# Electronic Supplementary Material (ESI) for Chemical Science.
# This journal is © The Royal Society of Chemistry 2024

####################################################################### 
# 
# 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_jnm116
_database_code_depnum_ccdc_archive 'CCDC 2237924'
loop_
_audit_author_name
_audit_author_address
'Jennifer Murphy'
;University of Guelph
Canada
;
_audit_update_record             
;
2023-01-25 deposited with the CCDC.	2024-04-11 downloaded from the CCDC.
;
_audit_creation_date             2021-03-03
_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         'C42 H42 Cl4 Cu N6 O4, 2(C H4 O)'
_chemical_formula_sum            'C44 H50 Cl4 Cu N6 O6'
_chemical_formula_weight         964.24
_chemical_melting_point          ?
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0181 0.0091 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Cl Cl 0.3639 0.7018 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Cu Cu -1.9646 0.5888 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0311 0.0180 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0492 0.0322 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_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                   8.1744(3)
_cell_length_b                   11.9929(5)
_cell_length_c                   13.8763(6)
_cell_angle_alpha                68.678(2)
_cell_angle_beta                 77.480(2)
_cell_angle_gamma                81.887(2)
_cell_volume                     1234.20(9)
_cell_formula_units_Z            1
_cell_measurement_reflns_used    9879
_cell_measurement_temperature    170.0
_cell_measurement_theta_max      77.3480
_cell_measurement_theta_min      3.9530
_shelx_estimated_absorpt_T_max   0.915
_shelx_estimated_absorpt_T_min   0.314
_exptl_absorpt_coefficient_mu    3.021
_exptl_absorpt_correction_T_max  0.7538
_exptl_absorpt_correction_T_min  0.5531
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
;
SADABS-2016/2 (Bruker,2016/2) was used for absorption correction.
wR2(int) was 0.1368 before and 0.0931 after correction.
The Ratio of minimum to maximum transmission is 0.7337.
The λ/2 correction factor is Not present.
;
_exptl_absorpt_special_details   ?
_exptl_crystal_colour            'clear violet'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_primary    violet
_exptl_crystal_density_diffrn    1.297
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       plate
_exptl_crystal_F_000             501
_exptl_crystal_size_max          0.5
_exptl_crystal_size_mid          0.2
_exptl_crystal_size_min          0.03
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0650
_diffrn_reflns_av_unetI/netI     0.0475
_diffrn_reflns_Laue_measured_fraction_full 0.995
_diffrn_reflns_Laue_measured_fraction_max 0.985
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            22244
_diffrn_reflns_point_group_measured_fraction_full 0.995
_diffrn_reflns_point_group_measured_fraction_max 0.985
_diffrn_reflns_theta_full        67.679
_diffrn_reflns_theta_max         74.781
_diffrn_reflns_theta_min         3.475
_diffrn_ambient_temperature      170.0
_diffrn_detector_area_resol_mean ?
_diffrn_measured_fraction_theta_full 0.995
_diffrn_measured_fraction_theta_max 0.985
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       'φ and ω scans'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54178
_diffrn_source                   ?
_diffrn_standards_number         0
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                4169
_reflns_number_total             4990
_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 Structure factors included contributions from the .fab file.
 
 _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       'SAINT V8.38A (?, 2016)'
_computing_data_collection       ?
_computing_data_reduction        'SAINT V8.38A (?, 2016)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'XL (Sheldrick, 2008)'
_computing_structure_solution    'XT (Sheldrick, 2015)'
_refine_diff_density_max         0.672
_refine_diff_density_min         -0.534
_refine_diff_density_rms         0.085
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.064
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     279
_refine_ls_number_reflns         4990
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0692
_refine_ls_R_factor_gt           0.0585
_refine_ls_restrained_S_all      1.064
_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)+(0.0744P)²+1.6402P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1520
_refine_ls_wR_factor_ref         0.1613
_refine_special_details          ?
_olex2_refinement_description    
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups, All N(H) groups
 At 1.5 times of:
  All C(H,H,H) groups, All O(H) groups
2.a Riding coordinates:
 N007(H007)
2.b Secondary CH2 refined with riding coordinates:
 C2(H2A,H2B), C18(H18A,H18B), C19(H19A,H19B), C20(H20A,H20B), C21(H21A,H21B)
2.c Aromatic/amide H refined with riding coordinates:
 C4(H4), C5(H5), C6(H6), C7(H7), C11(H11), C12(H12), C13(H13), C15(H15),
 C16(H16), C17(H17)
2.d Idealised Me refined as rotating group:
 C22(H22A,H22B,H22C)
2.e Idealised tetrahedral OH refined as rotating group:
 O3(H3)
;
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     dual
_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
Cu1 Cu 0.500000 0.500000 0.500000 0.02671(17) Uani 1 2 d S T P . .
Cl1 Cl 0.44567(11) 0.55643(8) 0.78342(8) 0.0536(3) Uani 1 1 d . . . . .
Cl2 Cl 0.29629(12) 1.03327(8) 0.68756(8) 0.0506(2) Uani 1 1 d . . . . .
O1 O 0.4320(2) 0.65878(18) 0.51457(17) 0.0327(5) Uani 1 1 d . . . . .
O2 O 0.3657(3) 0.6941(2) 0.35939(18) 0.0413(5) Uani 1 1 d . . . . .
N1 N 0.2707(3) 0.4512(2) 0.56433(19) 0.0296(5) Uani 1 1 d . . . . .
N2 N 0.0121(3) 0.4475(2) 0.65168(19) 0.0317(5) Uani 1 1 d . . . . .
N007 N 0.3381(3) 0.8011(2) 0.6461(2) 0.0343(6) Uani 1 1 d . . . . .
H007 H 0.388236 0.739892 0.628116 0.041 Uiso 1 1 d R . . . .
C1 C 0.3688(3) 0.7260(3) 0.4348(2) 0.0314(6) Uani 1 1 d . . . . .
C2 C 0.2904(4) 0.8482(3) 0.4372(3) 0.0366(7) Uani 1 1 d . . . . .
H2A H 0.377433 0.893689 0.443394 0.044 Uiso 1 1 calc R . . . .
H2B H 0.251446 0.893476 0.369921 0.044 Uiso 1 1 calc R . . . .
C3 C 0.1437(4) 0.8401(2) 0.5271(2) 0.0320(6) Uani 1 1 d . . . . .
C4 C -0.0199(4) 0.8559(3) 0.5092(3) 0.0395(7) Uani 1 1 d . . . . .
H4 H -0.038797 0.868027 0.440834 0.047 Uiso 1 1 calc R . . . .
C5 C -0.1563(4) 0.8545(3) 0.5886(3) 0.0442(8) Uani 1 1 d . . . . .
H5 H -0.267416 0.864504 0.574985 0.053 Uiso 1 1 calc R . . . .
C6 C -0.1297(4) 0.8385(3) 0.6873(3) 0.0414(8) Uani 1 1 d . . . . .
H6 H -0.222766 0.838809 0.741843 0.050 Uiso 1 1 calc R . . . .
C7 C 0.0328(4) 0.8219(3) 0.7079(3) 0.0371(7) Uani 1 1 d . . . . .
H7 H 0.050276 0.811323 0.776257 0.044 Uiso 1 1 calc R . . . .
C8 C 0.1700(3) 0.8209(3) 0.6286(2) 0.0307(6) Uani 1 1 d . . . . .
C9 C 0.3773(4) 0.7939(3) 0.7419(2) 0.0349(7) Uani 1 1 d . . . . .
C10 C 0.4371(4) 0.6876(3) 0.8114(3) 0.0396(7) Uani 1 1 d . . . . .
C11 C 0.4875(5) 0.6822(4) 0.9023(3) 0.0515(9) Uani 1 1 d . . . . .
H11 H 0.532487 0.608649 0.946620 0.062 Uiso 1 1 calc R . . . .
C12 C 0.4719(6) 0.7834(4) 0.9274(3) 0.0619(11) Uani 1 1 d . . . . .
H12 H 0.502797 0.779570 0.990778 0.074 Uiso 1 1 calc R . . . .
C13 C 0.4120(5) 0.8908(4) 0.8622(3) 0.0542(9) Uani 1 1 d . . . . .
H13 H 0.402124 0.961093 0.880016 0.065 Uiso 1 1 calc R . . . .
C14 C 0.3660(4) 0.8959(3) 0.7704(3) 0.0407(7) Uani 1 1 d . . . . .
C15 C 0.1989(4) 0.3551(3) 0.5633(3) 0.0349(7) Uani 1 1 d . . . . .
H15 H 0.252688 0.299534 0.530059 0.042 Uiso 1 1 calc R . . . .
C16 C 0.0400(4) 0.3520(3) 0.6168(3) 0.0382(7) Uani 1 1 d . . . . .
H16 H -0.037790 0.294658 0.628143 0.046 Uiso 1 1 calc R . . . .
C17 C 0.1533(4) 0.5051(3) 0.6182(2) 0.0328(6) Uani 1 1 d . . . . .
H17 H 0.167807 0.575209 0.631315 0.039 Uiso 1 1 calc R . . . .
C18 C -0.1448(4) 0.4764(3) 0.7160(2) 0.0378(7) Uani 1 1 d . . . . .
H18A H -0.238937 0.442748 0.703548 0.045 Uiso 1 1 calc R . . . .
H18B H -0.166896 0.564585 0.693480 0.045 Uiso 1 1 calc R . . . .
C19 C -0.1388(4) 0.4271(3) 0.8332(3) 0.0434(8) Uani 1 1 d . . . . .
H19A H -0.255109 0.423356 0.873333 0.052 Uiso 1 1 calc R . . . .
H19B H -0.086066 0.344311 0.851457 0.052 Uiso 1 1 calc R . . . .
C20 C -0.0417(4) 0.5023(3) 0.8663(3) 0.0425(8) Uani 1 1 d . . . . .
H20A H 0.076574 0.501105 0.829815 0.051 Uiso 1 1 calc R . . . .
H20B H -0.089178 0.586463 0.842914 0.051 Uiso 1 1 calc R . . . .
C21 C -0.0446(5) 0.4605(4) 0.9834(3) 0.0469(8) Uani 1 1 d . . . . .
H21A H 0.008590 0.377912 1.006149 0.056 Uiso 1 1 calc R . . . .
H21B H -0.162965 0.457514 1.020155 0.056 Uiso 1 1 calc R . . . .
O3 O 0.4794(7) 0.1959(5) 0.8435(3) 0.1112(15) Uani 1 1 d . . . . .
H3 H 0.534943 0.233822 0.784792 0.167 Uiso 1 1 calc GR . . . .
C22 C 0.3065(7) 0.2389(5) 0.8478(4) 0.0792(14) Uani 1 1 d . . . . .
H22A H 0.238957 0.186070 0.911060 0.119 Uiso 1 1 calc GR . . . .
H22B H 0.268434 0.239616 0.785327 0.119 Uiso 1 1 calc GR . . . .
H22C H 0.293778 0.320430 0.850102 0.119 Uiso 1 1 calc GR . . . .


