .
H14B H 0.878266 0.757695 0.676538 0.102 Uiso 1 1 calc GR . . . .
H14C H 0.816406 0.810886 0.658638 0.102 Uiso 1 1 calc GR . . . .
C15B C 0.8324(6) 0.7254(4) 0.5050(4) 0.042(2) Uani 1 1 d . . . . .
H15A H 0.842405 0.676208 0.515777 0.051 Uiso 1 1 calc R . . . .
H15B H 0.766791 0.716886 0.500626 0.051 Uiso 1 1 calc R . . . .
C16B C 0.8456(5) 0.7310(4) 0.4322(4) 0.0375(18) Uani 1 1 d . . . . .
H16A H 0.912227 0.743523 0.437180 0.045 Uiso 1 1 calc R . . . .
H16B H 0.830768 0.777553 0.419298 0.045 Uiso 1 1 calc R . . . .
C17B C 0.7843(5) 0.6517(4) 0.3704(4) 0.0332(17) Uani 1 1 d . . . . .
H17A H 0.803538 0.657178 0.327556 0.040 Uiso 1 1 calc R . . . .
H17B H 0.795694 0.604392 0.384637 0.040 Uiso 1 1 calc R . . . .
C18B C 0.6277(5) 0.5705(4) 0.3668(3) 0.0262(16) Uani 1 1 d . . . . .
H18B H 0.658325 0.540285 0.390743 0.031 Uiso 1 1 calc R . . . .
C19B C 0.5245(5) 0.5411(4) 0.3514(3) 0.0228(15) Uani 1 1 d . . . . .
C20B C 0.4866(5) 0.4755(4) 0.3818(3) 0.0310(17) Uani 1 1 d . . . . .
H20B H 0.526927 0.454235 0.408448 0.037 Uiso 1 1 calc R . . . .
C21B C 0.3923(5) 0.4429(4) 0.3726(4) 0.0335(18) Uani 1 1 d . . . . .
C22B C 0.3308(5) 0.4741(4) 0.3337(4) 0.0329(17) Uani 1 1 d . . . . .
H22B H 0.265879 0.451333 0.327286 0.039 Uiso 1 1 calc R . . . .
C23B C 0.3672(5) 0.5389(4) 0.3049(4) 0.0313(17) Uani 1 1 d . . . . .
C24B C 0.4642(5) 0.5756(4) 0.3115(3) 0.0263(16) Uani 1 1 d . . . . .
Zn1C Zn 0.59134(6) 0.33836(5) 0.26264(4) 0.0294(2) Uani 1 1 d . . . . .
Cl1C Cl 0.25162(15) 0.23934(13) 0.20255(13) 0.0560(6) Uani 1 1 d . . . . .
Cl2C Cl 0.24746(13) 0.48489(12) 0.07051(10) 0.0376(4) Uani 1 1 d . . . . .
Cl3C Cl 0.87503(19) 0.25488(17) 0.57223(13) 0.0721(7) Uani 1 1 d . . . . .
Cl4C Cl 0.74686(16) 0.49460(13) 0.51501(10) 0.0502(6) Uani 1 1 d . . . . .
Si1C Si 0.90342(16) 0.40303(14) 0.11810(13) 0.0419(6) Uani 1 1 d . . . . .
Si2C Si 0.82708(16) 0.21022(14) 0.11747(12) 0.0390(5) Uani 1 1 d . . . . .
O1C O 0.4553(3) 0.3056(3) 0.2256(3) 0.0337(12) Uani 1 1 d . . . . .
O2C O 0.6603(4) 0.3876(3) 0.3667(2) 0.0362(12) Uani 1 1 d . . . . .
O3C O 0.8724(4) 0.3117(3) 0.1366(3) 0.0411(13) Uani 1 1 d . . . . .
N1C N 0.6261(4) 0.4305(3) 0.2147(3) 0.0257(13) Uani 1 1 d . . . . .
N2C N 0.6204(4) 0.2336(3) 0.2547(3) 0.0296(14) Uani 1 1 d . . . . .
C1C C 0.4131(5) 0.3469(4) 0.1911(3) 0.0277(16) Uani 1 1 d . . . . .
C2C C 0.3134(5) 0.3242(4) 0.1744(4) 0.0339(17) Uani 1 1 d . . . . .
C3C C 0.2629(5) 0.3645(4) 0.1372(4) 0.0341(18) Uani 1 1 d . . . . .
H3AA H 0.197035 0.345978 0.126482 0.041 Uiso 1 1 calc R . . . .
C4C C 0.3115(5) 0.4324(4) 0.1162(3) 0.0288(16) Uani 1 1 d . . . . .
C5C C 0.4069(5) 0.4590(4) 0.1304(3) 0.0270(16) Uani 1 1 d . . . . .
H4AA H 0.438241 0.504772 0.115209 0.032 Uiso 1 1 calc R . . . .
C6C C 0.4598(5) 0.4182(4) 0.1679(3) 0.0257(15) Uani 1 1 d . . . . .
C7C C 0.5620(5) 0.4549(4) 0.1812(3) 0.0246(15) Uani 1 1 d . . . . .
H5AA H 0.583720 0.501272 0.163403 0.030 Uiso 1 1 calc R . . . .
C8C C 0.7258(5) 0.4773(4) 0.2203(4) 0.0313(17) Uani 1 1 d . . . . .
H6AA H 0.766408 0.494423 0.271035 0.038 Uiso 1 1 calc R . . . .
H7AA H 0.730443 0.527798 0.204379 0.038 Uiso 1 1 calc R . . . .
C9C C 0.7601(5) 0.4245(4) 0.1742(4) 0.0360(18) Uani 1 1 d . . . . .
H8AA H 0.716635 0.404658 0.124243 0.043 Uiso 1 1 calc R . . . .
H9AA H 0.757986 0.375556 0.192028 0.043 Uiso 1 1 calc R . . . .
C10C C 0.8601(5) 0.4700(5) 0.1740(4) 0.043(2) Uani 1 1 d . . . . .
H0BA H 0.903418 0.491017 0.224137 0.051 Uiso 1 1 calc R . . . .
H1BA H 0.861906 0.518288 0.155174 0.051 Uiso 1 1 calc R . . . .
C11C C 0.8454(7) 0.3888(6) 0.0192(5) 0.070(3) Uani 1 1 d . . . . .
H2BA H 0.856477 0.345048 -0.009438 0.105 Uiso 1 1 calc GR . . . .
H3BA H 0.871909 0.440490 0.007037 0.105 Uiso 1 1 calc GR . . . .
H4BA H 0.777962 0.373349 0.008994 0.105 Uiso 1 1 calc GR . . . .
C12C C 1.0359(6) 0.4501(6) 0.1429(6) 0.075(3) Uani 1 1 d . . . . .
H5BA H 1.064775 0.455919 0.193866 0.112 Uiso 1 1 calc GR . . . .
H6BA H 1.055106 0.504574 0.133830 0.112 Uiso 1 1 calc GR . . . .
H7BA H 1.056036 0.414194 0.113800 0.112 Uiso 1 1 calc GR . . . .
C13C C 0.7572(7) 0.1659(6) 0.0176(4) 0.065(3) Uani 1 1 d . . . . .
H0CA H 0.711600 0.191062 0.004829 0.097 Uiso 1 1 calc GR . . . .
H1CA H 0.724282 0.106010 0.006859 0.097 Uiso 1 1 calc GR . . . .
H2CA H 0.799886 0.177766 -0.010350 0.097 Uiso 1 1 calc GR . . . .
C14C C 0.9255(7) 0.1723(6) 0.1440(6) 0.072(3) Uani 1 1 d . . . . .
H3CA H 0.971054 0.193099 0.119950 0.108 Uiso 1 1 calc GR . . . .
H4CA H 0.899606 0.111829 0.129572 0.108 Uiso 1 1 calc GR . . . .
H5CA H 0.956462 0.192489 0.196121 0.108 Uiso 1 1 calc GR . . . .
C15C C 0.7444(5) 0.1806(5) 0.1714(4) 0.0395(19) Uani 1 1 d . . . . .
H6CA H 0.734316 0.123778 0.174929 0.047 Uiso 1 1 calc R . . . .
H7CA H 0.774666 0.218011 0.220767 0.047 Uiso 1 1 calc R . . . .
C16C C 0.6470(5) 0.1849(4) 0.1385(4) 0.0307(17) Uani 1 1 d . . . . .
H8CA H 0.657305 0.240304 0.130940 0.037 Uiso 1 1 calc R . . . .
H9CA H 0.614368 0.143936 0.090860 0.037 Uiso 1 1 calc R . . . .
C17C C 0.5822(5) 0.1682(4) 0.1856(4) 0.0366(18) Uani 1 1 d . . . . .
H0DA H 0.519558 0.164983 0.158567 0.044 Uiso 1 1 calc R . . . .
H1DA H 0.574484 0.114235 0.195733 0.044 Uiso 1 1 calc R . . . .
C18C C 0.6672(5) 0.2204(4) 0.3127(4) 0.0286(16) Uani 1 1 d . . . . .
H2DA H 0.673448 0.168796 0.306268 0.034 Uiso 1 1 calc R . . . .
C19C C 0.7110(5) 0.2753(4) 0.3862(4) 0.0290(16) Uani 1 1 d . . . . .
C20C C 0.7638(5) 0.2452(5) 0.4377(4) 0.0384(19) Uani 1 1 d . . . . .
H3DA H 0.767536 0.193323 0.422599 0.046 Uiso 1 1 calc R . . . .
C21C C 0.8087(6) 0.2913(5) 0.5087(4) 0.045(2) Uani 1 1 d . . . . .
C22C C 0.8025(6) 0.3674(5) 0.5340(4) 0.043(2) Uani 1 1 d . . . . .
H4DA H 0.831325 0.397286 0.583176 0.051 Uiso 1 1 calc R . . . .
C23C C 0.7526(5) 0.3979(4) 0.4843(4) 0.0332(17) Uani 1 1 d . . . . .
C24C C 0.7052(5) 0.3537(4) 0.4093(4) 0.0284(16) Uani 1 1 d . . . . .
Cl1 Cl 0.9374(3) 0.5073(3) 0.40163(19) 0.1188(12) Uani 1 1 d D . . . .
Cl2 Cl 1.047(9) 0.413(5) 0.366(4) 0.176(3) Uani 0.065(10) 1 d D . P A 1
Cl2X Cl 0.9722(6) 0.3734(3) 0.3234(3) 0.176(3) Uani 0.935(10) 1 d D . P A 2
C1 C 1.016(10) 0.457(10) 0.431(5) 0.104(5) Uani 0.065(10) 1 d D . P A 1
H5DA H 1.072722 0.498714 0.469385 0.124 Uiso 0.065(10) 1 calc R . P A 1
H6DA H 0.984927 0.414582 0.452989 0.124 Uiso 0.065(10) 1 calc R . P A 1
C1X C 0.9669(10) 0.4182(8) 0.4029(8) 0.104(5) Uani 0.935(10) 1 d D . P A 2
H7DA H 1.028318 0.434957 0.440427 0.124 Uiso 0.935(10) 1 calc R . P A 2
H8DA H 0.919618 0.377088 0.416045 0.124 Uiso 0.935(10) 1 calc R . P A 2


_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
Zn1A O1A 1.908(5) . ?
Zn1A O2A 1.903(4) . ?
Zn1A N1A 1.999(5) . ?
Zn1A N2A 2.010(5) . ?
Cl1A C2A 1.728(7) . ?
Cl2A C4A 1.732(7) . ?
Cl3A C21A 1.746(6) . ?
Cl4A C23A 1.735(6) . ?
Si1A O3A 1.617(6) . ?
Si1A C10A 1.858(7) . ?
Si1A C11A 1.837(8) . ?
Si1A C12A 1.838(8) . ?
Si2A O3A 1.622(6) . ?
Si2A C13A 1.856(8) . ?
Si2A C14A 1.847(8) . ?
Si2A C15A 1.878(8) . ?
O1A C1A 1.305(7) . ?
O2A C24A 1.300(7) . ?
N1A C7A 1.291(8) . ?
N1A C8A 1.486(8) . ?
N2A C17A 1.466(8) . ?
N2A C18A 1.299(8) . ?
C1A C2A 1.427(9) . ?
C1A C6A 1.424(9) . ?
C2A C3A 1.366(9) . ?
C3A C4A 1.377(10) . ?
C4A C5A 1.370(9) . ?
C5A C6A 1.422(9) . ?
C6A C7A 1.440(9) . ?
C8A C9A 1.517(9) . ?
C9A C10A 1.513(9) . ?
C15A C16A 1.535(9) . ?
C16A C17A 1.517(9) . ?
C18A C19A 1.441(9) . ?
C19A C20A 1.402(8) . ?
C19A C24A 1.430(9) . ?
C20A C21A 1.353(9) . ?
C21A C22A 1.388(9) . ?
C22A C23A 1.373(9) . ?
C23A C24A 1.415(9) . ?
Zn1B O1B 1.924(4) . ?
Zn1B O2B 1.917(5) . ?
Zn1B N1B 1.994(5) . ?
Zn1B N2B 1.985(5) . ?
Cl1B C2B 1.728(8) . ?
Cl2B C4B 1.746(7) . ?
Cl3B C21B 1.748(7) . ?
Cl4B C23B 1.741(7) . ?
Si1B O3B 1.626(5) . ?
Si1B C10B 1.871(7) . ?
Si1B C11B 1.845(8) . ?
Si1B C12B 1.864(7) . ?
Si2B O3B 1.616(5) . ?
Si2B C13B 1.845(8) . ?
Si2B C14B 1.842(8) . ?
Si2B C15B 1.881(7) . ?
O1B C1B 1.296(7) . ?
O2B C24B 1.307(7) . ?
N1B C7B 1.291(8) . ?