_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
Cu1 O1 1.9770(19) 2_666 ?
Cu1 O1 1.9771(19) . ?
Cu1 N1 1.963(2) . ?
Cu1 N1 1.964(2) 2_666 ?
Cl1 C10 1.741(4) . ?
Cl2 C14 1.733(4) . ?
O1 C1 1.273(4) . ?
O2 C1 1.244(4) . ?
N1 C15 1.372(4) . ?
N1 C17 1.328(4) . ?
N2 C16 1.371(4) . ?
N2 C17 1.336(4) . ?
N2 C18 1.471(4) . ?
N007 C8 1.419(4) . ?
N007 C9 1.404(4) . ?
C1 C2 1.524(4) . ?
C2 C3 1.517(4) . ?
C3 C4 1.387(4) . ?
C3 C8 1.401(4) . ?
C4 C5 1.385(5) . ?
C5 C6 1.373(5) . ?
C6 C7 1.391(4) . ?
C7 C8 1.393(4) . ?
C9 C10 1.389(5) . ?
C9 C14 1.401(5) . ?
C10 C11 1.387(5) . ?
C11 C12 1.362(6) . ?
C12 C13 1.373(6) . ?
C13 C14 1.383(5) . ?
C15 C16 1.348(4) . ?
C18 C19 1.525(5) . ?
C19 C20 1.522(5) . ?
C20 C21 1.512(5) . ?
C21 C21 1.517(7) 2_567 ?
O3 C22 1.431(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
O1 Cu1 O1 180.0 2_666 . ?
N1 Cu1 O1 89.46(9) . . ?
N1 Cu1 O1 89.46(9) 2_666 2_666 ?
N1 Cu1 O1 90.54(9) . 2_666 ?
N1 Cu1 O1 90.54(9) 2_666 . ?
N1 Cu1 N1 180.0 . 2_666 ?
C1 O1 Cu1 108.52(18) . . ?
C15 N1 Cu1 127.4(2) . . ?
C17 N1 Cu1 126.7(2) . . ?
C17 N1 C15 105.9(2) . . ?
C16 N2 C18 125.0(3) . . ?
C17 N2 C16 107.2(2) . . ?
C17 N2 C18 127.8(3) . . ?
C9 N007 C8 121.7(3) . . ?
O1 C1 C2 116.5(3) . . ?
O2 C1 O1 122.8(3) . . ?
O2 C1 C2 120.6(3) . . ?
C3 C2 C1 113.2(3) . . ?
C4 C3 C2 120.2(3) . . ?
C4 C3 C8 118.7(3) . . ?
C8 C3 C2 121.0(3) . . ?
C5 C4 C3 121.6(3) . . ?
C6 C5 C4 119.5(3) . . ?
C5 C6 C7 120.3(3) . . ?
C6 C7 C8 120.3(3) . . ?
C3 C8 N007 117.9(3) . . ?
C7 C8 N007 122.5(3) . . ?
C7 C8 C3 119.6(3) . . ?
C10 C9 N007 122.4(3) . . ?
C10 C9 C14 116.1(3) . . ?
C14 C9 N007 121.4(3) . . ?
C9 C10 Cl1 118.3(3) . . ?
C11 C10 Cl1 119.2(3) . . ?
C11 C10 C9 122.4(3) . . ?
C12 C11 C10 119.3(4) . . ?
C11 C12 C13 120.7(3) . . ?
C12 C13 C14 119.5(4) . . ?
C9 C14 Cl2 119.4(2) . . ?
C13 C14 Cl2 118.7(3) . . ?
C13 C14 C9 121.9(3) . . ?
C16 C15 N1 109.2(3) . . ?
C15 C16 N2 106.8(3) . . ?
N1 C17 N2 110.9(3) . . ?
N2 C18 C19 112.7(3) . . ?
C20 C19 C18 113.2(3) . . ?
C21 C20 C19 114.2(3) . . ?
C20 C21 C21 114.0(4) . 2_567 ?

_smtbx_masks_special_details     ?
loop_
_smtbx_masks_void_nr
_smtbx_masks_void_average_x
_smtbx_masks_void_average_y
_smtbx_masks_void_average_z
_smtbx_masks_void_volume
_smtbx_masks_void_count_electrons
_smtbx_masks_void_content
1 0.269 0.000 0.000 177.9 39.8 ?


# end Validation Reply Form
_olex2_submission_special_instructions 'No special instructions were received'
# start Validation Reply Form
_vrf_PLAT906_jnm116              
;
PROBLEM: Large K Value in the Analysis of Variance ......      2.006 Check 
RESPONSE: The last round of least squares gave a K value of 2.480
for the Fc/Fc(max) groups between 0.000 and 0.009. These K values likely
result from contributions of essentially unobserved reflections. For all other
Fc/Fc(max) groups, K ranged from 0.965 to 1.266.
;
_vrf_PLAT911_jnm116              
;
PROBLEM: Missing FCF Refl Between Thmin & STh/L=    0.600         22 Report
RESPONSE: This represents only a very small number of reflections compared 
with the total number that were collected, and may result from weak diffraction,
or partial obstruction by the beamstop.
;
_vrf_PLAT976_jnm116              
;
PROBLEM: Check Calcd Resid. Dens.  0.70A   From O3             -0.53 eA-3  
RESPONSE: This Q peak is near MeOH in the lattice. The H atoms of this MeOH
were introduced in calculated positions. I believe the Q peaks surrounding
the MeOH are due to disorder. However, the MeOH could not be modelled in a 
way to incorporate the surrounding Q peaks because they are too far apart
to be an additional or split MeOH molecule. A solvent mask was used to 
remove residual electron density from un-refinable MeOH. These crystals
lose MeOH very quickly once out of solvent and this structure and the 
refinement statistics associated with it are the absolute best I could do.
;
####################################################################### 
# 
# 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_cu_jnm108
_database_code_depnum_ccdc_archive 'CCDC 2237927'
loop_
_audit_author_name
_audit_author_address
'Jennifer Murphy'
;University of Guelph
Canada
;
_audit_update_record             
;
2023-01-25 deposited with the CCDC.	2024-04-11 downloaded from the CCDC.
;
_audit_creation_date             2021-02-17
_audit_creation_method           
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_shelx_SHELXL_version_number     2017/1
_chemical_name_common            ?
_chemical_name_systematic        ?
_chemical_formula_moiety         'C44 H50 Cl4 Mn N6 O6'
_chemical_formula_sum            'C44 H50 Cl4 Mn N6 O6'
_chemical_formula_weight         955.64
_chemical_melting_point          ?
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0181 0.0091 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Cl Cl 0.3639 0.7018 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Mn Mn -0.5299 2.8052 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0311 0.0180 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0492 0.0322 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_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/n 1'
_space_group_name_Hall           '-P 2yn'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x+1/2, y+1/2, -z+1/2'
'-x, -y, -z'
'x-1/2, -y-1/2, z-1/2'