N1B C8B 1.467(8) . ?
N2B C17B 1.482(8) . ?
N2B C18B 1.286(8) . ?
C1B C2B 1.419(9) . ?
C1B C6B 1.425(9) . ?
C2B C3B 1.374(9) . ?
C3B C4B 1.405(11) . ?
C4B C5B 1.352(10) . ?
C5B C6B 1.416(9) . ?
C6B C7B 1.432(9) . ?
C8B C9B 1.545(9) . ?
C9B C10B 1.509(9) . ?
C15B C16B 1.507(9) . ?
C16B C17B 1.513(9) . ?
C18B C19B 1.461(9) . ?
C19B C20B 1.407(9) . ?
C19B C24B 1.425(9) . ?
C20B C21B 1.350(10) . ?
C21B C22B 1.386(10) . ?
C22B C23B 1.371(9) . ?
C23B C24B 1.405(9) . ?
Zn1C O1C 1.921(5) . ?
Zn1C O2C 1.940(5) . ?
Zn1C N1C 1.989(5) . ?
Zn1C N2C 2.018(5) . ?
Cl1C C2C 1.744(7) . ?
Cl2C C4C 1.753(7) . ?
Cl3C C21C 1.756(7) . ?
Cl4C C23C 1.735(7) . ?
Si1C O3C 1.638(5) . ?
Si1C C10C 1.873(8) . ?
Si1C C11C 1.856(9) . ?
Si1C C12C 1.862(8) . ?
Si2C O3C 1.614(5) . ?
Si2C C13C 1.869(8) . ?
Si2C C14C 1.864(8) . ?
Si2C C15C 1.872(7) . ?
O1C C1C 1.292(8) . ?
O2C C24C 1.298(7) . ?
N1C C7C 1.291(8) . ?
N1C C8C 1.474(8) . ?
N2C C17C 1.457(8) . ?
N2C C18C 1.289(8) . ?
C1C C2C 1.415(9) . ?
C1C C6C 1.431(9) . ?
C2C C3C 1.379(10) . ?
C3C C4C 1.373(9) . ?
C4C C5C 1.351(9) . ?
C5C C6C 1.411(9) . ?
C6C C7C 1.452(9) . ?
C8C C9C 1.499(9) . ?
C9C C10C 1.508(10) . ?
C15C C16C 1.533(10) . ?
C16C C17C 1.531(9) . ?
C18C C19C 1.440(9) . ?
C19C C20C 1.423(9) . ?
C19C C24C 1.410(9) . ?
C20C C21C 1.356(10) . ?
C21C C22C 1.382(10) . ?
C22C C23C 1.381(10) . ?
C23C C24C 1.416(9) . ?
Cl1 C1 1.764(16) . ?
Cl1 C1X 1.764(12) . ?
Cl2 C1 1.658(17) . ?
Cl2X C1X 1.658(13) . ?

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
O1A Zn1A N1A 95.2(2) . . ?
O1A Zn1A N2A 101.9(2) . . ?
O2A Zn1A O1A 122.9(2) . . ?
O2A Zn1A N1A 107.4(2) . . ?
O2A Zn1A N2A 95.5(2) . . ?
N1A Zn1A N2A 137.4(2) . . ?
O3A Si1A C10A 106.1(3) . . ?
O3A Si1A C11A 108.4(4) . . ?
O3A Si1A C12A 108.3(4) . . ?
C11A Si1A C10A 110.7(4) . . ?
C11A Si1A C12A 113.3(4) . . ?
C12A Si1A C10A 109.8(4) . . ?
O3A Si2A C13A 108.7(4) . . ?
O3A Si2A C14A 110.4(4) . . ?
O3A Si2A C15A 105.3(3) . . ?
C13A Si2A C15A 111.8(4) . . ?
C14A Si2A C13A 110.6(4) . . ?
C14A Si2A C15A 110.0(4) . . ?
C1A O1A Zn1A 124.7(4) . . ?
C24A O2A Zn1A 126.3(4) . . ?
Si1A O3A Si2A 160.9(4) . . ?
C7A N1A Zn1A 122.8(5) . . ?
C7A N1A C8A 117.4(5) . . ?
C8A N1A Zn1A 119.7(4) . . ?
C17A N2A Zn1A 119.4(4) . . ?
C18A N2A Zn1A 121.6(4) . . ?
C18A N2A C17A 118.7(6) . . ?
O1A C1A C2A 118.7(6) . . ?
O1A C1A C6A 125.2(6) . . ?
C6A C1A C2A 116.1(6) . . ?
C1A C2A Cl1A 118.2(5) . . ?
C3A C2A Cl1A 119.4(5) . . ?
C3A C2A C1A 122.4(6) . . ?
C2A C3A C4A 120.5(6) . . ?
C3A C4A Cl2A 118.5(5) . . ?
C5A C4A Cl2A 121.1(6) . . ?
C5A C4A C3A 120.3(6) . . ?
C4A C5A C6A 120.6(6) . . ?
C1A C6A C7A 124.2(6) . . ?
C5A C6A C1A 120.0(6) . . ?
C5A C6A C7A 115.8(6) . . ?
N1A C7A C6A 125.7(6) . . ?
N1A C8A C9A 111.6(5) . . ?
C10A C9A C8A 115.6(6) . . ?
C9A C10A Si1A 114.4(5) . . ?
C16A C15A Si2A 113.9(5) . . ?
C17A C16A C15A 113.7(6) . . ?
N2A C17A C16A 110.8(5) . . ?
N2A C18A C19A 127.1(6) . . ?
C20A C19A C18A 116.0(6) . . ?
C20A C19A C24A 120.5(6) . . ?
C24A C19A C18A 123.5(6) . . ?
C21A C20A C19A 121.1(6) . . ?
C20A C21A Cl3A 121.0(5) . . ?
C20A C21A C22A 120.4(6) . . ?
C22A C21A Cl3A 118.5(5) . . ?
C23A C22A C21A 119.5(6) . . ?
C22A C23A Cl4A 120.1(5) . . ?
C22A C23A C24A 123.0(6) . . ?
C24A C23A Cl4A 116.8(5) . . ?
O2A C24A C19A 125.2(6) . . ?
O2A C24A C23A 119.4(6) . . ?
C23A C24A C19A 115.4(6) . . ?
O1B Zn1B N1B 96.4(2) . . ?
O1B Zn1B N2B 104.4(2) . . ?
O2B Zn1B O1B 120.8(2) . . ?
O2B Zn1B N1B 106.7(2) . . ?
O2B Zn1B N2B 97.8(2) . . ?
N2B Zn1B N1B 133.4(2) . . ?
O3B Si1B C10B 109.1(3) . . ?
O3B Si1B C11B 107.2(3) . . ?
O3B Si1B C12B 110.2(3) . . ?
C11B Si1B C10B 110.9(3) . . ?
C11B Si1B C12B 110.1(4) . . ?
C12B Si1B C10B 109.3(3) . . ?
O3B Si2B C13B 107.9(3) . . ?
O3B Si2B C14B 109.7(4) . . ?
O3B Si2B C15B 106.6(3) . . ?
C13B Si2B C15B 112.5(4) . . ?
C14B Si2B C13B 109.7(4) . . ?
C14B Si2B C15B 110.3(4) . . ?
C1B O1B Zn1B 125.2(4) . . ?
C24B O2B Zn1B 124.3(4) . . ?
Si2B O3B Si1B 159.4(3) . . ?
C7B N1B Zn1B 120.8(5) . . ?
C7B N1B C8B 120.2(6) . . ?
C8B N1B Zn1B 118.2(4) . . ?
C17B N2B Zn1B 120.5(4) . . ?
C18B N2B Zn1B 120.7(5) . . ?
C18B N2B C17B 118.1(6) . . ?
O1B C1B C2B 118.4(6) . . ?
O1B C1B C6B 124.9(6) . . ?
C2B C1B C6B 116.7(6) . . ?
C1B C2B Cl1B 118.1(5) . . ?
C3B C2B Cl1B 118.7(6) . . ?
C3B C2B C1B 123.2(7) . . ?
C2B C3B C4B 118.4(7) . . ?
C3B C4B Cl2B 118.0(6) . . ?
C5B C4B Cl2B 121.1(7) . . ?
C5B C4B C3B 120.9(7) . . ?
C4B C5B C6B 121.5(7) . . ?
C1B C6B C7B 124.5(6) . . ?
C5B C6B C1B 119.3(6) . . ?
C5B C6B C7B 116.1(6) . . ?
N1B C7B C6B 127.9(6) . . ?
N1B C8B C9B 112.1(5) . . ?
C10B C9B C8B 114.6(6) . . ?
C9B C10B Si1B 114.8(5) . . ?
C16B C15B Si2B 115.3(5) . . ?
C15B C16B C17B 114.0(6) . . ?
N2B C17B C16B 113.3(5) . . ?
N2B C18B C19B 126.9(6) . . ?
C20B C19B C18B 114.6(6) . . ?
C20B C19B C24B 120.4(6) . . ?
C24B C19B C18B 125.0(6) . . ?
C21B C20B C19B 120.9(7) . . ?
C20B C21B Cl3B 120.6(6) . . ?
C20B C21B C22B 120.7(7) . . ?
C22B C21B Cl3B 118.7(6) . . ?
C23B C22B C21B 119.0(7) . . ?
C22B C23B Cl4B 117.9(6) . . ?
C22B C23B C24B 123.7(7) . . ?
C24B C23B Cl4B 118.4(5) . . ?
O2B C24B C19B 124.8(6) . . ?
O2B C24B C23B 119.8(6) . . ?
C23B C24B C19B 115.3(6) . . ?
O1C Zn1C O2C 120.3(2) . . ?
O1C Zn1C N1C 97.1(2) . . ?
O1C Zn1C N2C 108.8(2) . . ?
O2C Zn1C N1C 106.6(2) . . ?
O2C Zn1C N2C 96.2(2) . . ?
N1C Zn1C N2C 130.0(2) . . ?
O3C Si1C C10C 106.9(3) . . ?
O3C Si1C C11C 109.9(4) . . ?
O3C Si1C C12C 108.7(4) . . ?
C11C Si1C C10C 109.5(4) . . ?
C11C Si1C C12C 110.5(5) . . ?
C12C Si1C C10C 111.4(4) . . ?
O3C Si2C C13C 109.1(4) . . ?
O3C Si2C C14C 108.9(4) . . ?
O3C Si2C C15C 107.6(3) . . ?
C13C Si2C C15C 109.1(4) . . ?
C14C Si2C C13C 111.7(4) . . ?
C14C Si2C C15C 110.3(4) . . ?
C1C O1C Zn1C 124.7(4) . . ?
C24C O2C Zn1C 125.4(4) . . ?
Si2C O3C Si1C 155.6(3) . . ?
C7C N1C Zn1C 120.6(5) . . ?
C7C N1C C8C 117.5(6) . . ?
C8C N1C Zn1C 121.8(4) . . ?
C17C N2C Zn1C 121.3(5) . . ?
C18C N2C Zn1C 119.8(5) . . ?
C18C N2C C17C 118.6(6) . . ?
O1C C1C C2C 120.5(6) . . ?
O1C C1C C6C 125.0(6) . . ?
C2C C1C C6C 114.4(6) . . ?
C1C C2C Cl1C 117.2(5) . . ?
C3C C2C Cl1C 118.6(6) . . ?
C3C C2C C1C 124.1(6) . . ?
C4C C3C C2C 118.8(7) . . ?
C3C C4C Cl2C 118.8(6) . . ?
C5C C4C Cl2C 120.2(5) . . ?
C5C C4C C3C 121.0(6) . . ?
C4C C5C C6C 121.0(6) . . ?
C1C C6C C7C 124.5(6) . . ?
C5C C6C C1C 120.6(6) . . ?
C5C C6C C7C 115.0(6) . . ?
N1C C7C C6C 127.4(6) . . ?
N1C C8C C9C 111.3(5) . . ?
C8C C9C C10C 114.2(6) . . ?
C9C C10C Si1C 113.9(5) . . ?
C16C C15C Si2C 113.8(5) . . ?
C17C C16C C15C 114.2(6) . . ?
N2C C17C C16C 112.2(6) . . ?
N2C C18C C19C 128.4(6) . . ?
C20C C19C C18C 115.0(6) . . ?
C24C C19C C18C 125.4(6) . . ?
C24C C19C C20C 119.5(6) . . ?
C21C C20C C19C 120.6(7) . . ?
C20C C21C Cl3C 120.8(6) . . ?
C20C C21C C22C 121.6(7) . . ?
C22C C21C Cl3C 117.6(6) . . ?
C23C C22C C21C 118.4(7) . . ?
C22C C23C Cl4C 118.8(6) . . ?
C22C C23C C24C 123.0(7) . . ?
C24C C23C Cl4C 118.2(5) . . ?
O2C C24C C19C 124.5(6) . . ?
O2C C24C C23C 118.6(6) . . ?
C19C C24C C23C 116.8(6) . . ?
Cl2 C1 Cl1 115(6) . . ?
Cl2X C1X Cl1 113.3(7) . . ?

_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 1.207
_oxdiff_exptl_absorpt_empirical_full_min 0.800
####################################################################### 
# 
# This file contains crystal structure data downloaded from the 
# Cambridge Structural Database (CSD) hosted by the Cambridge 
# Crystallographic Data Centre (CCDC).
# 
# Full information about CCDC data access policies and citation 
# guidelines are available at http://www.ccdc.cam.ac.uk/access/V1 
# 
# Audit and citation data items may have been added by the CCDC. 
# Please retain this information to preserve the provenance of 
# this file and to allow appropriate attribution of the data. 
# 
#######################################################################

data_md_4270_mada
_database_code_depnum_ccdc_archive 'CCDC 1982350'
loop_
_audit_author_name
_audit_author_address
'Dascalu Mihaela'
;Petru Poni Institute of Macromolecular Chemistry, Iasi
Romania
;
_audit_update_record             
;
2021-08-01 deposited with the CCDC.	2021-08-20 downloaded from the CCDC.