_cell_length_a                   8.5583(9)
_cell_length_b                   21.737(3)
_cell_length_c                   12.8769(19)
_cell_angle_alpha                90
_cell_angle_beta                 108.475(14)
_cell_angle_gamma                90
_cell_volume                     2272.1(5)
_cell_formula_units_Z            2
_cell_measurement_reflns_used    2045
_cell_measurement_temperature    170
_cell_measurement_theta_max      55.3160
_cell_measurement_theta_min      4.0540
_shelx_estimated_absorpt_T_max   0.789
_shelx_estimated_absorpt_T_min   0.437
_exptl_absorpt_coefficient_mu    4.965
_exptl_absorpt_correction_T_max  ?
_exptl_absorpt_correction_T_min  ?
_exptl_absorpt_correction_type   none
_exptl_absorpt_process_details   ?
_exptl_absorpt_special_details   ?
_exptl_crystal_colour            'clear colourless'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.397
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       irregular
_exptl_crystal_F_000             994
_exptl_crystal_size_max          0.2
_exptl_crystal_size_mid          0.05
_exptl_crystal_size_min          0.05
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.1870
_diffrn_reflns_av_unetI/netI     0.1128
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_k_max       25
_diffrn_reflns_limit_k_min       -25
_diffrn_reflns_limit_l_max       14
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_number            24612
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_theta_full        66.588
_diffrn_reflns_theta_max         66.588
_diffrn_reflns_theta_min         4.067
_diffrn_ambient_temperature      170
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean ?
_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    182.13 278.13   1.00   60.00    --  -99.06 -59.25 140.08   96
  2  ω    182.13 278.13   1.00   60.00    --  -99.06 -59.25 -19.92   96
  3  ω   -130.71 -19.71   1.00   60.00    --  -99.06  83.74  90.05  111
  4  ω   -130.71 -19.71   1.00   60.00    --  -99.06  83.74-109.95  111
  5  ω      3.93  99.93   1.00   60.00    --   20.69  59.25 -20.08   96
  6  ω    197.13 293.13   1.00   60.00    --  -84.06 -59.25-159.92   96
  7  ω    197.13 293.13   1.00   60.00    --  -84.06 -59.25 -69.92   96
  8  ω      3.93  99.93   1.00   60.00    --   20.69  59.25  69.92   96
  9  ω   -130.71 -19.71   1.00   60.00    --  -99.06  83.74  50.05  111
 10  ω    -26.23  72.77   1.00   60.00    --   50.69 -83.74 -75.05   99
 11  ω   -130.71 -19.71   1.00   60.00    --  -99.06  83.74 -29.95  111
 12  ω    197.13 293.13   1.00   60.00    --  -84.06 -59.25  20.08   96
 13  ω   -130.71 -19.71   1.00   60.00    --  -99.06  83.74 170.05  111
;
_diffrn_measurement_device       'abstract diffractometer'
_diffrn_measurement_device_type  
'Saxi-CrysAlisPro-abstract goniometer imported SAXI images'
_diffrn_measurement_method       'ω scans'
_diffrn_orient_matrix_type       
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      -0.0116964000
_diffrn_orient_matrix_UB_12      -0.0700556000
_diffrn_orient_matrix_UB_13      -0.0191136000
_diffrn_orient_matrix_UB_21      -0.0864465000
_diffrn_orient_matrix_UB_22      0.0107767000
_diffrn_orient_matrix_UB_23      -0.1231060000
_diffrn_orient_matrix_UB_31      0.1685802000
_diffrn_orient_matrix_UB_32      0.0006449000
_diffrn_orient_matrix_UB_33      -0.0194845000
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_source                   'fine-focus sealed X-ray tube'
_diffrn_source_type              'Enhance (Cu) X-ray Source'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                2185
_reflns_number_total             4000
_reflns_odcompleteness_completeness 96.54
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     76.12
_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
;
_reflns_threshold_expression     'I > 2σ(I)'
_computing_cell_refinement       'CrysAlisPro 1.171.40.53 (Rigaku OD, 2019)'
_computing_data_collection       'CrysAlisPro 1.171.40.53 (Rigaku OD, 2019)'
_computing_data_reduction        'CrysAlisPro 1.171.40.53 (Rigaku OD, 2019)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_computing_structure_solution    'XT (Sheldrick, 2015)'
_refine_diff_density_max         0.813
_refine_diff_density_min         -0.695
_refine_diff_density_rms         0.089
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.967
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     285
_refine_ls_number_reflns         4000
_refine_ls_number_restraints     3
_refine_ls_R_factor_all          0.1362
_refine_ls_R_factor_gt           0.0754
_refine_ls_restrained_S_all      0.968
_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)+(0.1129P)²] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1829
_refine_ls_wR_factor_ref         0.2346
_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, All O(H) groups
2. Restrained distances
 O3-H3
 0.85 with sigma of 0.01
 C21-H3
 1.910527 with sigma of 0.02
 Mn1-H3
 2.81661 with sigma of 0.02
3.a Secondary CH2 refined with riding coordinates:
 C2(H2A,H2B), C18(H18A,H18B), C19(H19A,H19B), C20(H20A,H20B), C21(H21A,H21B)
3.b Aromatic/amide H refined with riding coordinates:
 C5(H5), C6(H6), C7(H7), C8(H8), C11(H11), C12(H12), C13(H13), C15(H15),
 C16(H16), C17(H17)
3.c Idealised Me refined as rotating group:
 C22(H22A,H22B,H22C)
;
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     dual
_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
Mn1 Mn 0.500000 0.500000 0.500000 0.0437(4) Uani 1 2 d DS T P . .
Cl1 Cl 0.5664(2) 0.35258(9) 1.16347(14) 0.0694(5) Uani 1 1 d . . . . .
Cl2 Cl 0.69214(19) 0.26670(8) 0.80271(14) 0.0650(5) Uani 1 1 d . . . . .
O1 O 0.4234(5) 0.49261(18) 0.6440(3) 0.0512(10) Uani 1 1 d . . . . .
O2 O 0.5872(5) 0.41750(19) 0.7369(3) 0.0578(11) Uani 1 1 d . . . . .
O3 O 0.3747(5) 0.58922(19) 0.4577(3) 0.0545(11) Uani 1 1 d D . . . .
H3 H 0.391(5) 0.6149(16) 0.412(4) 0.082 Uiso 1 1 d DR . . . .
N1 N 0.2734(5) 0.4499(2) 0.3987(4) 0.0492(12) Uani 1 1 d . . . . .
N2 N 0.1089(6) 0.4020(2) 0.2552(4) 0.0484(12) Uani 1 1 d . . . . .
N3 N 0.5559(6) 0.3581(2) 0.9279(4) 0.0477(12) Uani 1 1 d . . . . .
C1 C 0.4826(7) 0.4595(3) 0.7272(5) 0.0440(14) Uani 1 1 d . . . . .
C2 C 0.4213(7) 0.4710(3) 0.8248(5) 0.0490(14) Uani 1 1 d . . . . .
H2A H 0.517343 0.475655 0.891724 0.059 Uiso 1 1 calc R . . . .
H2B H 0.358402 0.509969 0.813025 0.059 Uiso 1 1 calc R . . . .
C3 C 0.3141(7) 0.4200(3) 0.8418(4) 0.0441(13) Uani 1 1 d . . . . .
C4 C 0.3829(7) 0.3655(3) 0.8972(4) 0.0433(14) Uani 1 1 d . . . . .
C5 C 0.2804(7) 0.3217(3) 0.9209(5) 0.0487(15) Uani 1 1 d . . . . .
H5 H 0.326671 0.286513 0.963217 0.058 Uiso 1 1 calc R . . . .
C6 C 0.1100(7) 0.3294(3) 0.8826(5) 0.0556(16) Uani 1 1 d . . . . .
H6 H 0.040721 0.299046 0.898213 0.067 Uiso 1 1 calc R . . . .
C7 C 0.0422(7) 0.3799(3) 0.8232(5) 0.0565(16) Uani 1 1 d . . . . .
H7 H -0.074215 0.383869 0.795125 0.068 Uiso 1 1 calc R . . . .
C8 C 0.1431(7) 0.4261(3) 0.8030(5) 0.0496(15) Uani 1 1 d . . . . .
H8 H 0.094828 0.461719 0.762766 0.060 Uiso 1 1 calc R . . . .
C9 C 0.6322(7) 0.3060(3) 0.9867(5) 0.0508(15) Uani 1 1 d . . . . .
C10 C 0.6465(7) 0.2981(3) 1.0971(5) 0.0562(16) Uani 1 1 d . . . . .
C11 C 0.7272(8) 0.2470(3) 1.1560(6) 0.0651(19) Uani 1 1 d . . . . .
H11 H 0.731551 0.241713 1.230139 0.078 Uiso 1 1 calc R . . . .
C12 C 0.7998(8) 0.2046(3) 1.1079(7) 0.073(2) Uani 1 1 d . . . . .
H12 H 0.856231 0.170483 1.149135 0.087 Uiso 1 1 calc R . . . .
C13 C 0.7916(8) 0.2111(3) 0.9991(6) 0.0664(19) Uani 1 1 d . . . . .
H13 H 0.843013 0.181863 0.965731 0.080 Uiso 1 1 calc R . . . .
C14 C 0.7075(7) 0.2607(3) 0.9398(5) 0.0519(16) Uani 1 1 d . . . . .
C15 C 0.1233(7) 0.4390(3) 0.4145(5) 0.0501(15) Uani 1 1 d . . . . .
H15 H 0.096094 0.450217 0.477986 0.060 Uiso 1 1 calc R . . . .
C16 C 0.0217(7) 0.4103(3) 0.3263(5) 0.0526(15) Uani 1 1 d . . . . .
H16 H -0.088917 0.398192 0.315667 0.063 Uiso 1 1 calc R . . . .
C17 C 0.2583(7) 0.4271(3) 0.3014(5) 0.0490(15) Uani 1 1 d . . . . .
H17 H 0.342488 0.428237 0.267933 0.059 Uiso 1 1 calc R . . . .
C18 C 0.0458(7) 0.3764(3) 0.1434(5) 0.0524(15) Uani 1 1 d . . . . .
H18A H -0.025509 0.340573 0.143445 0.063 Uiso 1 1 calc R . . . .
H18B H 0.139618 0.361879 0.120495 0.063 Uiso 1 1 calc R . . . .
C19 C -0.0521(7) 0.4239(3) 0.0614(5) 0.0507(15) Uani 1 1 d . . . . .
H19A H -0.104999 0.403063 -0.009450 0.061 Uiso 1 1 calc R . . . .
H19B H -0.140792 0.440221 0.087647 0.061 Uiso 1 1 calc R . . . .
C20 C 0.0491(7) 0.4774(3) 0.0423(5) 0.0491(15) Uani 1 1 d . . . . .
H20A H 0.098473 0.499369 0.112400 0.059 Uiso 1 1 calc R . . . .
H20B H 0.140336 0.461120 0.018504 0.059 Uiso 1 1 calc R . . . .
C21 C 0.2174(7) 0.6022(3) 0.4710(5) 0.0618(18) Uani 1 1 d D . . . .
H21A H 0.211251 0.581619 0.538215 0.074 Uiso 1 1 calc R . . . .
H21B H 0.129336 0.584839 0.408066 0.074 Uiso 1 1 calc R . . . .
C22 C 0.1889(10) 0.6676(3) 0.4786(7) 0.089(3) Uani 1 1 d . . . . .
H22A H 0.179242 0.687262 0.408349 0.133 Uiso 1 1 calc GR . . . .
H22B H 0.281287 0.685748 0.536147 0.133 Uiso 1 1 calc GR . . . .
H22C H 0.086748 0.673817 0.496249 0.133 Uiso 1 1 calc GR . . . .
H3A H 0.587(7) 0.362(3) 0.862(5) 0.054(18) Uiso 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
Mn1 O1 2.160(4) . ?
Mn1 O1 2.160(4) 3_666 ?
Mn1 O3 2.199(4) . ?
Mn1 O3 2.199(4) 3_666 ?
Mn1 N1 2.247(5) . ?
Mn1 N1 2.247(5) 3_666 ?
Cl1 C10 1.724(7) . ?
Cl2 C14 1.733(7) . ?
O1 C1 1.257(7) . ?
O2 C1 1.256(7) . ?
O3 H3 0.855(9) . ?
O3 C21 1.437(7) . ?
N1 C15 1.383(7) . ?
N1 C17 1.315(7) . ?
N2 C16 1.364(7) . ?
N2 C17 1.343(7) . ?
N2 C18 1.477(7) . ?
N3 C4 1.415(7) . ?
N3 C9 1.403(7) . ?
N3 H3A 0.97(6) . ?
C1 C2 1.528(8) . ?
C2 H2A 0.9900 . ?
C2 H2B 0.9900 . ?
C2 C3 1.498(8) . ?
C3 C4 1.413(8) . ?
C3 C8 1.395(8) . ?
C4 C5 1.392(7) . ?
C5 H5 0.9500 . ?
C5 C6 1.393(8) . ?
C6 H6 0.9500 . ?
C6 C7 1.359(8) . ?
C7 H7 0.9500 . ?
C7 C8 1.402(8) . ?
C8 H8 0.9500 . ?
C9 C10 1.399(9) . ?
C9 C14 1.412(8) . ?
C10 C11 1.398(9) . ?
C11 H11 0.9500 . ?
C11 C12 1.365(10) . ?
C12 H12 0.9500 . ?
C12 C13 1.388(10) . ?
C13 H13 0.9500 . ?
C13 C14 1.384(8) . ?
C15 H15 0.9500 . ?
C15 C16 1.346(8) . ?
C16 H16 0.9500 . ?
C17 H17 0.9500 . ?
C18 H18A 0.9900 . ?
C18 H18B 0.9900 . ?
C18 C19 1.523(8) . ?
C19 H19A 0.9900 . ?
C19 H19B 0.9900 . ?
C19 C20 1.516(8) . ?
C20 C20 1.509(11) 3_565 ?
C20 H20A 0.9900 . ?
C20 H20B 0.9900 . ?
C21 H21A 0.9900 . ?
C21 H21B 0.9900 . ?
C21 C22 1.450(9) . ?
C22 H22A 0.9800 . ?
C22 H22B 0.9800 . ?
C22 H22C 0.9800 . ?

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
O1 Mn1 O1 180.0 . 3_666 ?
O1 Mn1 O3 88.78(15) 3_666 . ?
O1 Mn1 O3 91.22(15) . . ?
O1 Mn1 O3 91.22(15) 3_666 3_666 ?
O1 Mn1 O3 88.78(15) . 3_666 ?
O1 Mn1 N1 88.77(16) 3_666 . ?
O1 Mn1 N1 91.23(16) . . ?
O1 Mn1 N1 88.77(16) . 3_666 ?
O1 Mn1 N1 91.23(16) 3_666 3_666 ?
O3 Mn1 O3 180.0 3_666 . ?
O3 Mn1 N1 88.81(16) 3_666 . ?
O3 Mn1 N1 88.81(16) . 3_666 ?
O3 Mn1 N1 91.19(16) . . ?
O3 Mn1 N1 91.19(16) 3_666 3_666 ?
N1 Mn1 N1 180.0 . 3_666 ?
C1 O1 Mn1 128.7(4) . . ?
Mn1 O3 H3 125.1(17) . . ?
C21 O3 Mn1 123.0(4) . . ?
C21 O3 H3 108.3(16) . . ?
C15 N1 Mn1 131.9(4) . . ?
C17 N1 Mn1 122.8(4) . . ?
C17 N1 C15 105.1(5) . . ?
C16 N2 C18 126.6(5) . . ?
C17 N2 C16 107.1(5) . . ?
C17 N2 C18 126.0(5) . . ?
C4 N3 H3A 107(3) . . ?
C9 N3 C4 120.6(5) . . ?
C9 N3 H3A 110(3) . . ?
O1 C1 C2 117.2(5) . . ?
O2 C1 O1 125.6(5) . . ?
O2 C1 C2 117.2(5) . . ?
C1 C2 H2A 109.1 . . ?
C1 C2 H2B 109.1 . . ?
H2A C2 H2B 107.8 . . ?
C3 C2 C1 112.7(5) . . ?
C3 C2 H2A 109.1 . . ?
C3 C2 H2B 109.1 . . ?
C4 C3 C2 121.2(5) . . ?
C8 C3 C2 120.0(5) . . ?
C8 C3 C4 118.9(5) . . ?
C3 C4 N3 117.9(5) . . ?
C5 C4 N3 122.5(5) . . ?
C5 C4 C3 119.5(5) . . ?
C4 C5 H5 119.9 . . ?
C4 C5 C6 120.2(6) . . ?
C6 C5 H5 119.9 . . ?
C5 C6 H6 119.7 . . ?
C7 C6 C5 120.6(6) . . ?
C7 C6 H6 119.7 . . ?
C6 C7 H7 119.8 . . ?
C6 C7 C8 120.3(6) . . ?
C8 C7 H7 119.8 . . ?
C3 C8 C7 120.2(5) . . ?
C3 C8 H8 119.9 . . ?
C7 C8 H8 119.9 . . ?
N3 C9 C14 121.9(6) . . ?
C10 C9 N3 121.6(6) . . ?
C10 C9 C14 116.4(5) . . ?
C9 C10 Cl1 119.9(5) . . ?
C11 C10 Cl1 118.8(6) . . ?
C11 C10 C9 121.2(6) . . ?
C10 C11 H11 119.7 . . ?
C12 C11 C10 120.5(7) . . ?
C12 C11 H11 119.7 . . ?
C11 C12 H12 119.8 . . ?
C11 C12 C13 120.3(6) . . ?
C13 C12 H12 119.8 . . ?
C12 C13 H13 120.4 . . ?
C14 C13 C12 119.2(7) . . ?
C14 C13 H13 120.4 . . ?
C9 C14 Cl2 119.1(4) . . ?
C13 C14 Cl2 118.6(5) . . ?
C13 C14 C9 122.3(6) . . ?
N1 C15 H15 125.2 . . ?
C16 C15 N1 109.7(5) . . ?
C16 C15 H15 125.2 . . ?
N2 C16 H16 126.8 . . ?
C15 C16 N2 106.5(5) . . ?
C15 C16 H16 126.8 . . ?
N1 C17 N2 111.6(5) . . ?
N1 C17 H17 124.2 . . ?
N2 C17 H17 124.2 . . ?
N2 C18 H18A 109.3 . . ?
N2 C18 H18B 109.3 . . ?
N2 C18 C19 111.8(5) . . ?
H18A C18 H18B 107.9 . . ?
C19 C18 H18A 109.3 . . ?
C19 C18 H18B 109.3 . . ?
C18 C19 H19A 108.6 . . ?
C18 C19 H19B 108.6 . . ?
H19A C19 H19B 107.6 . . ?
C20 C19 C18 114.5(5) . . ?
C20 C19 H19A 108.6 . . ?
C20 C19 H19B 108.6 . . ?
C19 C20 H20A 108.8 . . ?
C19 C20 H20B 108.8 . . ?
C20 C20 C19 113.6(6) 3_565 . ?
C20 C20 H20A 108.8 3_565 . ?
C20 C20 H20B 108.8 3_565 . ?
H20A C20 H20B 107.7 . . ?
O3 C21 H21A 109.1 . . ?
O3 C21 H21B 109.1 . . ?
O3 C21 C22 112.6(6) . . ?
H21A C21 H21B 107.8 . . ?
C22 C21 H21A 109.1 . . ?
C22 C21 H21B 109.1 . . ?
C21 C22 H22A 109.5 . . ?
C21 C22 H22B 109.5 . . ?
C21 C22 H22C 109.5 . . ?
H22A C22 H22B 109.5 . . ?
H22A C22 H22C 109.5 . . ?
H22B C22 H22C 109.5 . . ?

# end Validation Reply Form
_olex2_submission_special_instructions 'No special instructions were received'
_vrf_PLAT020_cu_jnm108           
;
PROBLEM: The Value of Rint is Greater Than 0.12 .........      0.187 Report
RESPONSE: These were low quality crystals that did not result in
super satisfactory results despite many attempts to grow better crystals.
;
_vrf_PLAT341_cu_jnm108           
;
PROBLEM: Low Bond Precision on  C-C Bonds ...............    0.00916 Ang.  
RESPONSE: Crystals were small and thin, and they diffracted weakly.
Several attempts to grow more suitable crystals, resulted in this dataset,
with the best refinement statistics. All metrics are reported with their
associated standard uncertainties.
;
_vrf_PLAT911_cu_jnm108           
;
PROBLEM: Missing FCF Refl Between Thmin & STh/L=    0.595          6 Report
RESPONSE: This represents only a very small number of reflections compared 
with the total number that were collected, and may result from weak diffraction,
or partial obstruction by the beamstop.
;
_vrf_PLAT973_cu_jnm108           
;
PROBLEM: Check Calcd Positive Resid. Density on       Mn1       1.23 eA-3  
RESPONSE: According to the last round of least squares:
Electron density synthesis with coefficients Fo-Fc
Highest peak    0.81  at  0.0000  0.0000  1.0000  [  0.00 A from MN1 ]
Deepest hole   -0.70  at  0.1070  0.0001  0.9910  [  0.96 A from MN1 ]
These coordinates put the highest residual peak nearest the heaviest atom, 
which is sensible, it does not correspond to an incorrectly assigned atom.
;
# start Validation Reply Form
_vrf_RINTA01_cu_jnm108           
;
PROBLEM: The value of Rint is greater than 0.18
RESPONSE: These were low quality crystals that did not result in
super satisfactory results despite many attempts to grow better crystals.
;
####################################################################### 
# 
# 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_cu_jnm056
_database_code_depnum_ccdc_archive 'CCDC 2237925'
loop_
_audit_author_name
_audit_author_address
'Jennifer Murphy'
;University of Guelph
Canada
;
_audit_update_record             
;
2023-01-25 deposited with the CCDC.	2024-04-11 downloaded from the CCDC.
;
_audit_creation_date             2020-09-11
_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         'C42 H46 Cl4 Mg N6 O6'
_chemical_formula_sum            'C42 H46 Cl4 Mg N6 O6'
_chemical_formula_weight         896.96
_chemical_melting_point          ?
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0181 0.0091 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Cl Cl 0.3639 0.7018 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Mg Mg 0.1719 0.1771 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0311 0.0180 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0492 0.0322 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_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/n 1'
_space_group_name_Hall           '-P 2yn'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x+1/2, y+1/2, -z+1/2'
'-x, -y, -z'
'x-1/2, -y-1/2, z-1/2'