;
_audit_creation_date             2020-02-06
_audit_creation_method           
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_shelx_SHELXL_version_number     2018/3
_chemical_name_common            ?
_chemical_name_systematic        ?
_chemical_formula_moiety         '3(C24 H30 Cl4 Co N2 O3 Si2), C H2 Cl2'
_chemical_formula_sum            'C73 H92 Cl14 Co3 N6 O9 Si6'
_chemical_formula_weight         2039.15
_chemical_melting_point          ?
_chemical_oxdiff_formula         C30H30N2O4Cl2Si2Co1
_chemical_oxdiff_usercomment     C105
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'
Co Co 0.3494 0.9721 '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'
Si Si 0.0817 0.0704 '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                   15.6932(7)
_cell_length_b                   17.4257(10)
_cell_length_c                   19.5315(9)
_cell_angle_alpha                99.440(4)
_cell_angle_beta                 104.592(4)
_cell_angle_gamma                109.205(5)
_cell_volume                     4699.7(4)
_cell_formula_units_Z            2
_cell_measurement_reflns_used    7839
_cell_measurement_temperature    180.1(2)
_cell_measurement_theta_max      25.6330
_cell_measurement_theta_min      1.5240
_shelx_estimated_absorpt_T_max   0.969
_shelx_estimated_absorpt_T_min   0.622
_exptl_absorpt_coefficient_mu    1.051
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.83729
_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            'clear light orange'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   light
_exptl_crystal_colour_primary    orange
_exptl_crystal_density_diffrn    1.441
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       prism
_exptl_crystal_F_000             2094
_exptl_crystal_preparation       ?
_exptl_crystal_size_max          0.5
_exptl_crystal_size_mid          0.05
_exptl_crystal_size_min          0.03
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0720
_diffrn_reflns_av_unetI/netI     0.1649
_diffrn_reflns_Laue_measured_fraction_full 0.996
_diffrn_reflns_Laue_measured_fraction_max 0.996
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_h_min       -18
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_number            37110
_diffrn_reflns_point_group_measured_fraction_full 0.996
_diffrn_reflns_point_group_measured_fraction_max 0.996
_diffrn_reflns_theta_full        25.026
_diffrn_reflns_theta_max         25.026
_diffrn_reflns_theta_min         1.811
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      180.1(2)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 8.0797
_diffrn_detector_type            Eos
_diffrn_measured_fraction_theta_full 0.996
_diffrn_measured_fraction_theta_max 0.996
_diffrn_measurement_details      
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  tₑₓₚ   ω     θ     κ     φ   Frames
#--------------------------------------------------------------------------
  1  ω    -18.00  23.00   1.00  100.00    --  -15.60 -99.00-120.00   41
  2  ω     65.00  90.00   1.00  100.00    --   17.79-178.00   0.00   25
  3  ω    -10.00  52.00   1.00  100.00    --   17.79 -99.00 150.00   62
  4  ω    -19.00   7.00   1.00  100.00    --  -15.60 -99.00  30.00   26
  5  ω    -22.00  56.00   1.00  100.00    --   17.79 -99.00  30.00   78
  6  ω    -20.00  87.00   1.00  100.00    --   17.79   0.00   0.00  107
  7  ω      2.00  84.00   1.00  100.00    --   17.79  38.00-120.00   82
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'Xcalibur, Eos'
_diffrn_measurement_method       'ω scans'
_diffrn_orient_matrix_type       
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      -0.0248448000
_diffrn_orient_matrix_UB_12      -0.0215476000
_diffrn_orient_matrix_UB_13      -0.0376812000
_diffrn_orient_matrix_UB_21      0.0132813000
_diffrn_orient_matrix_UB_22      -0.0343314000
_diffrn_orient_matrix_UB_23      0.0052262000
_diffrn_orient_matrix_UB_31      -0.0421177000
_diffrn_orient_matrix_UB_32      -0.0190052000
_diffrn_orient_matrix_UB_33      0.0084788000
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_source                   'fine-focus sealed X-ray tube'
_diffrn_source_type              'Enhance (Mo) X-ray Source'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                9380
_reflns_number_total             16537
_reflns_odcompleteness_completeness 99.69
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     26.32
_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    'olex2.solve (Bourhis et al., 2015)'
_refine_diff_density_max         0.570
_refine_diff_density_min         -0.545
_refine_diff_density_rms         0.075
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.838
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1012
_refine_ls_number_reflns         16537
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.1127
_refine_ls_R_factor_gt           0.0515
_refine_ls_restrained_S_all      0.838
_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)] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0659
_refine_ls_wR_factor_ref         0.0845
_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.a Secondary CH2 refined with riding coordinates:
 C16A(HE,HF), C17A(HG,HH), C16B(HI,HJ), C17B(HM,HN), C9C(H9CA,H9CB), C8A(HO,
 HP), C8B(HR,HS), C17C(H17A,H17B), C15B(HV,HW), C9B(HY,HZ), C15A(H0AA,H1AA),
 C9A(H2AA,H3AA), C16C(H16A,H16B), C8C(H8CA,H8CB), C10C(H10A,H10B), C10A(H5AA,
 H6AA), C15C(H15A,H15B), C10B(H7AA,H8AA), C1(H5DA,H6DA)
2.b Aromatic/amide H refined with riding coordinates:
 C7A(H), C18A(HA), C3B(HB), C20C(H20C), C3A(HC), C7C(H7C), C5A(HD), C7B(HK),
 C22A(HL), C18C(H18C), C20A(HQ), C22C(H22C), C5C(H5C), C20B(HT), C18B(HU),
 C5B(HX), C3C(H3C), C22B(H4AA)
2.c Idealised Me refined as rotating group:
 C14B(H9AA,H0BA,H1BA), C14A(H2BA,H3BA,H4BA), C12A(H5BA,H6BA,H7BA), C13B(H8BA,
 H9BA,H0CA), C13A(H1CA,H2CA,H3CA), C14C(H14A,H14B,H14C), C11A(H4CA,H5CA,H6CA),
 C11B(H7CA,H0DA,H1DA), C11C(H11A,H11B,H11C), C12C(H12A,H12B,H12C), C13C(H13A,
 H13B,H13C), C12B(H2DA,H3DA,H4DA)
;
_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
Co1C Co 0.59050(4) 0.33916(4) 0.26509(4) 0.02861(16) Uani 1 1 d . . . . .
Co1A Co 0.43788(4) 0.96005(4) 0.24125(3) 0.02632(16) Uani 1 1 d . . . . .
Co1B Co 0.62034(4) 0.69213(4) 0.28492(3) 0.02737(16) Uani 1 1 d . . . . .
Cl4C Cl 0.24694(8) 0.48449(7) 0.07093(7) 0.0376(3) Uani 1 1 d . . . . .
Cl1A Cl 0.55010(8) 0.94081(7) 0.03826(7) 0.0377(3) Uani 1 1 d . . . . .
Cl2A Cl 0.45687(8) 0.60729(7) 0.00257(7) 0.0403(3) Uani 1 1 d . . . . .
Cl1B Cl 0.28917(8) 0.57912(7) 0.26064(7) 0.0417(3) Uani 1 1 d . . . . .
Cl3B Cl 0.70339(9) 0.61236(8) 0.07556(7) 0.0466(4) Uani 1 1 d . . . . .
Cl1C Cl 0.74994(9) 0.49665(8) 0.51557(7) 0.0495(4) Uani 1 1 d . . . . .
Cl2B Cl 0.34719(9) 0.36295(8) 0.41411(8) 0.0508(4) Uani 1 1 d . . . . .
Si2B Si 0.85685(9) 0.97095(8) 0.55006(8) 0.0322(3) Uani 1 1 d . . . . .
Cl3A Cl 0.62467(9) 1.05352(8) 0.49287(7) 0.0518(4) Uani 1 1 d . . . . .
Cl3C Cl 0.25207(8) 0.23888(8) 0.20340(9) 0.0554(4) Uani 1 1 d . . . . .
Si2A Si 0.04652(9) 0.92090(9) 0.14365(8) 0.0377(4) Uani 1 1 d . . . . .
Si1A Si 0.04304(9) 0.74649(8) 0.17617(9) 0.0388(4) Uani 1 1 d . . . . .
Si1B Si 0.91476(10) 0.81880(9) 0.58323(8) 0.0411(4) Uani 1 1 d . . . . .
Si2C Si 0.90235(9) 0.40253(9) 0.11766(9) 0.0413(4) Uani 1 1 d . . . . .
Cl4B Cl 0.76353(9) 0.91841(9) 0.02909(9) 0.0635(5) Uani 1 1 d . . . . .
Si1C Si 0.82494(10) 0.20936(9) 0.11735(8) 0.0381(4) Uani 1 1 d . . . . .
Cl2C Cl 0.87616(10) 0.25586(9) 0.57353(8) 0.0653(4) Uani 1 1 d . . . . .
Cl4A Cl 0.52900(11) 1.32056(9) 0.53133(8) 0.0721(5) Uani 1 1 d . . . . .
Cl1 Cl 0.93694(12) 0.50794(14) 0.40143(12) 0.1095(7) Uani 1 1 d . . . . .
O1B O 0.49238(18) 0.63583(16) 0.28165(16) 0.0278(8) Uani 1 1 d . . . . .
O1C O 0.6621(2) 0.38869(17) 0.36719(17) 0.0336(8) Uani 1 1 d . . . . .
O2A O 0.51661(19) 1.01836(17) 0.34028(17) 0.0329(8) Uani 1 1 d . . . . .
O1A O 0.48258(19) 0.93531(17) 0.16182(16) 0.0304(8) Uani 1 1 d . . . . .
O2B O 0.6643(2) 0.67961(17) 0.20331(17) 0.0348(8) Uani 1 1 d . . . . .
O2C O 0.45549(18) 0.30504(17) 0.22585(17) 0.0311(8) Uani 1 1 d . . . . .
Cl2 Cl 0.9734(2) 0.37414(15) 0.32356(14) 0.1835(12) Uani 1 1 d . . . . .
N1A N 0.3801(2) 0.8415(2) 0.24461(19) 0.0245(9) Uani 1 1 d . . . . .
N2A N 0.3873(2) 1.0492(2) 0.2246(2) 0.0228(9) Uani 1 1 d . . . . .
O3B O 0.9017(2) 0.90035(18) 0.56072(18) 0.0410(9) Uani 1 1 d . . . . .
N1B N 0.6800(2) 0.6347(2) 0.34973(19) 0.0229(9) Uani 1 1 d . . . . .
N2B N 0.6435(2) 0.8137(2) 0.2982(2) 0.0253(9) Uani 1 1 d . . . . .
O3C O 0.8717(2) 0.31171(18) 0.13636(17) 0.0401(9) Uani 1 1 d . . . . .
N1C N 0.6209(2) 0.2361(2) 0.2572(2) 0.0277(9) Uani 1 1 d . . . . .
N2C N 0.6241(2) 0.4290(2) 0.21463(19) 0.0232(9) Uani 1 1 d . . . . .
C1B C 0.4643(3) 0.5748(2) 0.3119(2) 0.0242(11) Uani 1 1 d . . . . .
C7A C 0.3927(3) 0.7808(3) 0.2063(2) 0.0269(11) Uani 1 1 d . . . . .
H H 0.374480 0.729507 0.218082 0.032 Uiso 1 1 calc R . . . .
C18A C 0.4105(3) 1.1157(3) 0.2760(2) 0.0244(11) Uani 1 1 d . . . . .
HA H 0.389775 1.156874 0.262383 0.029 Uiso 1 1 calc R . . . .
C3B C 0.3318(3) 0.4738(3) 0.3352(2) 0.0290(12) Uani 1 1 d . . . . .
HB H 0.267031 0.450990 0.329399 0.035 Uiso 1 1 calc R . . . .
C19A C 0.4642(3) 1.1341(3) 0.3515(2) 0.0239(11) Uani 1 1 d . . . . .
O3A O 0.0608(2) 0.8404(2) 0.1674(2) 0.0623(12) Uani 1 1 d . . . . .
C1A C 0.4716(3) 0.8599(3) 0.1271(2) 0.0255(11) Uani 1 1 d . . . . .
C2A C 0.5016(3) 0.8504(3) 0.0645(2) 0.0242(11) Uani 1 1 d . . . . .
C20C C 0.4067(3) 0.4592(3) 0.1304(2) 0.0272(11) Uani 1 1 d . . . . .
H20C H 0.437962 0.505143 0.115053 0.033 Uiso 1 1 calc R . . . .
C21C C 0.3102(3) 0.4324(3) 0.1163(2) 0.0270(11) Uani 1 1 d . . . . .
C19C C 0.4595(3) 0.4184(3) 0.1678(2) 0.0225(11) Uani 1 1 d . . . . .
C4A C 0.4611(3) 0.7029(3) 0.0495(2) 0.0257(11) Uani 1 1 d . . . . .
C3A C 0.4962(3) 0.7748(3) 0.0265(2) 0.0275(11) Uani 1 1 d . . . . .
HC H 0.516029 0.771457 -0.014541 0.033 Uiso 1 1 calc R . . . .
C24C C 0.4128(3) 0.3471(3) 0.1918(3) 0.0268(11) Uani 1 1 d . . . . .
C24A C 0.5137(3) 1.0849(3) 0.3801(3) 0.0262(11) Uani 1 1 d . . . . .
C6A C 0.4325(3) 0.7844(3) 0.1468(2) 0.0221(11) Uani 1 1 d . . . . .
C7C C 0.6669(3) 0.2206(3) 0.3141(3) 0.0290(12) Uani 1 1 d . . . . .