_cell_length_a                   8.48440(10)
_cell_length_b                   20.9466(2)
_cell_length_c                   12.84190(10)
_cell_angle_alpha                90
_cell_angle_beta                 107.4270(10)
_cell_angle_gamma                90
_cell_volume                     2177.50(4)
_cell_formula_units_Z            2
_cell_measurement_reflns_used    18603
_cell_measurement_temperature    170
_cell_measurement_theta_max      78.6040
_cell_measurement_theta_min      4.1740
_shelx_estimated_absorpt_T_max   0.580
_shelx_estimated_absorpt_T_min   0.375
_exptl_absorpt_coefficient_mu    3.053
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.70072
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
;
CrysAlisPro 1.171.40.53 (Rigaku Oxford Diffraction, 2019)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_absorpt_special_details   ?
_exptl_crystal_colour            'clear colourless'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.368
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       prism
_exptl_crystal_F_000             936
_exptl_crystal_size_max          0.4
_exptl_crystal_size_mid          0.3
_exptl_crystal_size_min          0.2
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0473
_diffrn_reflns_av_unetI/netI     0.0241
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.995
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       26
_diffrn_reflns_limit_k_min       -26
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_number            40598
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.995
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         79.260
_diffrn_reflns_theta_min         4.180
_diffrn_ambient_temperature      170
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean ?
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.995
_diffrn_measurement_details      
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  tₑₓₚ   ω     θ     κ     φ   Frames
#--------------------------------------------------------------------------
  1  ω   -136.76 -25.76   1.00   15.00    -- -105.12  83.74 -29.95  111
  2  ω    176.08 271.08   1.00   15.00    -- -105.12 -59.25 -99.92   95
  3  ω    176.08 271.08   1.00   15.00    -- -105.12 -59.25  20.08   95
  4  ω   -136.76 -25.76   1.00   15.00    -- -105.12  83.74-149.95  111
  5  ω      3.93  99.93   1.00   15.00    --   20.69  59.25  69.92   96
  6  ω    176.08 271.08   1.00   15.00    -- -105.12 -59.25-139.92   95
  7  ω   -136.76 -25.76   1.00   15.00    -- -105.12  83.74  90.05  111
  8  ω      3.93  99.93   1.00   15.00    --   20.69  59.25 159.92   96
  9  ω    176.08 271.08   1.00   15.00    -- -105.12 -59.25 -19.92   95
 10  ω    176.08 271.08   1.00   15.00    -- -105.12 -59.25  60.08   95
 11  ω    176.08 271.08   1.00   15.00    -- -105.12 -59.25-179.92   95
 12  ω    -26.23  72.77   1.00   15.00    --   50.69 -83.74 131.95   99
 13  ω   -136.76 -25.76   1.00   15.00    -- -105.12  83.74  10.05  111
 14  ω   -136.76 -25.76   1.00   15.00    -- -105.12  83.74 170.05  111
 15  ω   -136.76 -25.76   1.00   15.00    -- -105.12  83.74 130.05  111
 16  ω    191.08 286.08   1.00   15.00    --  -90.12 -59.25 110.08   95
 17  ω   -136.76 -25.76   1.00   15.00    -- -105.12  83.74-109.95  111
 18  ω   -136.76 -25.76   1.00   15.00    -- -105.12  83.74  50.05  111
 19  ω    176.08 271.08   1.00   15.00    -- -105.12 -59.25 -59.92   95
 20  ω   -136.76 -25.76   1.00   15.00    -- -105.12  83.74 -69.95  111
 21  ω    176.08 271.08   1.00   15.00    -- -105.12 -59.25 140.08   95
;
_diffrn_measurement_device       'abstract diffractometer'
_diffrn_measurement_device_type  
'Saxi-CrysAlisPro-abstract goniometer imported SAXI images'
_diffrn_measurement_method       'ω scans'
_diffrn_orient_matrix_type       
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      0.0844795000
_diffrn_orient_matrix_UB_12      -0.0631585000
_diffrn_orient_matrix_UB_13      0.0473560000
_diffrn_orient_matrix_UB_21      0.0963709000
_diffrn_orient_matrix_UB_22      0.0349907000
_diffrn_orient_matrix_UB_23      0.1053506000
_diffrn_orient_matrix_UB_31      -0.1406391000
_diffrn_orient_matrix_UB_32      -0.0139726000
_diffrn_orient_matrix_UB_33      0.0497304000
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_source                   'fine-focus sealed X-ray tube'
_diffrn_source_type              'Enhance (Cu) X-ray Source'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                4314
_reflns_number_total             4696
_reflns_odcompleteness_completeness 99.40
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     79.01
_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
;
_reflns_threshold_expression     'I > 2σ(I)'
_computing_cell_refinement       'CrysAlisPro 1.171.40.53 (Rigaku OD, 2019)'
_computing_data_collection       'CrysAlisPro 1.171.40.53 (Rigaku OD, 2019)'
_computing_data_reduction        'CrysAlisPro 1.171.40.53 (Rigaku OD, 2019)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'XL (Sheldrick, 2008)'
_computing_structure_solution    'XT (Sheldrick, 2015)'
_refine_diff_density_max         0.349
_refine_diff_density_min         -0.586
_refine_diff_density_rms         0.127
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.072
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     272
_refine_ls_number_reflns         4696
_refine_ls_number_restraints     3
_refine_ls_R_factor_all          0.0463
_refine_ls_R_factor_gt           0.0431
_refine_ls_restrained_S_all      1.075
_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)+(0.0738P)²+0.7125P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1135
_refine_ls_wR_factor_ref         0.1169
_refine_special_details          ?
_olex2_refinement_description    
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups, All N(H) groups
 At 1.5 times of:
  All C(H,H,H) groups, All O(H) groups
2. Restrained distances
 O3-H3
 0.87 with sigma of 0.01
 C20-H3
 1.889432 with sigma of 0.02
 Mg1-H3
 2.613869 with sigma of 0.02
3.a Riding coordinates:
 N3(H3A)
3.b Secondary CH2 refined with riding coordinates:
 C2(H2A,H2B), C17(H17A,H17B), C18(H18A,H18B), C19(H19A,H19B)
3.c Aromatic/amide H refined with riding coordinates:
 C00K(H00K), C5(H5), C6(H6), C7(H7), C8(H8), C11(H11), C12(H12), C13(H13),
 C15(H15), C16(H16)
3.d Idealised Me refined as rotating group:
 C20(H20A,H20B,H20C)
;
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     dual
_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
Cl1 Cl 0.45264(6) 0.64699(2) 0.33837(3) 0.03965(14) Uani 1 1 d . . . . .
Cl2 Cl 0.32534(5) 0.73464(2) 0.70165(3) 0.03090(12) Uani 1 1 d . . . . .
Mg1 Mg 0.500000 0.500000 1.000000 0.01905(16) Uani 1 2 d DS T P . .
O1 O 0.58169(13) 0.50557(5) 0.86471(8) 0.0227(2) Uani 1 1 d . . . . .
O2 O 0.42561(14) 0.58251(5) 0.76489(9) 0.0282(3) Uani 1 1 d . . . . .
O3 O 0.60834(15) 0.40973(5) 1.04023(9) 0.0274(2) Uani 1 1 d D . . . .
H3 H 0.619(2) 0.4025(9) 1.1097(9) 0.041 Uiso 1 1 d DR . . . .
N1 N 0.27325(15) 0.45377(6) 0.90007(10) 0.0229(3) Uani 1 1 d . . . . .
N2 N 0.10220(16) 0.40344(6) 0.75999(10) 0.0225(3) Uani 1 1 d . . . . .
N3 N 0.46460(15) 0.64116(6) 0.57473(10) 0.0207(3) Uani 1 1 d . . . . .
H3A H 0.426902 0.633222 0.630222 0.025 Uiso 1 1 d R . . . .
C00K C 0.01846(19) 0.41281(8) 0.83506(13) 0.0272(3) Uani 1 1 d . . . . .
H00K H -0.091717 0.400308 0.828524 0.033 Uiso 1 1 calc R . . . .
C1 C 0.53340(17) 0.53945(6) 0.78017(11) 0.0190(3) Uani 1 1 d . . . . .
C2 C 0.61078(19) 0.52737(7) 0.68893(12) 0.0220(3) Uani 1 1 d . . . . .
H2A H 0.682336 0.489139 0.707609 0.026 Uiso 1 1 calc R . . . .
H2B H 0.521684 0.517933 0.620778 0.026 Uiso 1 1 calc R . . . .
C3 C 0.71235(18) 0.58269(7) 0.66824(11) 0.0189(3) Uani 1 1 d . . . . .
C4 C 0.63796(17) 0.63634(7) 0.60695(11) 0.0184(3) Uani 1 1 d . . . . .
C5 C 0.73710(18) 0.68301(7) 0.58026(12) 0.0225(3) Uani 1 1 d . . . . .
H5 H 0.687129 0.718223 0.536000 0.027 Uiso 1 1 calc R . . . .
C6 C 0.90815(19) 0.67829(8) 0.61796(13) 0.0264(3) Uani 1 1 d . . . . .
H6 H 0.974380 0.710073 0.598776 0.032 Uiso 1 1 calc R . . . .
C7 C 0.98278(19) 0.62745(8) 0.68344(13) 0.0283(3) Uani 1 1 d . . . . .
H7 H 1.099698 0.625008 0.711549 0.034 Uiso 1 1 calc R . . . .
C8 C 0.8842(2) 0.58017(8) 0.70736(12) 0.0253(3) Uani 1 1 d . . . . .
H8 H 0.935338 0.545126 0.751620 0.030 Uiso 1 1 calc R . . . .
C9 C 0.38350(17) 0.69446(7) 0.51611(12) 0.0212(3) Uani 1 1 d . . . . .
C10 C 0.30759(18) 0.74064(7) 0.56382(13) 0.0239(3) Uani 1 1 d . . . . .
C11 C 0.2202(2) 0.79193(8) 0.50557(16) 0.0330(4) Uani 1 1 d . . . . .
H11 H 0.167133 0.821632 0.539868 0.040 Uiso 1 1 calc R . . . .
C12 C 0.2116(2) 0.79909(8) 0.39716(17) 0.0390(4) Uani 1 1 d . . . . .
H12 H 0.153530 0.834296 0.356775 0.047 Uiso 1 1 calc R . . . .
C13 C 0.2870(2) 0.75537(9) 0.34702(15) 0.0361(4) Uani 1 1 d . . . . .
H13 H 0.282512 0.760745 0.272726 0.043 Uiso 1 1 calc R . . . .
C14 C 0.3692(2) 0.70360(8) 0.40605(13) 0.0270(3) Uani 1 1 d . . . . .
C15 C 0.25332(18) 0.42876(7) 0.80241(12) 0.0234(3) Uani 1 1 d . . . . .
H15 H 0.336233 0.428701 0.766463 0.028 Uiso 1 1 calc R . . . .
C16 C 0.1252(2) 0.44365(8) 0.92079(13) 0.0266(3) Uani 1 1 d . . . . .
H16 H 0.101125 0.456317 0.985406 0.032 Uiso 1 1 calc R . . . .
C17 C 0.0364(2) 0.37559(7) 0.65051(12) 0.0261(3) Uani 1 1 d . . . . .
H17A H -0.037389 0.339505 0.653709 0.031 Uiso 1 1 calc R . . . .
H17B H 0.129023 0.358499 0.626930 0.031 Uiso 1 1 calc R . . . .
C18 C -0.05911(19) 0.42386(8) 0.56671(12) 0.0246(3) Uani 1 1 d . . . . .
H18A H -0.146161 0.443315 0.593364 0.030 Uiso 1 1 calc R . . . .
H18B H -0.114328 0.401219 0.497753 0.030 Uiso 1 1 calc R . . . .
C19 C 0.04881(18) 0.47676(7) 0.54333(12) 0.0230(3) Uani 1 1 d . . . . .
H19A H 0.101162 0.500500 0.611605 0.028 Uiso 1 1 calc R . . . .
H19B H 0.137906 0.457424 0.518592 0.028 Uiso 1 1 calc R . . . .
C20 C 0.7343(3) 0.37699(12) 1.01349(18) 0.0518(6) Uani 1 1 d D . . . .
H20A H 0.712373 0.377112 0.934097 0.078 Uiso 1 1 calc GR . . . .
H20B H 0.738783 0.332854 1.039528 0.078 Uiso 1 1 calc GR . . . .
H20C H 0.840288 0.398033 1.048085 0.078 Uiso 1 1 calc GR . . . .


_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
Cl1 C14 1.7408(18) . ?
Cl2 C10 1.7354(17) . ?
Mg1 O1 2.0576(10) . ?
Mg1 O1 2.0576(10) 3_667 ?
Mg1 O3 2.0982(11) . ?
Mg1 O3 2.0982(11) 3_667 ?
Mg1 N1 2.1924(13) 3_667 ?
Mg1 N1 2.1924(13) . ?
O1 C1 1.2584(17) . ?
O2 C1 1.2574(18) . ?
O3 C20 1.397(2) . ?
N1 C15 1.322(2) . ?
N1 C16 1.376(2) . ?
N2 C00K 1.372(2) . ?
N2 C15 1.3430(19) . ?
N2 C17 1.4692(19) . ?
N3 C4 1.4072(18) . ?
N3 C9 1.4058(18) . ?
C00K C16 1.361(2) . ?
C1 C2 1.5261(19) . ?
C2 C3 1.5144(19) . ?
C3 C4 1.4081(19) . ?
C3 C8 1.394(2) . ?
C4 C5 1.398(2) . ?
C5 C6 1.389(2) . ?
C6 C7 1.387(2) . ?
C7 C8 1.389(2) . ?
C9 C10 1.401(2) . ?
C9 C14 1.395(2) . ?
C10 C11 1.390(2) . ?
C11 C12 1.380(3) . ?
C12 C13 1.382(3) . ?
C13 C14 1.386(2) . ?
C17 C18 1.521(2) . ?
C18 C19 1.524(2) . ?
C19 C19 1.523(3) 3_566 ?

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
O1 Mg1 O1 180.0 . 3_667 ?
O1 Mg1 O3 91.46(4) 3_667 3_667 ?
O1 Mg1 O3 88.54(4) . 3_667 ?
O1 Mg1 O3 88.54(4) 3_667 . ?
O1 Mg1 O3 91.46(4) . . ?
O1 Mg1 N1 89.38(4) 3_667 3_667 ?
O1 Mg1 N1 90.62(4) . 3_667 ?
O1 Mg1 N1 89.38(4) . . ?
O1 Mg1 N1 90.62(5) 3_667 . ?
O3 Mg1 O3 180.0 . 3_667 ?
O3 Mg1 N1 90.63(5) . 3_667 ?
O3 Mg1 N1 90.63(5) 3_667 . ?
O3 Mg1 N1 89.37(5) 3_667 3_667 ?
O3 Mg1 N1 89.37(5) . . ?
N1 Mg1 N1 180.0 3_667 . ?
C1 O1 Mg1 130.95(10) . . ?
C20 O3 Mg1 133.87(12) . . ?
C15 N1 Mg1 124.79(10) . . ?
C15 N1 C16 104.92(13) . . ?
C16 N1 Mg1 130.29(10) . . ?
C00K N2 C17 126.92(13) . . ?
C15 N2 C00K 106.91(13) . . ?
C15 N2 C17 126.02(13) . . ?
C9 N3 C4 121.02(11) . . ?
C16 C00K N2 106.07(14) . . ?
O1 C1 C2 117.72(13) . . ?
O2 C1 O1 124.95(13) . . ?
O2 C1 C2 117.33(12) . . ?
C3 C2 C1 113.96(11) . . ?
C4 C3 C2 121.69(13) . . ?
C8 C3 C2 119.78(13) . . ?
C8 C3 C4 118.50(13) . . ?
N3 C4 C3 118.41(12) . . ?
C5 C4 N3 122.04(13) . . ?
C5 C4 C3 119.56(13) . . ?
C6 C5 C4 120.50(14) . . ?
C7 C6 C5 120.37(14) . . ?
C6 C7 C8 119.07(14) . . ?
C7 C8 C3 121.84(14) . . ?
C10 C9 N3 121.98(13) . . ?
C14 C9 N3 122.11(14) . . ?
C14 C9 C10 115.89(14) . . ?
C9 C10 Cl2 119.03(11) . . ?
C11 C10 Cl2 118.32(13) . . ?
C11 C10 C9 122.65(15) . . ?
C12 C11 C10 119.04(17) . . ?
C11 C12 C13 120.40(15) . . ?
C12 C13 C14 119.42(17) . . ?
C9 C14 Cl1 119.17(12) . . ?
C13 C14 Cl1 118.24(14) . . ?
C13 C14 C9 122.57(16) . . ?
N1 C15 N2 112.12(13) . . ?
C00K C16 N1 109.98(14) . . ?
N2 C17 C18 112.47(13) . . ?
C17 C18 C19 113.49(12) . . ?
C19 C19 C18 112.42(15) 3_566 . ?

_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
- Detector area scaling
;
_oxdiff_exptl_absorpt_empirical_full_max 1.296
_oxdiff_exptl_absorpt_empirical_full_min 0.758
# start Validation Reply Form
_vrf_PLAT977_cu_jnm056           
;
PROBLEM: Check Negative Difference Density on H17B             -0.33 eA-3  
RESPONSE: This H atom was introduced in a calculated position, it is not the
result of an incorrect AFIX.
;
# end Validation Reply Form
####################################################################### 
# 
# 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_jnm122
_database_code_depnum_ccdc_archive 'CCDC 2237926'
loop_
_audit_author_name
_audit_author_address
'Jennifer Murphy'
;University of Guelph
Canada
;
_audit_update_record             
;
2023-01-25 deposited with the CCDC.	2024-04-11 downloaded from the CCDC.
;
_audit_creation_date             2021-04-14
_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         'C42 H42 Cl4 N6 O4 Zn'
_chemical_formula_sum            'C42 H42 Cl4 N6 O4 Zn'
_chemical_formula_weight         901.98
_chemical_melting_point          ?
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0181 0.0091 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Cl Cl 0.3639 0.7018 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0311 0.0180 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0492 0.0322 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Zn Zn -1.5491 0.6778 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