H7C H 0.670535 0.167806 0.306974 0.035 Uiso 1 1 calc R . . . .
C5A C 0.4294(3) 0.7075(3) 0.1082(2) 0.0257(11) Uani 1 1 d . . . . .
HD H 0.405278 0.658977 0.122956 0.031 Uiso 1 1 calc R . . . .
C4B C 0.3927(3) 0.4427(2) 0.3738(3) 0.0295(12) Uani 1 1 d . . . . .
C16A C 0.2295(3) 0.9783(2) 0.1270(2) 0.0290(11) Uani 1 1 d . . . . .
HE H 0.199708 0.968429 0.074690 0.035 Uiso 1 1 calc R . . . .
HF H 0.231687 0.925452 0.135257 0.035 Uiso 1 1 calc R . . . .
C17A C 0.3317(3) 1.0433(3) 0.1502(2) 0.0283(11) Uani 1 1 d . . . . .
HG H 0.362583 1.027871 0.116094 0.034 Uiso 1 1 calc R . . . .
HH H 0.330261 1.098122 0.147973 0.034 Uiso 1 1 calc R . . . .
C24B C 0.6879(3) 0.7358(3) 0.1680(2) 0.0270(11) Uani 1 1 d . . . . .
C2B C 0.3663(3) 0.5382(3) 0.3055(2) 0.0254(11) Uani 1 1 d . . . . .
C16B C 0.6811(3) 0.8718(3) 0.4326(2) 0.0283(11) Uani 1 1 d . . . . .
HI H 0.689724 0.820197 0.437749 0.034 Uiso 1 1 calc R . . . .
HJ H 0.650411 0.885787 0.467390 0.034 Uiso 1 1 calc R . . . .
C7B C 0.6272(3) 0.5711(3) 0.3668(2) 0.0266(11) Uani 1 1 d . . . . .
HK H 0.658377 0.541274 0.391054 0.032 Uiso 1 1 calc R . . . .
C1C C 0.7072(3) 0.3555(3) 0.4098(3) 0.0282(12) Uani 1 1 d . . . . .
C22A C 0.5683(3) 1.1824(3) 0.5013(3) 0.0343(12) Uani 1 1 d . . . . .
HL H 0.602793 1.198461 0.551168 0.041 Uiso 1 1 calc R . . . .
C18C C 0.5614(3) 0.4537(3) 0.1812(2) 0.0254(11) Uani 1 1 d . . . . .
H18C H 0.583882 0.500052 0.163336 0.030 Uiso 1 1 calc R . . . .
C17B C 0.6152(3) 0.8555(3) 0.3557(2) 0.0321(12) Uani 1 1 d . . . . .
HM H 0.550738 0.820276 0.351655 0.038 Uiso 1 1 calc R . . . .
HN H 0.614698 0.908717 0.347367 0.038 Uiso 1 1 calc R . . . .
C23B C 0.7091(3) 0.7137(3) 0.1033(3) 0.0311(12) Uani 1 1 d . . . . .
C9C C 0.6458(3) 0.1855(3) 0.1399(2) 0.0330(12) Uani 1 1 d . . . . .
H9CA H 0.656875 0.241194 0.132488 0.040 Uiso 1 1 calc R . . . .
H9CB H 0.612397 0.144749 0.092167 0.040 Uiso 1 1 calc R . . . .
C8A C 0.3354(3) 0.8233(3) 0.3008(2) 0.0300(12) Uani 1 1 d . . . . .
HO H 0.372822 0.866840 0.346655 0.036 Uiso 1 1 calc R . . . .
HP H 0.334563 0.769758 0.309070 0.036 Uiso 1 1 calc R . . . .
C20A C 0.4710(3) 1.2080(3) 0.3993(3) 0.0326(12) Uani 1 1 d . . . . .
HQ H 0.441029 1.241770 0.380703 0.039 Uiso 1 1 calc R . . . .
C6B C 0.5244(3) 0.5412(3) 0.3523(2) 0.0240(11) Uani 1 1 d . . . . .
C19B C 0.6931(3) 0.8203(3) 0.1893(2) 0.0264(11) Uani 1 1 d . . . . .
C6C C 0.7137(3) 0.2757(3) 0.3879(3) 0.0286(12) Uani 1 1 d . . . . .
C22C C 0.2626(3) 0.3637(3) 0.1385(3) 0.0347(13) Uani 1 1 d . . . . .
H22C H 0.196926 0.345275 0.128777 0.042 Uiso 1 1 calc R . . . .
C5C C 0.7654(3) 0.2458(3) 0.4395(3) 0.0332(12) Uani 1 1 d . . . . .
H5C H 0.768821 0.193641 0.424876 0.040 Uiso 1 1 calc R . . . .
C8B C 0.7826(3) 0.6519(3) 0.3685(3) 0.0349(13) Uani 1 1 d . . . . .
HR H 0.801275 0.657234 0.325232 0.042 Uiso 1 1 calc R . . . .
HS H 0.793689 0.604202 0.382540 0.042 Uiso 1 1 calc R . . . .
C20B C 0.7180(3) 0.8753(3) 0.1457(3) 0.0364(13) Uani 1 1 d . . . . .
HT H 0.722914 0.930603 0.160237 0.044 Uiso 1 1 calc R . . . .
C18B C 0.6699(3) 0.8525(3) 0.2523(3) 0.0313(12) Uani 1 1 d . . . . .
HU H 0.674801 0.908134 0.260399 0.038 Uiso 1 1 calc R . . . .
C23A C 0.5642(3) 1.1114(3) 0.4562(3) 0.0317(12) Uani 1 1 d . . . . .
C17C C 0.7248(3) 0.4766(3) 0.2206(2) 0.0297(12) Uani 1 1 d . . . . .
H17A H 0.765363 0.493290 0.271407 0.036 Uiso 1 1 calc R . . . .
H17B H 0.729617 0.527344 0.204761 0.036 Uiso 1 1 calc R . . . .
C15B C 0.7796(3) 0.9426(3) 0.4530(2) 0.0341(12) Uani 1 1 d . . . . .
HV H 0.770737 0.992549 0.442714 0.041 Uiso 1 1 calc R . . . .
HW H 0.812797 0.925797 0.421403 0.041 Uiso 1 1 calc R . . . .
C23C C 0.3128(3) 0.3233(3) 0.1747(3) 0.0284(12) Uani 1 1 d . . . . .
C5B C 0.4880(3) 0.4749(3) 0.3828(2) 0.0291(11) Uani 1 1 d . . . . .
HX H 0.528444 0.453176 0.408872 0.035 Uiso 1 1 calc R . . . .
C3C C 0.8048(3) 0.3700(3) 0.5342(3) 0.0392(13) Uani 1 1 d . . . . .
H3C H 0.834736 0.401268 0.583140 0.047 Uiso 1 1 calc R . . . .
C21A C 0.5210(3) 1.2300(3) 0.4722(3) 0.0403(13) Uani 1 1 d . . . . .
C2C C 0.7547(3) 0.3990(3) 0.4846(3) 0.0339(12) Uani 1 1 d . . . . .
C9B C 0.8452(3) 0.7314(3) 0.4306(3) 0.0434(14) Uani 1 1 d . . . . .
HY H 0.911599 0.743763 0.434908 0.052 Uiso 1 1 calc R . . . .
HZ H 0.830340 0.778323 0.418275 0.052 Uiso 1 1 calc R . . . .
C15A C 0.1675(3) 1.0036(3) 0.1673(3) 0.0357(13) Uani 1 1 d . . . . .
H0AA H 0.161192 1.054081 0.155988 0.043 Uiso 1 1 calc R . . . .
H1AA H 0.199536 1.017574 0.219766 0.043 Uiso 1 1 calc R . . . .
C9A C 0.2338(3) 0.8198(3) 0.2775(3) 0.0363(13) Uani 1 1 d . . . . .
H2AA H 0.234813 0.871838 0.265465 0.044 Uiso 1 1 calc R . . . .
H3AA H 0.210200 0.816421 0.318748 0.044 Uiso 1 1 calc R . . . .
C16C C 0.7588(3) 0.4231(3) 0.1737(3) 0.0362(13) Uani 1 1 d . . . . .
H16A H 0.715546 0.403830 0.123471 0.043 Uiso 1 1 calc R . . . .
H16B H 0.756266 0.373687 0.191161 0.043 Uiso 1 1 calc R . . . .
C8C C 0.5816(3) 0.1697(3) 0.1873(2) 0.0331(12) Uani 1 1 d . . . . .
H8CA H 0.519158 0.166970 0.160282 0.040 Uiso 1 1 calc R . . . .
H8CB H 0.573347 0.115582 0.197609 0.040 Uiso 1 1 calc R . . . .
C10C C 0.7427(3) 0.1800(3) 0.1717(3) 0.0363(12) Uani 1 1 d . . . . .
H10A H 0.731914 0.122707 0.174664 0.044 Uiso 1 1 calc R . . . .
H10B H 0.773671 0.216828 0.221306 0.044 Uiso 1 1 calc R . . . .
C21B C 0.7349(3) 0.8493(3) 0.0829(3) 0.0401(14) Uani 1 1 d . . . . .
C22B C 0.7305(3) 0.7677(3) 0.0607(3) 0.0430(14) Uani 1 1 d . . . . .
H4AA H 0.741809 0.750003 0.017492 0.052 Uiso 1 1 calc R . . . .
C10A C 0.1644(3) 0.7456(3) 0.2118(3) 0.0425(14) Uani 1 1 d . . . . .
H5AA H 0.158182 0.693615 0.225706 0.051 Uiso 1 1 calc R . . . .
H6AA H 0.191593 0.745418 0.172334 0.051 Uiso 1 1 calc R . . . .
C15C C 0.8597(3) 0.4697(3) 0.1742(3) 0.0377(13) Uani 1 1 d . . . . .
H15A H 0.902823 0.489944 0.224516 0.045 Uiso 1 1 calc R . . . .
H15B H 0.861971 0.518400 0.155726 0.045 Uiso 1 1 calc R . . . .
C4C C 0.8103(3) 0.2926(3) 0.5104(3) 0.0383(13) Uani 1 1 d . . . . .
C10B C 0.8329(3) 0.7248(3) 0.5023(3) 0.0460(15) Uani 1 1 d . . . . .
H7AA H 0.842952 0.675135 0.512370 0.055 Uiso 1 1 calc R . . . .
H8AA H 0.767350 0.716016 0.498395 0.055 Uiso 1 1 calc R . . . .
C14B C 0.9596(3) 1.0733(3) 0.5738(3) 0.0496(15) Uani 1 1 d . . . . .
H9AA H 0.999598 1.085715 0.623584 0.074 Uiso 1 1 calc GR . . . .
H0BA H 0.936401 1.117314 0.568575 0.074 Uiso 1 1 calc GR . . . .
H1BA H 0.995943 1.069772 0.541339 0.074 Uiso 1 1 calc GR . . . .
C14A C -0.0225(3) 0.9577(3) 0.1961(3) 0.0576(17) Uani 1 1 d . . . . .
H2BA H -0.080087 0.911179 0.190262 0.086 Uiso 1 1 calc GR . . . .
H3BA H -0.038460 1.000951 0.178120 0.086 Uiso 1 1 calc GR . . . .
H4BA H 0.015233 0.979990 0.247252 0.086 Uiso 1 1 calc GR . . . .
C12A C -0.0245(3) 0.7272(3) 0.2414(3) 0.0524(16) Uani 1 1 d . . . . .
H5BA H 0.007600 0.772257 0.285963 0.079 Uiso 1 1 calc GR . . . .
H6BA H -0.028301 0.674671 0.252310 0.079 Uiso 1 1 calc GR . . . .
H7BA H -0.087811 0.724757 0.219741 0.079 Uiso 1 1 calc GR . . . .
C13B C 0.7858(3) 0.9763(3) 0.6120(3) 0.0559(16) Uani 1 1 d . . . . .
H8BA H 0.742282 0.920396 0.607040 0.084 Uiso 1 1 calc GR . . . .
H9BA H 0.750448 1.010457 0.599293 0.084 Uiso 1 1 calc GR . . . .
H0CA H 0.827872 1.000698 0.661943 0.084 Uiso 1 1 calc GR . . . .
C13A C -0.0139(3) 0.8897(3) 0.0439(3) 0.0605(17) Uani 1 1 d . . . . .
H1CA H 0.023786 0.870264 0.019131 0.091 Uiso 1 1 calc GR . . . .
H2CA H -0.021730 0.937369 0.028696 0.091 Uiso 1 1 calc GR . . . .
H3CA H -0.075495 0.845216 0.031658 0.091 Uiso 1 1 calc GR . . . .
C14C C 0.8451(3) 0.3881(3) 0.0181(3) 0.0626(17) Uani 1 1 d . . . . .
H14A H 0.859802 0.346810 -0.010308 0.094 Uiso 1 1 calc GR . . . .
H14B H 0.868821 0.440793 0.006419 0.094 Uiso 1 1 calc GR . . . .
H14C H 0.777136 0.369173 0.006919 0.094 Uiso 1 1 calc GR . . . .
C11A C -0.0237(3) 0.6686(3) 0.0861(3) 0.0599(17) Uani 1 1 d . . . . .
H4CA H -0.088561 0.664542 0.071002 0.090 Uiso 1 1 calc GR . . . .
H5CA H -0.022970 0.614558 0.089828 0.090 Uiso 1 1 calc GR . . . .
H6CA H 0.005488 0.686083 0.050642 0.090 Uiso 1 1 calc GR . . . .
C11B C 0.8824(3) 0.8068(3) 0.6660(3) 0.0688(18) Uani 1 1 d . . . . .
H7CA H 0.923427 0.855784 0.706086 0.103 Uiso 1 1 calc GR . . . .
H0DA H 0.889710 0.757609 0.678077 0.103 Uiso 1 1 calc GR . . . .
H1DA H 0.817228 0.800779 0.657022 0.103 Uiso 1 1 calc GR . . . .
C11C C 0.9223(3) 0.1713(3) 0.1446(3) 0.070(2) Uani 1 1 d . . . . .
H11A H 0.964583 0.186724 0.116738 0.105 Uiso 1 1 calc GR . . . .
H11B H 0.895506 0.110951 0.135126 0.105 Uiso 1 1 calc GR . . . .
H11C H 0.957211 0.196337 0.196027 0.105 Uiso 1 1 calc GR . . . .
C12C C 0.7567(3) 0.1652(3) 0.0182(3) 0.0644(18) Uani 1 1 d . . . . .
H12A H 0.713071 0.192126 0.004446 0.097 Uiso 1 1 calc GR . . . .
H12B H 0.721543 0.105599 0.008005 0.097 Uiso 1 1 calc GR . . . .
H12C H 0.800008 0.174806 -0.009489 0.097 Uiso 1 1 calc GR . . . .
C13C C 1.0342(3) 0.4502(3) 0.1431(3) 0.071(2) Uani 1 1 d . . . . .
H13A H 1.062726 0.454127 0.193810 0.106 Uiso 1 1 calc GR . . . .
H13B H 1.053367 0.505622 0.135581 0.106 Uiso 1 1 calc GR . . . .
H13C H 1.054773 0.415585 0.112966 0.106 Uiso 1 1 calc GR . . . .
C12B C 1.0408(3) 0.8349(3) 0.6022(3) 0.0734(19) Uani 1 1 d . . . . .
H2DA H 1.058211 0.841424 0.559129 0.110 Uiso 1 1 calc GR . . . .
H3DA H 1.050457 0.786934 0.615392 0.110 Uiso 1 1 calc GR . . . .
H4DA H 1.079784 0.884704 0.641980 0.110 Uiso 1 1 calc GR . . . .
C1 C 0.9672(5) 0.4203(4) 0.4037(4) 0.112(3) Uani 1 1 d . . . . .
H5DA H 1.028602 0.437711 0.441570 0.134 Uiso 1 1 calc R . . . .
H6DA H 0.920195 0.379082 0.417224 0.134 Uiso 1 1 calc R . . . .


_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
Co1C O1C 1.911(3) . ?
Co1C O2C 1.906(3) . ?
Co1C N1C 1.998(3) . ?
Co1C N2C 1.981(3) . ?
Co1A O2A 1.904(3) . ?
Co1A O1A 1.901(3) . ?
Co1A N1A 1.984(3) . ?
Co1A N2A 1.999(3) . ?
Co1B O1B 1.902(3) . ?
Co1B O2B 1.899(3) . ?
Co1B N1B 1.979(3) . ?
Co1B N2B 1.988(3) . ?
Cl4C C21C 1.734(4) . ?
Cl1A C2A 1.731(4) . ?
Cl2A C4A 1.737(4) . ?
Cl1B C2B 1.727(4) . ?
Cl3B C23B 1.726(4) . ?
Cl1C C2C 1.742(4) . ?
Cl2B C4B 1.747(4) . ?
Si2B O3B 1.622(3) . ?
Si2B C15B 1.857(5) . ?
Si2B C14B 1.860(4) . ?
Si2B C13B 1.852(4) . ?
Cl3A C23A 1.720(5) . ?
Cl3C C23C 1.733(4) . ?
Si2A O3A 1.612(3) . ?
Si2A C15A 1.853(4) . ?
Si2A C14A 1.854(4) . ?
Si2A C13A 1.837(5) . ?
Si1A O3A 1.613(3) . ?
Si1A C10A 1.862(4) . ?
Si1A C12A 1.857(4) . ?
Si1A C11A 1.840(5) . ?
Si1B O3B 1.614(3) . ?
Si1B C10B 1.891(5) . ?
Si1B C11B 1.835(5) . ?
Si1B C12B 1.833(4) . ?
Si2C O3C 1.627(3) . ?
Si2C C15C 1.870(4) . ?
Si2C C14C 1.860(5) . ?
Si2C C13C 1.853(4) . ?
Cl4B C21B 1.747(5) . ?
Si1C O3C 1.625(3) . ?
Si1C C10C 1.868(4) . ?
Si1C C11C 1.852(4) . ?
Si1C C12C 1.848(5) . ?
Cl2C C4C 1.747(5) . ?
Cl4A C21A 1.743(4) . ?
Cl1 C1 1.747(7) . ?
O1B C1B 1.305(4) . ?
O1C C1C 1.287(5) . ?
O2A C24A 1.307(4) . ?
O1A C1A 1.309(5) . ?
O2B C24B 1.297(5) . ?
O2C C24C 1.298(5) . ?
Cl2 C1 1.680(7) . ?
N1A C7A 1.293(5) . ?
N1A C8A 1.468(4) . ?
N2A C18A 1.280(5) . ?
N2A C17A 1.462(5) . ?
N1B C7B 1.297(4) . ?
N1B C8B 1.472(5) . ?
N2B C17B 1.477(5) . ?
N2B C18B 1.279(5) . ?
N1C C7C 1.284(5) . ?
N1C C8C 1.473(5) . ?
N2C C18C 1.276(5) . ?
N2C C17C 1.488(4) . ?
C1B C2B 1.421(5) . ?
C1B C6B 1.413(6) . ?
C7A C6A 1.452(5) . ?
C18A C19A 1.423(6) . ?
C3B C4B 1.374(6) . ?
C3B C2B 1.364(5) . ?
C19A C24A 1.425(6) . ?
C19A C20A 1.416(5) . ?
C1A C2A 1.421(5) . ?
C1A C6A 1.417(5) . ?
C2A C3A 1.368(5) . ?
C20C C21C 1.368(5) . ?
C20C C19C 1.407(5) . ?
C21C C22C 1.388(5) . ?
C19C C24C 1.437(5) . ?
C19C C18C 1.447(5) . ?
C4A C3A 1.388(5) . ?
C4A C5A 1.361(5) . ?
C24C C23C 1.417(5) . ?
C24A C23A 1.411(6) . ?
C6A C5A 1.406(5) . ?
C7C C6C 1.445(6) . ?
C4B C5B 1.365(5) . ?
C16A C17A 1.527(5) . ?
C16A C15A 1.522(5) . ?
C24B C23B 1.413(5) . ?
C24B C19B 1.432(6) . ?
C16B C17B 1.514(6) . ?
C16B C15B 1.530(5) . ?
C7B C6B 1.456(5) . ?
C1C C6C 1.430(6) . ?
C1C C2C 1.408(6) . ?
C22A C23A 1.367(5) . ?
C22A C21A 1.382(6) . ?
C23B C22B 1.371(6) . ?
C9C C8C 1.524(5) . ?
C9C C10C 1.531(5) . ?
C8A C9A 1.521(5) . ?
C20A C21A 1.361(6) . ?
C6B C5B 1.406(5) . ?
C19B C20B 1.410(6) . ?
C19B C18B 1.448(5) . ?
C6C C5C 1.410(6) . ?
C22C C23C 1.365(6) . ?
C5C C4C 1.357(6) . ?
C8B C9B 1.520(6) . ?
C20B C21B 1.356(6) . ?
C17C C16C 1.511(5) . ?
C3C C2C 1.361(6) . ?
C3C C4C 1.390(6) . ?
C9B C10B 1.480(6) . ?
C9A C10A 1.526(6) . ?
C16C C15C 1.520(5) . ?
C21B C22B 1.390(6) . ?

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
O1C Co1C N1C 95.69(14) . . ?
O1C Co1C N2C 107.02(13) . . ?
O2C Co1C O1C 123.62(12) . . ?
O2C Co1C N1C 108.62(13) . . ?
O2C Co1C N2C 96.41(13) . . ?
N2C Co1C N1C 128.35(13) . . ?
O2A Co1A N1A 103.54(13) . . ?
O2A Co1A N2A 95.25(14) . . ?
O1A Co1A O2A 125.37(12) . . ?
O1A Co1A N1A 95.87(13) . . ?
O1A Co1A N2A 106.42(13) . . ?
N1A Co1A N2A 134.40(13) . . ?
O1B Co1B N1B 97.47(13) . . ?
O1B Co1B N2B 107.02(12) . . ?
O2B Co1B O1B 124.51(13) . . ?
O2B Co1B N1B 104.16(13) . . ?
O2B Co1B N2B 96.34(13) . . ?
N1B Co1B N2B 130.57(14) . . ?
O3B Si2B C15B 109.02(19) . . ?
O3B Si2B C14B 106.52(19) . . ?
O3B Si2B C13B 110.1(2) . . ?
C15B Si2B C14B 111.0(2) . . ?
C13B Si2B C15B 109.9(2) . . ?
C13B Si2B C14B 110.2(2) . . ?
O3A Si2A C15A 106.81(19) . . ?
O3A Si2A C14A 108.7(2) . . ?
O3A Si2A C13A 108.5(2) . . ?
C15A Si2A C14A 110.5(2) . . ?
C13A Si2A C15A 109.8(2) . . ?
C13A Si2A C14A 112.5(2) . . ?
O3A Si1A C10A 105.27(19) . . ?
O3A Si1A C12A 108.5(2) . . ?
O3A Si1A C11A 109.9(2) . . ?
C12A Si1A C10A 112.2(2) . . ?
C11A Si1A C10A 110.1(2) . . ?
C11A Si1A C12A 110.7(2) . . ?
O3B Si1B C10B 106.3(2) . . ?
O3B Si1B C11B 110.7(2) . . ?
O3B Si1B C12B 107.8(2) . . ?
C11B Si1B C10B 110.6(2) . . ?
C12B Si1B C10B 112.4(2) . . ?
C12B Si1B C11B 109.1(3) . . ?
O3C Si2C C15C 106.75(18) . . ?
O3C Si2C C14C 109.9(2) . . ?
O3C Si2C C13C 108.8(2) . . ?
C14C Si2C C15C 110.4(2) . . ?
C13C Si2C C15C 110.5(2) . . ?
C13C Si2C C14C 110.5(2) . . ?
O3C Si1C C10C 108.04(18) . . ?
O3C Si1C C11C 108.6(2) . . ?
O3C Si1C C12C 109.3(2) . . ?
C11C Si1C C10C 109.7(2) . . ?
C12C Si1C C10C 109.6(2) . . ?
C12C Si1C C11C 111.5(3) . . ?
C1B O1B Co1B 124.9(3) . . ?
C1C O1C Co1C 126.1(3) . . ?
C24A O2A Co1A 125.7(3) . . ?
C1A O1A Co1A 125.5(3) . . ?
C24B O2B Co1B 125.9(3) . . ?
C24C O2C Co1C 124.9(3) . . ?
C7A N1A Co1A 122.0(3) . . ?
C7A N1A C8A 117.8(4) . . ?
C8A N1A Co1A 119.4(3) . . ?
C18A N2A Co1A 121.5(3) . . ?
C18A N2A C17A 118.9(4) . . ?
C17A N2A Co1A 119.3(3) . . ?
Si1B O3B Si2B 159.0(2) . . ?
C7B N1B Co1B 120.3(3) . . ?
C7B N1B C8B 117.6(4) . . ?
C8B N1B Co1B 121.2(3) . . ?
C17B N2B Co1B 118.5(3) . . ?
C18B N2B Co1B 121.2(3) . . ?
C18B N2B C17B 119.6(4) . . ?
Si1C O3C Si2C 155.6(2) . . ?
C7C N1C Co1C 121.5(3) . . ?
C7C N1C C8C 117.0(4) . . ?
C8C N1C Co1C 121.0(3) . . ?
C18C N2C Co1C 121.3(3) . . ?
C18C N2C C17C 116.9(3) . . ?
C17C N2C Co1C 121.5(3) . . ?
O1B C1B C2B 119.3(4) . . ?
O1B C1B C6B 125.1(4) . . ?
C6B C1B C2B 115.6(4) . . ?
N1A C7A C6A 126.6(4) . . ?
N2A C18A C19A 127.9(4) . . ?
C2B C3B C4B 120.0(4) . . ?
C18A C19A C24A 123.8(4) . . ?
C20A C19A C18A 117.0(4) . . ?
C20A C19A C24A 119.1(4) . . ?
Si2A O3A Si1A 163.3(2) . . ?
O1A C1A C2A 119.1(4) . . ?
O1A C1A C6A 125.7(4) . . ?
C6A C1A C2A 115.2(4) . . ?
C1A C2A Cl1A 117.1(3) . . ?
C3A C2A Cl1A 119.7(3) . . ?
C3A C2A C1A 123.2(4) . . ?
C21C C20C C19C 120.9(4) . . ?
C20C C21C Cl4C 120.1(3) . . ?
C20C C21C C22C 120.2(4) . . ?
C22C C21C Cl4C 119.7(3) . . ?
C20C C19C C24C 120.6(4) . . ?
C20C C19C C18C 115.9(4) . . ?
C24C C19C C18C 123.5(4) . . ?
C3A C4A Cl2A 119.8(3) . . ?
C5A C4A Cl2A 120.3(3) . . ?
C5A C4A C3A 120.0(4) . . ?
C2A C3A C4A 119.7(4) . . ?
O2C C24C C19C 124.7(4) . . ?
O2C C24C C23C 120.5(4) . . ?
C23C C24C C19C 114.8(4) . . ?
O2A C24A C19A 124.2(4) . . ?
O2A C24A C23A 118.5(4) . . ?
C23A C24A C19A 117.3(4) . . ?
C1A C6A C7A 123.1(4) . . ?
C5A C6A C7A 116.0(4) . . ?
C5A C6A C1A 120.9(4) . . ?
N1C C7C C6C 127.5(4) . . ?
C4A C5A C6A 120.9(4) . . ?