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

_cell_length_a                   11.3205(4)
_cell_length_b                   13.1000(5)
_cell_length_c                   15.6723(6)
_cell_angle_alpha                113.7270(10)
_cell_angle_beta                 98.6240(10)
_cell_angle_gamma                97.2980(10)
_cell_volume                     2058.10(13)
_cell_formula_units_Z            2
_cell_measurement_reflns_used    9846
_cell_measurement_temperature    170(2)
_cell_measurement_theta_max      72.10
_cell_measurement_theta_min      3.16
_shelx_estimated_absorpt_T_max   0.713
_shelx_estimated_absorpt_T_min   0.531
_exptl_absorpt_coefficient_mu    3.625
_exptl_absorpt_correction_T_max  0.7536
_exptl_absorpt_correction_T_min  0.5788
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
'SADABS-2016/2 (Bruker,2016/2) was used for absorption correction. wR2(int) was 0.0820 before and 0.0577 after correction. The Ratio of minimum to maximum transmission is 0.7680. The λ/2 correction factor is Not present.'
_exptl_absorpt_special_details   ?
_exptl_crystal_colour            'clear colourless'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.455
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       prism
_exptl_crystal_F_000             932
_exptl_crystal_size_max          0.2
_exptl_crystal_size_mid          0.2
_exptl_crystal_size_min          0.1
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0361
_diffrn_reflns_av_unetI/netI     0.0222
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.996
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            46068
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.996
_diffrn_reflns_theta_full        67.679
_diffrn_reflns_theta_max         72.097
_diffrn_reflns_theta_min         3.158
_diffrn_ambient_temperature      170.0
_diffrn_detector_area_resol_mean ?
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.996
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       'φ and ω scans'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54178
_diffrn_source                   ?
_diffrn_standards_number         0
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                7455
_reflns_number_total             8063
_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       'SAINT V8.38A (?, 2016)'
_computing_data_collection       ?
_computing_data_reduction        'SAINT V8.38A (?, 2016)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'XL (Sheldrick, 2008)'
_computing_structure_solution    'XT (Sheldrick, 2015)'
_refine_diff_density_max         0.752
_refine_diff_density_min         -0.743
_refine_diff_density_rms         0.078
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.051
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     522
_refine_ls_number_reflns         8063
_refine_ls_number_restraints     48
_refine_ls_R_factor_all          0.0391
_refine_ls_R_factor_gt           0.0361
_refine_ls_restrained_S_all      1.049
_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)+(0.0492P)²+1.5498P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0943
_refine_ls_wR_factor_ref         0.0968
_refine_special_details          ?
_olex2_refinement_description    
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
2. Uiso/Uaniso restraints and constraints
Uanis(C41) \\sim Ueq, Uanis(C40) \\sim Ueq, Uanis(C39) \\sim Ueq, Uanis(C38)
\\sim Ueq, Uanis(C42) \\sim Ueq: with sigma of 0.1 and sigma for terminal atoms
of 0.2
3. Rigid body (RIGU) restrains
 C37, C42
 with sigma for 1-2 distances of 0.002 and sigma for 1-3 distances of 0.002
 C42, C41
 with sigma for 1-2 distances of 0.002 and sigma for 1-3 distances of 0.002
 C41, C40
 with sigma for 1-2 distances of 0.002 and sigma for 1-3 distances of 0.002
 C40, C39
 with sigma for 1-2 distances of 0.002 and sigma for 1-3 distances of 0.002
 C39, C38
 with sigma for 1-2 distances of 0.002 and sigma for 1-3 distances of 0.002
 C38, C37
 with sigma for 1-2 distances of 0.002 and sigma for 1-3 distances of 0.002
4.a Secondary CH2 refined with riding coordinates:
 C4(H4A,H4B), C5(H5A,H5B), C6(H6A,H6B), C7(H7A,H7B), C11(H11A,H11B), C12(H12A,
 H12B), C13(H13A,H13B), C14(H14A,H14B), C16(H16A,H16B), C30(H30A,H30B)
4.b Aromatic/amide H refined with riding coordinates:
 C1(H1), C2(H2), C3(H3), C8(H8), C9(H9), C10(H10), C18(H18), C19(H19),
 C20(H20), C21(H21), C25(H25), C26(H26), C27(H27), C33(H33), C34(H34), C35(H35),
  C36(H36), C39(H39), C40(H40), C41(H41)
;
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     dual
_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
Zn01 Zn 0.14288(2) 0.55794(2) 0.27632(2) 0.02387(8) Uani 1 1 d . . . . .
Cl1 Cl 0.64315(6) 0.26162(5) 0.06492(5) 0.05324(17) Uani 1 1 d . . . . .
Cl2 Cl 0.27156(5) 0.22008(5) 0.23613(5) 0.04813(15) Uani 1 1 d . . . . .
Cl3 Cl 0.42941(5) 0.73133(4) 0.45185(4) 0.03817(13) Uani 1 1 d . . . . .
Cl4 Cl 0.34129(7) 1.14759(5) 0.65410(4) 0.05517(18) Uani 1 1 d . . . . .
O1 O 0.30112(12) 0.51736(12) 0.24170(9) 0.0281(3) Uani 1 1 d . . . . .
O2 O 0.26759(13) 0.64539(12) 0.18722(10) 0.0325(3) Uani 1 1 d . . . . .
O3 O 0.12972(12) 0.71633(11) 0.34664(10) 0.0295(3) Uani 1 1 d . . . . .
O4 O -0.07112(14) 0.65878(14) 0.32164(13) 0.0447(4) Uani 1 1 d . . . . .
N1 N 0.03114(14) 0.45529(13) 0.14997(12) 0.0280(3) Uani 1 1 d . . . . .
N2 N -0.02515(15) 0.33287(14) -0.00133(12) 0.0277(3) Uani 1 1 d . . . . .
N3 N 0.12908(15) 0.50542(14) 0.38124(12) 0.0279(3) Uani 1 1 d . . . . .
N4 N 0.16235(14) 0.51273(14) 0.52569(12) 0.0279(3) Uani 1 1 d . . . . .
N5 N 0.26871(15) 0.89764(14) 0.52063(12) 0.0267(3) Uani 1 1 d . . . . .
N6 N 0.42531(16) 0.32957(14) 0.14330(12) 0.0282(3) Uani 1 1 d . . . . .
C1 C -0.07631(18) 0.47350(17) 0.11035(15) 0.0310(4) Uani 1 1 d . . . . .
H1 H -0.118940 0.529887 0.143185 0.037 Uiso 1 1 calc R . . . .
C2 C -0.11182(19) 0.39820(18) 0.01692(15) 0.0320(4) Uani 1 1 d . . . . .
H2 H -0.182835 0.391964 -0.027217 0.038 Uiso 1 1 calc R . . . .
C3 C 0.05892(18) 0.36999(17) 0.08029(14) 0.0301(4) Uani 1 1 d . . . . .
H3 H 0.129316 0.339065 0.087229 0.036 Uiso 1 1 calc R . . . .
C4 C -0.0310(2) 0.23480(19) -0.09179(15) 0.0349(5) Uani 1 1 d . . . . .
H4A H 0.049055 0.212002 -0.091085 0.042 Uiso 1 1 calc R . . . .
H4B H -0.048509 0.256755 -0.145170 0.042 Uiso 1 1 calc R . . . .
C5 C -0.1297(2) 0.13410(18) -0.10804(15) 0.0345(5) Uani 1 1 d . . . . .
H5A H -0.133797 0.071872 -0.171504 0.041 Uiso 1 1 calc R . . . .
H5B H -0.209380 0.157700 -0.109813 0.041 Uiso 1 1 calc R . . . .
C6 C -0.11183(19) 0.08704(18) -0.03342(15) 0.0324(4) Uani 1 1 d . . . . .
H6A H -0.099600 0.150701 0.030754 0.039 Uiso 1 1 calc R . . . .
H6B H -0.187515 0.032617 -0.043599 0.039 Uiso 1 1 calc R . . . .
C7 C -0.00469(19) 0.02703(19) -0.03484(15) 0.0332(4) Uani 1 1 d . . . . .
H7A H -0.013229 -0.032894 -0.100267 0.040 Uiso 1 1 calc R . . . .
H7B H 0.072024 0.082912 -0.019160 0.040 Uiso 1 1 calc R . . . .
C8 C 0.09141(18) 0.39813(17) 0.37492(16) 0.0320(4) Uani 1 1 d . . . . .
H8 H 0.056363 0.331752 0.317272 0.038 Uiso 1 1 calc R . . . .
C9 C 0.11197(19) 0.40164(18) 0.46357(17) 0.0349(5) Uani 1 1 d . . . . .
H9 H 0.094829 0.339378 0.479458 0.042 Uiso 1 1 calc R . . . .
C10 C 0.17041(17) 0.57200(17) 0.47354(14) 0.0268(4) Uani 1 1 d . . . . .
H10 H 0.201817 0.651703 0.499528 0.032 Uiso 1 1 calc R . . . .
C11 C 0.2123(2) 0.5549(2) 0.62862(15) 0.0356(5) Uani 1 1 d . . . . .
H11A H 0.149173 0.531195 0.658188 0.043 Uiso 1 1 calc R . . . .
H11B H 0.232883 0.639232 0.658127 0.043 Uiso 1 1 calc R . . . .
C12 C 0.3256(2) 0.5104(2) 0.64927(17) 0.0404(5) Uani 1 1 d . . . . .
H12A H 0.303734 0.426100 0.618766 0.049 Uiso 1 1 calc R . . . .
H12B H 0.349414 0.535232 0.719140 0.049 Uiso 1 1 calc R . . . .
C13 C 0.43725(19) 0.5474(2) 0.61598(15) 0.0370(5) Uani 1 1 d . . . . .
H13A H 0.445892 0.629694 0.632386 0.044 Uiso 1 1 calc R . . . .
H13B H 0.510506 0.538401 0.653389 0.044 Uiso 1 1 calc R . . . .
C14 C 0.43787(17) 0.48536(18) 0.51024(14) 0.0297(4) Uani 1 1 d . . . . .