C3B C4B Cl2B 118.9(3) . . ?
C5B C4B Cl2B 120.0(4) . . ?
C5B C4B C3B 121.1(4) . . ?
C15A C16A C17A 114.4(3) . . ?
N2A C17A C16A 111.8(3) . . ?
O2B C24B C23B 119.1(4) . . ?
O2B C24B C19B 124.6(4) . . ?
C23B C24B C19B 116.2(4) . . ?
C1B C2B Cl1B 118.4(3) . . ?
C3B C2B Cl1B 119.1(3) . . ?
C3B C2B C1B 122.5(4) . . ?
C17B C16B C15B 114.8(4) . . ?
N1B C7B C6B 127.2(4) . . ?
O1C C1C C6C 125.4(4) . . ?
O1C C1C C2C 119.4(4) . . ?
C2C C1C C6C 115.2(4) . . ?
C23A C22A C21A 119.5(5) . . ?
N2C C18C C19C 127.7(4) . . ?
N2B C17B C16B 112.9(3) . . ?
C24B C23B Cl3B 117.7(3) . . ?
C22B C23B Cl3B 119.1(4) . . ?
C22B C23B C24B 123.2(4) . . ?
C8C C9C C10C 114.8(4) . . ?
N1A C8A C9A 111.2(4) . . ?
C21A C20A C19A 120.5(4) . . ?
C1B C6B C7B 124.3(4) . . ?
C5B C6B C1B 121.4(4) . . ?
C5B C6B C7B 114.3(4) . . ?
C24B C19B C18B 123.6(4) . . ?
C20B C19B C24B 119.4(4) . . ?
C20B C19B C18B 116.9(4) . . ?
C1C C6C C7C 123.3(4) . . ?
C5C C6C C7C 116.2(4) . . ?
C5C C6C C1C 120.4(4) . . ?
C23C C22C C21C 119.5(4) . . ?
C4C C5C C6C 120.4(4) . . ?
N1B C8B C9B 113.3(4) . . ?
C21B C20B C19B 121.4(5) . . ?
N2B C18B C19B 127.8(4) . . ?
C24A C23A Cl3A 118.7(4) . . ?
C22A C23A Cl3A 119.0(4) . . ?
C22A C23A C24A 122.3(4) . . ?
N2C C17C C16C 110.7(3) . . ?
C16B C15B Si2B 115.4(3) . . ?
C24C C23C Cl3C 117.3(4) . . ?
C22C C23C Cl3C 118.7(3) . . ?
C22C C23C C24C 124.0(4) . . ?
C4B C5B C6B 119.5(4) . . ?
C2C C3C C4C 118.7(5) . . ?
C22A C21A Cl4A 118.1(4) . . ?
C20A C21A Cl4A 120.7(4) . . ?
C20A C21A C22A 121.2(4) . . ?
C1C C2C Cl1C 118.0(4) . . ?
C3C C2C Cl1C 117.8(4) . . ?
C3C C2C C1C 124.2(4) . . ?
C10B C9B C8B 113.3(4) . . ?
C16A C15A Si2A 113.9(3) . . ?
C8A C9A C10A 114.2(4) . . ?
C17C C16C C15C 113.3(3) . . ?
N1C C8C C9C 112.3(3) . . ?
C9C C10C Si1C 114.2(3) . . ?
C20B C21B Cl4B 120.4(4) . . ?
C20B C21B C22B 120.6(4) . . ?
C22B C21B Cl4B 119.0(4) . . ?
C23B C22B C21B 119.1(5) . . ?
C9A C10A Si1A 114.8(3) . . ?
C16C C15C Si2C 113.1(3) . . ?
C5C C4C Cl2C 120.0(4) . . ?
C5C C4C C3C 121.1(5) . . ?
C3C C4C Cl2C 118.9(4) . . ?
C9B C10B Si1B 115.5(3) . . ?
Cl2 C1 Cl1 113.7(4) . . ?

_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 1.204
_oxdiff_exptl_absorpt_empirical_full_min 0.795
####################################################################### 
# 
# This file contains crystal structure data downloaded from the 
# Cambridge Structural Database (CSD) hosted by the Cambridge 
# Crystallographic Data Centre (CCDC).
# 
# Full information about CCDC data access policies and citation 
# guidelines are available at http://www.ccdc.cam.ac.uk/access/V1 
# 
# Audit and citation data items may have been added by the CCDC. 
# Please retain this information to preserve the provenance of 
# this file and to allow appropriate attribution of the data. 
# 
#######################################################################

data_shi_4158_mada
_database_code_depnum_ccdc_archive 'CCDC 1982364'
loop_
_audit_author_name
_audit_author_address
'Dascalu Mihaela'
;Petru Poni Institute of Macromolecular Chemistry, Iasi
Romania
;
_audit_update_record             
;
2021-08-01 deposited with the CCDC.	2021-08-20 downloaded from the CCDC.
;
_audit_creation_date             2021-07-30
_audit_creation_method           
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_shelx_SHELXL_version_number     2018/3
# end Validation Reply Form
_chemical_name_common            ?
_chemical_name_systematic        ?
_chemical_formula_moiety         '2(C24 H34 Cu N2 O5 Si2)'
_chemical_formula_sum            'C48 H68 Cu2 N4 O10 Si4'
_chemical_formula_weight         1100.50
_chemical_melting_point          ?
_chemical_oxdiff_formula         C20H20N2O5Si1Cl2Mn1
_chemical_oxdiff_usercomment     DS36
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'
Cu Cu 0.3201 1.2651 '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'
Si Si 0.0817 0.0704 '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      monoclinic
_space_group_IT_number           14
_space_group_name_H-M_alt        'P 1 21/c 1'
_space_group_name_Hall           '-P 2ybc'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, y+1/2, -z+1/2'
'-x, -y, -z'
'x, -y-1/2, z-1/2'

_cell_length_a                   14.9833(18)
_cell_length_b                   14.3565(11)
_cell_length_c                   26.913(2)
_cell_angle_alpha                90
_cell_angle_beta                 96.812(10)
_cell_angle_gamma                90
_cell_volume                     5748.3(9)
_cell_formula_units_Z            4
_cell_measurement_reflns_used    2938
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      22.1850
_cell_measurement_theta_min      1.6330
_shelx_estimated_absorpt_T_max   0.966
_shelx_estimated_absorpt_T_min   0.880
_exptl_absorpt_coefficient_mu    0.877
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.68391
_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            'clear light brown'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   light
_exptl_crystal_colour_primary    brown
_exptl_crystal_density_diffrn    1.272
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       plate
_exptl_crystal_F_000             2312
_exptl_crystal_size_max          0.15
_exptl_crystal_size_mid          0.15
_exptl_crystal_size_min          0.04
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.1282
_diffrn_reflns_av_unetI/netI     0.2586
_diffrn_reflns_Laue_measured_fraction_full 0.996
_diffrn_reflns_Laue_measured_fraction_max 0.996
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       32
_diffrn_reflns_limit_l_min       -30
_diffrn_reflns_number            21655
_diffrn_reflns_point_group_measured_fraction_full 0.996
_diffrn_reflns_point_group_measured_fraction_max 0.996
_diffrn_reflns_theta_full        25.027
_diffrn_reflns_theta_max         25.027
_diffrn_reflns_theta_min         1.610
_diffrn_ambient_temperature      293(2)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 8.0797
_diffrn_detector_type            Eos
_diffrn_measured_fraction_theta_full 0.996
_diffrn_measured_fraction_theta_max 0.996
_diffrn_measurement_details      
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  tₑₓₚ   ω     θ     κ     φ   Frames
#--------------------------------------------------------------------------
  1  ω    -18.00  25.00   1.00  100.00    --  -20.27 -99.00 150.00   43
  2  ω    -44.00  52.00   1.00  100.00    --  -20.27  77.00  60.00   96
  3  ω     65.00  91.00   1.00  100.00    --   22.30  57.00   0.00   26
  4  ω    -48.00  46.00   1.00  100.00    --   22.30 -57.00-150.00   94
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'Xcalibur, Eos'
_diffrn_measurement_method       'ω scans'
_diffrn_orient_matrix_type       
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      -0.0424808000
_diffrn_orient_matrix_UB_12      -0.0034693000
_diffrn_orient_matrix_UB_13      0.0090170000
_diffrn_orient_matrix_UB_21      -0.0064058000
_diffrn_orient_matrix_UB_22      0.0486791000
_diffrn_orient_matrix_UB_23      -0.0033837000
_diffrn_orient_matrix_UB_31      -0.0206674000
_diffrn_orient_matrix_UB_32      -0.0078865000
_diffrn_orient_matrix_UB_33      -0.0247165000
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_source                   'fine-focus sealed X-ray tube'
_diffrn_source_type              'Enhance (Mo) X-ray Source'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                3345
_reflns_number_total             10114
_reflns_odcompleteness_completeness 99.92
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     26.32
_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    'olex2.solve (Bourhis et al., 2015)'
_refine_diff_density_max         0.342
_refine_diff_density_min         -0.335
_refine_diff_density_rms         0.061
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.822
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     613
_refine_ls_number_reflns         10114
_refine_ls_number_restraints     24
_refine_ls_R_factor_all          0.2303
_refine_ls_R_factor_gt           0.0656
_refine_ls_restrained_S_all      0.823
_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)] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0774
_refine_ls_wR_factor_ref         0.1242
_refine_special_details          ?
_olex2_refinement_description    
;
1. Others
 Fixed Uiso: H2A(0.114) H5A(0.201) H3A(0.103) H4A(0.128) H5AA(0.107)
 H7A(0.081) H8AA(0.098) H8AB(0.098) H9AA(0.087) H9AB(0.087) H10A(0.096)
 H10B(0.096) H11A(0.251) H11B(0.251) H11C(0.251) H12A(0.215) H12B(0.215)
 H12C(0.215) H13A(0.199) H13B(0.199) H13C(0.199) H14A(0.209) H14B(0.209)
 H14C(0.209) H15A(0.111) H15B(0.111) H16A(0.103) H16B(0.103) H17A(0.082)
 H17B(0.082) H18A(0.084) H20A(0.137) H21A(0.166) H22A(0.156) H2B(0.176)
 H5B(0.164) H3B(0.123) H4B(0.147) H5BA(0.137) H7B(0.093) H8BA(0.092)
 H8BB(0.092) H9BA(0.106) H9BB(0.106) H10C(0.108) H10D(0.108) H11D(0.201)
 H11E(0.201) H11F(0.201) H12D(0.152) H12E(0.152) H12F(0.152) H13D(0.161)
 H13E(0.161) H13F(0.161) H14D(0.158) H14E(0.158) H14F(0.158) H15C(0.109)
 H15D(0.109) H16C(0.098) H16D(0.098) H17C(0.095) H17D(0.095) H18B(0.09)
 H20B(0.102) H21B(0.126) H22B(0.118)
 Fixed X: H2A(0.367937) H5A(0.087544) H3A(0.27018) H4A(0.131854)
 H5AA(0.062677) H7A(0.061539) H8AA(0.030372) H8AB(0.069161) H9AA(0.190555)
 H9AB(0.098301) H10A(0.188066) H10B(0.097777) H11A(0.193516) H11B(0.102826)
 H11C(0.139956) H12A(0.256459) H12B(0.187469) H12C(0.288929) H13A(0.478652)
 H13B(0.530572) H13C(0.435722) H14A(0.434634) H14B(0.524924) H14C(0.444264)
 H15A(0.410602) H15B(0.508624) H16A(0.370362) H16B(0.471805) H17A(0.503877)
 H17B(0.439687) H18A(0.461511) H20A(0.444321) H21A(0.356806) H22A(0.202488)
 H2B(0.089261) H5B(0.497773) H3B(-0.102414) H4B(-0.123537) H5BA(-0.016244)
 H7B(0.125859) H8BA(0.245668) H8BB(0.334717) H9BA(0.302123) H9BB(0.318046)
 H10C(0.143972) H10D(0.169593) H11D(0.032807) H11E(0.075927) H11F(0.074717)
 H12D(0.273107) H12E(0.275507) H12F(0.336397) H13D(0.099737) H13E(0.124847)
 H13F(0.073137) H14D(0.363967) H14E(0.314377) H14F(0.286207) H15C(0.325052)
 H15D(0.301994) H16C(0.185222) H16D(0.168447) H17C(0.291715) H17D(0.216151)
 H18B(0.424261) H20B(0.575685) H21B(0.700334) H22B(0.6867)
 Fixed Y: H2A(0.476415) H5A(0.716499) H3A(0.326506) H4A(0.262851)
 H5AA(0.288078) H7A(0.356472) H8AA(0.406083) H8AB(0.503791) H9AA(0.428654)
 H9AB(0.405512) H10A(0.282885) H10B(0.259797) H11A(0.248846) H11B(0.227606)
 H11C(0.329736) H12A(0.106227) H12B(0.083627) H12C(0.100227) H13A(0.162772)
 H13B(0.215442) H13C(0.172382) H14A(0.406621) H14B(0.353771) H14C(0.301381)
 H15A(0.463851) H15B(0.425983) H16A(0.36978) H16B(0.343681) H17A(0.502355)
 H17B(0.456911) H18A(0.633381) H20A(0.783251) H21A(0.89714) H22A(0.875195)
 H2B(0.658577) H5B(0.497367) H3B(0.581163) H4B(0.495448) H5BA(0.492875)
 H7B(0.541463) H8BA(0.562171) H8BB(0.581849) H9BA(0.74371) H9BB(0.701737)
 H10C(0.727641) H10D(0.706536) H11D(0.873851) H11E(0.875831) H11F(0.966331)
 H12D(0.96629) H12E(0.86483) H12F(0.89135) H13D(1.09311) H13E(1.08848)
 H13F(1.0056) H14D(1.052819) H14E(1.132159) H14F(1.108789) H15C(0.898843)
 H15D(0.984865) H16C(0.834067) H16D(0.918009) H17C(0.86909) H17D(0.792909)
 H18B(0.823347) H20B(0.790081) H21B(0.70983) H22B(0.586966)
 Fixed Z: H2A(0.675477) H5A(0.850623) H3A(0.594876) H4A(0.603145)
 H5AA(0.673844) H7A(0.753394) H8AA(0.821388) H8AB(0.838957) H9AA(0.88685)
 H9AB(0.905668) H10A(0.847128) H10B(0.868389) H11A(1.016707) H11B(0.983327)
 H11C(0.987577) H12A(0.893024) H12B(0.930814) H12C(0.950514) H13A(0.958107)
 H13B(0.919347) H13C(0.902317) H14A(1.017596) H14B(1.013166) H14C(1.032816)
 H15A(0.910149) H15B(0.911846) H16A(0.84023) H16B(0.840788) H17A(0.824697)
 H17B(0.780901) H18A(0.854887) H20A(0.88497) H21A(0.914219) H22A(0.912731)
 H2B(0.787244) H5B(0.659643) H3B(0.73707) H4B(0.664082) H5BA(0.611745)
 H7B(0.590231) H8BA(0.55781) H8BB(0.593098) H9BA(0.588197) H9BB(0.53631)
 H10C(0.561905) H10D(0.508292) H11D(0.508172) H11E(0.457882) H11F(0.490382)
 H12D(0.480041) H12E(0.458701) H12F(0.508101) H13D(0.602263) H13E(0.660423)
 H13F(0.632103) H14D(0.601894) H14E(0.627784) H14F(0.571184) H15C(0.670876)
 H15D(0.70258) H16C(0.682231) H16D(0.717067) H17C(0.77454) H17D(0.767562)
 H18B(0.769954) H20B(0.786299) H21B(0.768617) H22B(0.713676)
;
_atom_sites_solution_hydrogens   mixed
_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
Cu1A Cu 0.25009(6) 0.51816(7) 0.79599(3) 0.0615(3) Uani 1 1 d . . . . .
Si1A Si 0.41837(16) 0.31406(19) 0.94487(8) 0.0773(8) Uani 1 1 d . . . . .
Si2A Si 0.21788(17) 0.2442(2) 0.93213(8) 0.0820(8) Uani 1 1 d . . . . .
O1A O 0.2881(3) 0.4706(4) 0.73621(14) 0.0640(15) Uani 1 1 d . . . . .
O2A O 0.3656(3) 0.4297(4) 0.65497(15) 0.0763(16) Uani 1 1 d . . . . .
H2A H 0.367937 0.476415 0.675477 0.114 Uiso 1 1 d R . . . .
O4A O 0.2037(4) 0.6098(4) 0.83821(16) 0.0734(16) Uani 1 1 d . . . . .
O5A O 0.1087(5) 0.7391(5) 0.8783(2) 0.134(3) Uani 1 1 d . . . . .
H5A H 0.087544 0.716499 0.850623 0.201 Uiso 1 1 d R . . . .
O3A O 0.3125(3) 0.2997(4) 0.94155(18) 0.0948(19) Uani 1 1 d . . . . .
N1A N 0.1421(4) 0.4404(5) 0.7903(2) 0.0609(18) Uani 1 1 d . . . . .
N2A N 0.3757(4) 0.5468(5) 0.82216(18) 0.0571(17) Uani 1 1 d . . . . .
C1A C 0.2436(5) 0.4135(5) 0.7042(2) 0.055(2) Uani 1 1 d . . . . .
C2A C 0.2832(6) 0.3941(5) 0.6605(3) 0.062(2) Uani 1 1 d . . . . .
C3A C 0.2425(6) 0.3384(6) 0.6234(3) 0.086(3) Uani 1 1 d . . . . .
H3A H 0.270180 0.326506 0.594876 0.103 Uiso 1 1 calc R . . . .
C4A C 0.1600(7) 0.2999(7) 0.6287(3) 0.107(4) Uani 1 1 d . . . . .
H4A H 0.131854 0.262851 0.603145 0.128 Uiso 1 1 calc R . . . .
C5A C 0.1182(6) 0.3148(6) 0.6706(3) 0.089(3) Uani 1 1 d . . . . .
H5AA H 0.062677 0.288078 0.673844 0.107 Uiso 1 1 calc R . . . .
C6A C 0.1626(5) 0.3729(6) 0.7094(3) 0.061(2) Uani 1 1 d . . . . .
C7A C 0.1157(5) 0.3878(6) 0.7527(3) 0.068(2) Uani 1 1 d . . . . .
H7A H 0.061539 0.356472 0.753394 0.081 Uiso 1 1 calc R . . . .
C8A C 0.0853(5) 0.4403(6) 0.8316(2) 0.082(3) Uani 1 1 d . . . . .
H8AA H 0.030372 0.406083 0.821388 0.098 Uiso 1 1 calc R . . . .
H8AB H 0.069161 0.503791 0.838957 0.098 Uiso 1 1 calc R . . . .
C9A C 0.1342(5) 0.3960(6) 0.8784(2) 0.072(2) Uani 1 1 d . . . . .
H9AA H 0.190555 0.428654 0.886850 0.087 Uiso 1 1 calc R . . . .
H9AB H 0.098301 0.405512 0.905668 0.087 Uiso 1 1 calc R . . . .
C10A C 0.1541(5) 0.2933(5) 0.8752(2) 0.080(3) Uani 1 1 d . . . . .
H10A H 0.188066 0.282885 0.847128 0.096 Uiso 1 1 calc R . . . .
H10B H 0.097777 0.259797 0.868389 0.096 Uiso 1 1 calc R . . . .
C11A C 0.1562(5) 0.2651(8) 0.9865(2) 0.168(6) Uani 1 1 d . . . . .
H11A H 0.193516 0.248846 1.016707 0.251 Uiso 1 1 d R . . . .
H11B H 0.102826 0.227606 0.983327 0.251 Uiso 1 1 d R . . . .
H11C H 0.139956 0.329736 0.987577 0.251 Uiso 1 1 d R . . . .
C12A C 0.2404(6) 0.1185(6) 0.9259(3) 0.144(4) Uani 1 1 d . . . . .
H12A H 0.256459 0.106227 0.893024 0.215 Uiso 1 1 d R . . . .
H12B H 0.187469 0.083627 0.930814 0.215 Uiso 1 1 d R . . . .
H12C H 0.288929 0.100227 0.950514 0.215 Uiso 1 1 d R . . . .
C13A C 0.4723(6) 0.2027(6) 0.9293(3) 0.133(4) Uani 1 1 d . . . . .
H13A H 0.478652 0.162772 0.958107 0.199 Uiso 1 1 d R . . . .
H13B H 0.530572 0.215442 0.919347 0.199 Uiso 1 1 d R . . . .
H13C H 0.435722 0.172382 0.902317 0.199 Uiso 1 1 d R . . . .
C14A C 0.4607(5) 0.3480(7) 1.0100(2) 0.139(4) Uani 1 1 d . . . . .
H14A H 0.434634 0.406621 1.017596 0.209 Uiso 1 1 d R . . . .
H14B H 0.524924 0.353771 1.013166 0.209 Uiso 1 1 d R . . . .
H14C H 0.444264 0.301381 1.032816 0.209 Uiso 1 1 d R . . . .
C15A C 0.4459(5) 0.4098(6) 0.9031(2) 0.092(3) Uani 1 1 d . . . . .
H15A H 0.410602 0.463851 0.910149 0.111 Uiso 1 1 calc R . . . .
H15B H 0.508624 0.425983 0.911846 0.111 Uiso 1 1 calc R . . . .
C16A C 0.4312(5) 0.3927(6) 0.8487(2) 0.086(3) Uani 1 1 d . . . . .
H16A H 0.370362 0.369780 0.840230 0.103 Uiso 1 1 calc R . . . .
H16B H 0.471805 0.343681 0.840788 0.103 Uiso 1 1 calc R . . . .
C17A C 0.4445(4) 0.4762(6) 0.8157(2) 0.069(2) Uani 1 1 d . . . . .
H17A H 0.503877 0.502355 0.824697 0.082 Uiso 1 1 calc R . . . .
H17B H 0.439687 0.456911 0.780901 0.082 Uiso 1 1 calc R . . . .
C18A C 0.4002(6) 0.6235(6) 0.8466(2) 0.070(2) Uani 1 1 d . . . . .
H18A H 0.461511 0.633381 0.854887 0.084 Uiso 1 1 calc R . . . .
C19A C 0.3413(8) 0.6923(7) 0.8613(3) 0.077(3) Uani 1 1 d . . . . .
C20A C 0.3824(8) 0.7753(8) 0.8830(3) 0.114(4) Uani 1 1 d . U . . .
H20A H 0.444321 0.783251 0.884970 0.137 Uiso 1 1 calc R . . . .
C21A C 0.3304(10) 0.8426(10) 0.9009(4) 0.139(6) Uani 1 1 d . U . . .
H21A H 0.356806 0.897140 0.914219 0.166 Uiso 1 1 calc R . . . .
C22A C 0.2371(10) 0.8300(9) 0.8993(4) 0.130(6) Uani 1 1 d . . . . .
H22A H 0.202488 0.875195 0.912731 0.156 Uiso 1 1 calc R . . . .
C23A C 0.1970(9) 0.7518(9) 0.8782(3) 0.100(4) Uani 1 1 d . U . . .
C24A C 0.2489(8) 0.6828(7) 0.8579(3) 0.072(3) Uani 1 1 d . U . . .
Cu1B Cu 0.27943(6) 0.65444(7) 0.69102(3) 0.0628(3) Uani 1 1 d . . . . .
Si1B Si 0.18933(18) 0.8670(2) 0.52557(8) 0.0846(8) Uani 1 1 d . . . . .
Si2B Si 0.22488(17) 0.99749(19) 0.62109(8) 0.0796(8) Uani 1 1 d . . . . .
O1B O 0.1693(4) 0.6541(4) 0.71915(16) 0.0799(17) Uani 1 1 d . . . . .
O2B O 0.0366(4) 0.6645(5) 0.7753(2) 0.117(2) Uani 1 1 d . . . . .
H2B H 0.089261 0.658577 0.787244 0.176 Uiso 1 1 d R . . . .
O4B O 0.3966(3) 0.6143(4) 0.68086(16) 0.0700(16) Uani 1 1 d . . . . .
O5B O 0.5480(4) 0.5215(4) 0.6640(2) 0.110(2) Uani 1 1 d . . . . .
H5B H 0.497773 0.497367 0.659643 0.164 Uiso 1 1 d R . . . .
O3B O 0.2041(4) 0.9200(4) 0.57816(17) 0.123(2) Uani 1 1 d . . . . .
N1B N 0.2240(5) 0.6013(5) 0.6268(2) 0.0647(19) Uani 1 1 d . . . . .
N2B N 0.3263(5) 0.7576(4) 0.73574(19) 0.0595(18) Uani 1 1 d . . . . .
C1B C 0.0946(6) 0.6146(6) 0.7012(3) 0.071(3) Uani 1 1 d . . . . .
C2B C 0.0225(6) 0.6174(7) 0.7312(3) 0.084(3) Uani 1 1 d . . . . .
C3B C -0.0562(6) 0.5765(7) 0.7170(3) 0.103(3) Uani 1 1 d . U . . .
H3B H -0.102414 0.581163 0.737070 0.123 Uiso 1 1 calc R . . . .
C4B C -0.0697(7) 0.5270(8) 0.6727(4) 0.123(4) Uani 1 1 d . U . . .
H4B H -0.123537 0.495448 0.664082 0.147 Uiso 1 1 calc R . . . .
C5B C -0.0056(7) 0.5245(8) 0.6420(3) 0.114(4) Uani 1 1 d . . . . .
H5BA H -0.016244 0.492875 0.611745 0.137 Uiso 1 1 calc R . . . .
C6B C 0.0785(6) 0.5694(7) 0.6550(3) 0.082(3) Uani 1 1 d . . . . .
C7B C 0.1438(6) 0.5691(6) 0.6211(3) 0.078(3) Uani 1 1 d . . . . .
H7B H 0.125859 0.541463 0.590231 0.093 Uiso 1 1 calc R . . . .
C8B C 0.2739(5) 0.6038(6) 0.5834(2) 0.077(3) Uani 1 1 d . . . . .
H8BA H 0.245668 0.562171 0.557810 0.092 Uiso 1 1 calc R . . . .
H8BB H 0.334717 0.581849 0.593098 0.092 Uiso 1 1 calc R . . . .
C9B C 0.2773(5) 0.7019(6) 0.5618(3) 0.088(3) Uani 1 1 d . . . . .
H9BA H 0.302123 0.743710 0.588197 0.106 Uiso 1 1 calc R . . . .
H9BB H 0.318046 0.701737 0.536310 0.106 Uiso 1 1 calc R . . . .
C10B C 0.1883(5) 0.7397(6) 0.5392(2) 0.090(3) Uani 1 1 d . . . . .
H10C H 0.143972 0.727641 0.561905 0.108 Uiso 1 1 calc R . . . .
H10D H 0.169593 0.706536 0.508292 0.108 Uiso 1 1 calc R . . . .
C11B C 0.0802(5) 0.8997(6) 0.4914(3) 0.134(4) Uani 1 1 d . . . . .
H11D H 0.032807 0.873851 0.508172 0.201 Uiso 1 1 d R . . . .
H11E H 0.075927 0.875831 0.457882 0.201 Uiso 1 1 d R . . . .
H11F H 0.074717 0.966331 0.490382 0.201 Uiso 1 1 d R . . . .
C12B C 0.2793(5) 0.9016(6) 0.4887(2) 0.101(3) Uani 1 1 d . . . . .
H12D H 0.273107 0.966290 0.480041 0.152 Uiso 1 1 d R . . . .
H12E H 0.275507 0.864830 0.458701 0.152 Uiso 1 1 d R . . . .
H12F H 0.336397 0.891350 0.508101 0.152 Uiso 1 1 d R . . . .
C13B C 0.1180(5) 1.0528(6) 0.6301(3) 0.107(3) Uani 1 1 d . . . . .
H13D H 0.099737 1.093110 0.602263 0.161 Uiso 1 1 d R . . . .
H13E H 0.124847 1.088480 0.660423 0.161 Uiso 1 1 d R . . . .
H13F H 0.073137 1.005600 0.632103 0.161 Uiso 1 1 d R . . . .
C14B C 0.3072(5) 1.0831(6) 0.6034(2) 0.105(3) Uani 1 1 d . . . . .
H14D H 0.363967 1.052819 0.601894 0.158 Uiso 1 1 d R . . . .
H14E H 0.314377 1.132159 0.627784 0.158 Uiso 1 1 d R . . . .
H14F H 0.286207 1.108789 0.571184 0.158 Uiso 1 1 d R . . . .
C15B C 0.2761(5) 0.9377(5) 0.6794(2) 0.091(3) Uani 1 1 d . . . . .
H15C H 0.325052 0.898843 0.670876 0.109 Uiso 1 1 calc R . . . .
H15D H 0.301994 0.984865 0.702580 0.109 Uiso 1 1 calc R . . . .
C16B C 0.2147(5) 0.8786(5) 0.7059(2) 0.081(3) Uani 1 1 d . . . . .
H16C H 0.185222 0.834067 0.682231 0.098 Uiso 1 1 calc R . . . .
H16D H 0.168447 0.918009 0.717067 0.098 Uiso 1 1 calc R . . . .
C17B C 0.2610(5) 0.8253(5) 0.7509(2) 0.079(3) Uani 1 1 d . . . . .
H17C H 0.291715 0.869090 0.774540 0.095 Uiso 1 1 calc R . . . .
H17D H 0.216151 0.792909 0.767562 0.095 Uiso 1 1 calc R . . . .
C18B C 0.4102(7) 0.7710(6) 0.7502(2) 0.075(3) Uani 1 1 d . . . . .
H18B H 0.424261 0.823347 0.769954 0.090 Uiso 1 1 calc R . . . .
C19B C 0.4844(6) 0.7149(6) 0.7396(3) 0.069(2) Uani 1 1 d . . . . .
C20B C 0.5700(7) 0.7409(6) 0.7637(3) 0.085(3) Uani 1 1 d . . . . .
H20B H 0.575685 0.790081 0.786299 0.102 Uiso 1 1 calc R . . . .
C21B C 0.6438(7) 0.6929(8) 0.7532(4) 0.105(4) Uani 1 1 d . . . . .
H21B H 0.700334 0.709830 0.768617 0.126 Uiso 1 1 calc R . . . .
C22B C 0.6357(6) 0.6197(7) 0.7201(3) 0.098(3) Uani 1 1 d . . . . .
H22B H 0.686700 0.586966 0.713676 0.118 Uiso 1 1 calc R . . . .
C23B C 0.5529(6) 0.5943(6) 0.6964(3) 0.075(2) Uani 1 1 d . . . . .
C24B C 0.4738(6) 0.6414(6) 0.7054(3) 0.063(2) 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
Cu1A O1A 1.896(4) . ?
Cu1A O4A 1.922(5) . ?
Cu1A N1A 1.957(6) . ?
Cu1A N2A 1.972(6) . ?
Si1A O3A 1.591(5) . ?
Si1A C13A 1.862(8) . ?
Si1A C14A 1.856(7) . ?
Si1A C15A 1.854(7) . ?
Si2A O3A 1.620(6) . ?
Si2A C10A 1.847(7) . ?
Si2A C11A 1.845(7) . ?
Si2A C12A 1.848(8) . ?
O1A C1A 1.314(7) . ?
O2A C2A 1.361(8) . ?
O4A C24A 1.324(9) . ?
O5A C23A 1.337(12) . ?
N1A C7A 1.287(8) . ?
N1A C8A 1.479(7) . ?
N2A C17A 1.471(8) . ?
N2A C18A 1.313(9) . ?
C1A C2A 1.406(8) . ?
C1A C6A 1.369(9) . ?
C2A C3A 1.365(9) . ?
C3A C4A 1.377(10) . ?
C4A C5A 1.370(9) . ?
C5A C6A 1.435(9) . ?
C6A C7A 1.445(9) . ?
C8A C9A 1.518(8) . ?
C9A C10A 1.509(9) . ?
C15A C16A 1.475(7) . ?
C16A C17A 1.520(9) . ?
C18A C19A 1.412(10) . ?
C19A C20A 1.434(12) . ?
C19A C24A 1.383(11) . ?
C20A C21A 1.364(13) . ?
C21A C22A 1.404(15) . ?
C22A C23A 1.366(15) . ?
C23A C24A 1.408(12) . ?
Cu1B O1B 1.896(5) . ?
Cu1B O4B 1.898(5) . ?
Cu1B N1B 1.980(6) . ?
Cu1B N2B 1.984(6) . ?
Si1B O3B 1.599(5) . ?
Si1B C10B 1.864(8) . ?
Si1B C11B 1.839(8) . ?
Si1B C12B 1.834(7) . ?
Si2B O3B 1.608(6) . ?
Si2B C13B 1.829(7) . ?
Si2B C14B 1.844(7) . ?
Si2B C15B 1.872(7) . ?
O1B C1B 1.296(9) . ?
O2B C2B 1.361(9) . ?
O4B C24B 1.320(8) . ?
O5B C23B 1.357(9) . ?
N1B C7B 1.280(9) . ?
N1B C8B 1.460(8) . ?
N2B C17B 1.470(8) . ?
N2B C18B 1.286(9) . ?
C1B C2B 1.423(10) . ?
C1B C6B 1.397(10) . ?
C2B C3B 1.333(11) . ?
C3B C4B 1.382(11) . ?
C4B C5B 1.339(10) . ?
C5B C6B 1.421(11) . ?
C6B C7B 1.416(10) . ?
C8B C9B 1.527(9) . ?
C9B C10B 1.501(9) . ?
C15B C16B 1.494(9) . ?
C16B C17B 1.529(8) . ?
C18B C19B 1.428(10) . ?
C19B C20B 1.417(10) . ?
C19B C24B 1.398(10) . ?
C20B C21B 1.361(11) . ?
C21B C22B 1.374(11) . ?
C22B C23B 1.375(11) . ?
C23B C24B 1.411(10) . ?

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
O1A Cu1A O4A 156.1(2) . . ?
O1A Cu1A N1A 93.3(2) . . ?
O1A Cu1A N2A 90.5(2) . . ?
O4A Cu1A N1A 94.8(2) . . ?
O4A Cu1A N2A 92.4(2) . . ?
N1A Cu1A N2A 153.1(2) . . ?
O3A Si1A C13A 109.4(4) . . ?
O3A Si1A C14A 108.3(3) . . ?
O3A Si1A C15A 110.7(4) . . ?
C14A Si1A C13A 109.2(4) . . ?
C15A Si1A C13A 111.5(3) . . ?
C15A Si1A C14A 107.6(4) . . ?
O3A Si2A C10A 107.4(4) . . ?
O3A Si2A C11A 107.9(4) . . ?
O3A Si2A C12A 109.2(4) . . ?
C10A Si2A C12A 112.3(4) . . ?
C11A Si2A C10A 109.7(4) . . ?
C11A Si2A C12A 110.2(5) . . ?
C1A O1A Cu1A 127.0(5) . . ?
C24A O4A Cu1A 125.1(6) . . ?
Si1A O3A Si2A 157.0(4) . . ?
C7A N1A Cu1A 124.8(5) . . ?
C7A N1A C8A 116.1(7) . . ?
C8A N1A Cu1A 119.1(5) . . ?
C17A N2A Cu1A 117.8(5) . . ?
C18A N2A Cu1A 123.5(6) . . ?
C18A N2A C17A 118.6(7) . . ?
O1A C1A C2A 116.1(7) . . ?
O1A C1A C6A 125.9(7) . . ?
C6A C1A C2A 118.0(7) . . ?
O2A C2A C1A 119.7(7) . . ?
O2A C2A C3A 118.2(7) . . ?
C3A C2A C1A 122.1(8) . . ?
C2A C3A C4A 119.2(8) . . ?
C5A C4A C3A 121.8(8) . . ?
C4A C5A C6A 118.2(8) . . ?
C1A C6A C5A 120.8(7) . . ?
C1A C6A C7A 122.8(7) . . ?
C5A C6A C7A 116.4(8) . . ?
N1A C7A C6A 125.9(7) . . ?
N1A C8A C9A 111.1(6) . . ?
C10A C9A C8A 116.2(6) . . ?
C9A C10A Si2A 114.3(5) . . ?
C16A C15A Si1A 117.4(6) . . ?
C15A C16A C17A 115.7(7) . . ?
N2A C17A C16A 109.4(5) . . ?
N2A C18A C19A 125.5(9) . . ?
C18A C19A C20A 116.3(11) . . ?
C24A C19A C18A 124.5(10) . . ?
C24A C19A C20A 119.1(10) . . ?
C21A C20A C19A 119.8(13) . . ?
C20A C21A C22A 120.4(15) . . ?
C23A C22A C21A 120.4(14) . . ?
O5A C23A C22A 119.9(12) . . ?
O5A C23A C24A 119.9(12) . . ?
C22A C23A C24A 120.2(13) . . ?
O4A C24A C19A 124.4(9) . . ?
O4A C24A C23A 115.6(11) . . ?
C19A C24A C23A 120.0(10) . . ?
O1B Cu1B O4B 157.0(2) . . ?
O1B Cu1B N1B 93.0(2) . . ?
O1B Cu1B N2B 91.2(3) . . ?
O4B Cu1B N1B 93.3(2) . . ?
O4B Cu1B N2B 92.7(3) . . ?
N1B Cu1B N2B 154.0(2) . . ?
O3B Si1B C10B 107.2(3) . . ?
O3B Si1B C11B 110.0(4) . . ?
O3B Si1B C12B 108.5(3) . . ?
C11B Si1B C10B 108.7(4) . . ?
C12B Si1B C10B 113.3(4) . . ?
C12B Si1B C11B 109.1(3) . . ?
O3B Si2B C13B 107.3(4) . . ?
O3B Si2B C14B 110.8(3) . . ?
O3B Si2B C15B 108.1(4) . . ?
C13B Si2B C14B 111.6(4) . . ?
C13B Si2B C15B 111.5(3) . . ?
C14B Si2B C15B 107.6(4) . . ?
C1B O1B Cu1B 127.3(5) . . ?
C24B O4B Cu1B 127.5(5) . . ?
Si1B O3B Si2B 163.7(4) . . ?
C7B N1B Cu1B 122.3(5) . . ?
C7B N1B C8B 118.4(7) . . ?
C8B N1B Cu1B 119.2(5) . . ?
C17B N2B Cu1B 117.6(5) . . ?
C18B N2B Cu1B 123.9(6) . . ?
C18B N2B C17B 118.4(7) . . ?
O1B C1B C2B 117.1(8) . . ?
O1B C1B C6B 125.8(8) . . ?
C6B C1B C2B 117.1(8) . . ?
O2B C2B C1B 117.3(9) . . ?
C3B C2B O2B 120.7(9) . . ?
C3B C2B C1B 122.0(9) . . ?
C2B C3B C4B 120.5(10) . . ?
C5B C4B C3B 120.2(10) . . ?
C4B C5B C6B 121.1(10) . . ?
C1B C6B C5B 118.9(8) . . ?
C1B C6B C7B 121.1(9) . . ?
C7B C6B C5B 120.0(10) . . ?
N1B C7B C6B 129.2(8) . . ?
N1B C8B C9B 111.7(7) . . ?
C10B C9B C8B 114.8(7) . . ?
C9B C10B Si1B 114.0(6) . . ?
C16B C15B Si2B 116.5(6) . . ?
C15B C16B C17B 114.5(7) . . ?
N2B C17B C16B 111.4(5) . . ?
N2B C18B C19B 127.7(8) . . ?
C20B C19B C18B 116.4(9) . . ?
C24B C19B C18B 121.8(9) . . ?
C24B C19B C20B 121.7(8) . . ?
C21B C20B C19B 119.1(9) . . ?
C20B C21B C22B 120.7(10) . . ?
C21B C22B C23B 120.6(10) . . ?
O5B C23B C22B 118.6(9) . . ?
O5B C23B C24B 119.8(9) . . ?
C22B C23B C24B 121.6(9) . . ?
O4B C24B C19B 125.2(8) . . ?
O4B C24B C23B 118.5(8) . . ?
C19B C24B C23B 116.3(8) . . ?

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
O2A H2A O4B 0.87 2.03 2.765(7) 142.5 . yes
O5A H5A O2B 0.84 2.21 3.048(9) 176.2 . yes
O2B H2B O4A 0.82 2.18 2.957(7) 158.1 . yes
O5B H5B O2A 0.82 2.20 3.017(8) 174.9 . yes

_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 1.224
_oxdiff_exptl_absorpt_empirical_full_min 0.701
# start Validation Reply Form
_vrf_PLAT026_shi_4158_mada       
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PROBLEM: Ratio Observed/Unique Reflections (too) Low .. 33% Check 
RESPONSE: Crystal quality is quite low and therefore present low diffraction
capacity. The ratio between observed/unique reflections is quite low
;
_vrf_PLAT601_shi_4158_mada       
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PROBLEM: Structure Contains Solvent Accessible VOIDS of . 108 Ang**3
RESPONSE: This is a specific feature for the crystal structure
;