H14A H 0.415774 0.402115 0.489827 0.036 Uiso 1 1 calc R . . . .
H14B H 0.375380 0.506152 0.472364 0.036 Uiso 1 1 calc R . . . .
C15 C 0.32570(17) 0.57444(15) 0.19415(13) 0.0248(4) Uani 1 1 d . . . . .
C16 C 0.42764(18) 0.54639(16) 0.14052(14) 0.0280(4) Uani 1 1 d . . . . .
H16A H 0.455652 0.608798 0.123253 0.034 Uiso 1 1 calc R . . . .
H16B H 0.497848 0.538707 0.181872 0.034 Uiso 1 1 calc R . . . .
C17 C 0.38087(17) 0.43616(16) 0.05106(13) 0.0244(4) Uani 1 1 d . . . . .
C18 C 0.33509(18) 0.43634(17) -0.03650(14) 0.0288(4) Uani 1 1 d . . . . .
H18 H 0.334663 0.507201 -0.039666 0.035 Uiso 1 1 calc R . . . .
C19 C 0.29035(19) 0.33669(19) -0.11875(14) 0.0322(4) Uani 1 1 d . . . . .
H19 H 0.259537 0.339084 -0.177587 0.039 Uiso 1 1 calc R . . . .
C20 C 0.2909(2) 0.23301(18) -0.11454(14) 0.0325(4) Uani 1 1 d . . . . .
H20 H 0.260754 0.163876 -0.170786 0.039 Uiso 1 1 calc R . . . .
C21 C 0.33537(19) 0.23014(17) -0.02830(14) 0.0299(4) Uani 1 1 d . . . . .
H21 H 0.335152 0.158849 -0.025807 0.036 Uiso 1 1 calc R . . . .
C22 C 0.38031(17) 0.33062(16) 0.05457(13) 0.0246(4) Uani 1 1 d . . . . .
C23 C 0.45536(18) 0.23119(16) 0.14688(13) 0.0267(4) Uani 1 1 d . . . . .
C24 C 0.5536(2) 0.18809(18) 0.11068(16) 0.0333(4) Uani 1 1 d . . . . .
C25 C 0.5836(2) 0.0890(2) 0.11096(17) 0.0403(5) Uani 1 1 d . . . . .
H25 H 0.649377 0.061205 0.084102 0.048 Uiso 1 1 calc R . . . .
C26 C 0.5171(2) 0.03066(19) 0.15071(16) 0.0399(5) Uani 1 1 d . . . . .
H26 H 0.536436 -0.037779 0.150767 0.048 Uiso 1 1 calc R . . . .
C27 C 0.4226(2) 0.07222(19) 0.19016(15) 0.0376(5) Uani 1 1 d . . . . .
H27 H 0.378330 0.033714 0.219222 0.045 Uiso 1 1 calc R . . . .
C28 C 0.39226(18) 0.17031(18) 0.18744(14) 0.0300(4) Uani 1 1 d . . . . .
C29 C 0.02223(17) 0.73305(16) 0.35668(14) 0.0271(4) Uani 1 1 d . . . . .
C30 C 0.01905(19) 0.85525(17) 0.42219(16) 0.0334(4) Uani 1 1 d . . . . .
H30A H 0.075984 0.908625 0.409478 0.040 Uiso 1 1 calc R . . . .
H30B H -0.064224 0.868985 0.408631 0.040 Uiso 1 1 calc R . . . .
C31 C 0.05460(19) 0.87734(15) 0.52544(15) 0.0309(4) Uani 1 1 d . . . . .
C32 C 0.17721(19) 0.89714(15) 0.57196(14) 0.0285(4) Uani 1 1 d . . . . .
C33 C 0.2065(2) 0.91537(19) 0.66750(16) 0.0425(6) Uani 1 1 d . . . . .
H33 H 0.289272 0.926986 0.698221 0.051 Uiso 1 1 calc R . . . .
C34 C 0.1151(3) 0.9166(2) 0.71775(19) 0.0555(8) Uani 1 1 d . . . . .
H34 H 0.135626 0.929583 0.782841 0.067 Uiso 1 1 calc R . . . .
C35 C -0.0050(3) 0.8990(2) 0.6737(2) 0.0558(8) Uani 1 1 d . . . . .
H35 H -0.067298 0.900598 0.708345 0.067 Uiso 1 1 calc R . . . .
C36 C -0.0347(2) 0.87886(18) 0.5784(2) 0.0456(6) Uani 1 1 d . . . . .
H36 H -0.118025 0.865749 0.548274 0.055 Uiso 1 1 calc R . . . .
C37 C 0.39287(18) 0.93940(17) 0.56330(13) 0.0280(4) Uani 1 1 d . U . . .
C38 C 0.47925(19) 0.87130(18) 0.53804(15) 0.0311(4) Uani 1 1 d . U . . .
C39 C 0.6037(2) 0.9118(2) 0.57568(17) 0.0433(5) Uani 1 1 d . U . . .
H39 H 0.659445 0.863027 0.556404 0.052 Uiso 1 1 calc R . . . .
C40 C 0.6453(2) 1.0236(3) 0.64128(18) 0.0517(6) Uani 1 1 d . U . . .
H40 H 0.730318 1.051875 0.668028 0.062 Uiso 1 1 calc R . . . .
C41 C 0.5653(3) 1.0946(2) 0.66840(15) 0.0509(6) Uani 1 1 d . U . . .
H41 H 0.594820 1.171483 0.714185 0.061 Uiso 1 1 calc R . . . .
C42 C 0.4394(2) 1.05363(19) 0.62851(14) 0.0386(5) Uani 1 1 d . U . . .
H6 H 0.396(2) 0.365(2) 0.1849(19) 0.036(7) Uiso 1 1 d . . . . .
H5 H 0.251(2) 0.846(2) 0.4654(19) 0.034(6) Uiso 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
Zn01 O1 2.0218(13) . ?
Zn01 O3 1.9569(13) . ?
Zn01 N1 2.0008(16) . ?
Zn01 N3 2.0402(17) . ?
Cl1 C24 1.731(2) . ?
Cl2 C28 1.736(2) . ?
Cl3 C38 1.738(2) . ?
Cl4 C42 1.730(3) . ?
O1 C15 1.284(2) . ?
O2 C15 1.234(2) . ?
O3 C29 1.285(2) . ?
O4 C29 1.225(2) . ?
N1 C1 1.374(3) . ?
N1 C3 1.323(3) . ?
N2 C2 1.370(3) . ?
N2 C3 1.340(3) . ?
N2 C4 1.466(3) . ?
N3 C8 1.375(3) . ?
N3 C10 1.323(3) . ?
N4 C9 1.369(3) . ?
N4 C10 1.340(3) . ?
N4 C11 1.469(3) . ?
N5 C32 1.405(2) . ?
N5 C37 1.397(3) . ?
N6 C22 1.414(3) . ?
N6 C23 1.394(3) . ?
C1 C2 1.356(3) . ?
C4 C5 1.524(3) . ?
C5 C6 1.526(3) . ?
C6 C7 1.525(3) . ?
C7 C7 1.521(4) 2 ?
C8 C9 1.355(3) . ?
C11 C12 1.519(3) . ?
C12 C13 1.533(3) . ?
C13 C14 1.526(3) . ?
C14 C14 1.525(4) 2_666 ?
C15 C16 1.524(3) . ?
C16 C17 1.512(3) . ?
C17 C18 1.393(3) . ?
C17 C22 1.405(3) . ?
C18 C19 1.380(3) . ?
C19 C20 1.387(3) . ?
C20 C21 1.387(3) . ?
C21 C22 1.391(3) . ?
C23 C24 1.403(3) . ?
C23 C28 1.396(3) . ?
C24 C25 1.385(3) . ?
C25 C26 1.385(3) . ?
C26 C27 1.377(4) . ?
C27 C28 1.387(3) . ?
C29 C30 1.524(3) . ?
C30 C31 1.504(3) . ?
C31 C32 1.406(3) . ?
C31 C36 1.398(3) . ?
C32 C33 1.397(3) . ?
C33 C34 1.390(3) . ?
C34 C35 1.374(5) . ?
C35 C36 1.387(4) . ?
C37 C38 1.401(3) . ?
C37 C42 1.403(3) . ?
C38 C39 1.387(3) . ?
C39 C40 1.375(4) . ?
C40 C41 1.370(4) . ?
C41 C42 1.406(4) . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
O1 Zn01 N3 102.79(6) . . ?
O3 Zn01 O1 121.54(6) . . ?
O3 Zn01 N1 121.78(6) . . ?
O3 Zn01 N3 98.20(6) . . ?
N1 Zn01 O1 97.74(6) . . ?
N1 Zn01 N3 114.05(7) . . ?
C15 O1 Zn01 102.92(11) . . ?
C29 O3 Zn01 116.20(12) . . ?
C1 N1 Zn01 126.96(13) . . ?
C3 N1 Zn01 125.74(13) . . ?
C3 N1 C1 105.88(16) . . ?
C2 N2 C4 125.34(17) . . ?
C3 N2 C2 107.23(16) . . ?
C3 N2 C4 127.24(17) . . ?
C8 N3 Zn01 130.22(14) . . ?
C10 N3 Zn01 123.90(14) . . ?
C10 N3 C8 105.49(17) . . ?
C9 N4 C11 125.62(18) . . ?
C10 N4 C9 107.27(17) . . ?
C10 N4 C11 126.69(18) . . ?
C37 N5 C32 123.74(17) . . ?
C23 N6 C22 120.47(16) . . ?
C2 C1 N1 109.18(18) . . ?
C1 C2 N2 106.51(17) . . ?
N1 C3 N2 111.19(17) . . ?
N2 C4 C5 111.33(17) . . ?
C4 C5 C6 115.38(17) . . ?
C7 C6 C5 114.67(18) . . ?
C7 C7 C6 113.4(2) 2 . ?
C9 C8 N3 109.52(18) . . ?
C8 C9 N4 106.33(18) . . ?
N3 C10 N4 111.38(18) . . ?
N4 C11 C12 112.28(18) . . ?
C11 C12 C13 116.49(19) . . ?
C14 C13 C12 117.41(18) . . ?
C14 C14 C13 112.1(2) 2_666 . ?
O1 C15 C16 116.80(17) . . ?
O2 C15 O1 123.07(18) . . ?
O2 C15 C16 120.05(18) . . ?
C17 C16 C15 109.40(15) . . ?
C18 C17 C16 121.04(17) . . ?
C18 C17 C22 118.26(17) . . ?
C22 C17 C16 120.68(17) . . ?
C19 C18 C17 121.99(19) . . ?
C18 C19 C20 119.24(19) . . ?
C19 C20 C21 120.07(19) . . ?
C20 C21 C22 120.64(19) . . ?
C17 C22 N6 118.67(17) . . ?
C21 C22 N6 121.53(17) . . ?
C21 C22 C17 119.80(18) . . ?
N6 C23 C24 121.38(18) . . ?
N6 C23 C28 122.97(18) . . ?
C28 C23 C24 115.64(18) . . ?
C23 C24 Cl1 119.34(15) . . ?
C25 C24 Cl1 117.97(17) . . ?
C25 C24 C23 122.7(2) . . ?
C26 C25 C24 119.4(2) . . ?
C27 C26 C25 119.8(2) . . ?
C26 C27 C28 120.0(2) . . ?
C23 C28 Cl2 118.38(16) . . ?
C27 C28 Cl2 119.18(16) . . ?
C27 C28 C23 122.4(2) . . ?
O3 C29 C30 114.15(17) . . ?
O4 C29 O3 124.90(18) . . ?
O4 C29 C30 120.87(18) . . ?
C31 C30 C29 110.82(16) . . ?
C32 C31 C30 121.79(17) . . ?
C36 C31 C30 120.4(2) . . ?
C36 C31 C32 117.8(2) . . ?
N5 C32 C31 118.87(18) . . ?
C33 C32 N5 121.0(2) . . ?
C33 C32 C31 120.14(19) . . ?
C34 C33 C32 120.3(3) . . ?
C35 C34 C33 120.3(3) . . ?
C34 C35 C36 119.7(2) . . ?
C35 C36 C31 121.8(3) . . ?
N5 C37 C38 121.62(18) . . ?
N5 C37 C42 122.1(2) . . ?
C38 C37 C42 116.09(19) . . ?
C37 C38 Cl3 118.73(15) . . ?
C39 C38 Cl3 118.23(19) . . ?
C39 C38 C37 123.0(2) . . ?
C40 C39 C38 119.1(3) . . ?
C41 C40 C39 120.6(2) . . ?
C40 C41 C42 120.0(2) . . ?
C37 C42 Cl4 119.27(18) . . ?
C37 C42 C41 121.1(2) . . ?
C41 C42 Cl4 119.46(19) . . ?

# end Validation Reply Form
_olex2_submission_special_instructions 'No special instructions were received'
# start Validation Reply Form
_vrf_PLAT230_jnm122              
;
PROBLEM: Hirshfeld Test Diff for    C40      --C41      .        5.2 s.u.  
RESPONSE: This does not represent an incorrect atom assignment.
These C atoms part of a ring and should have similar anisotropic displacement, there is some disorder which I have modelled with 
RIGU and ISOR that gives better refinement statistics than using 
EADP.
;
_vrf_PLAT911_jnm122              
;
PROBLEM: Missing FCF Refl Between Thmin & STh/L=    0.600         12 Report
RESPONSE: This represents only a very small number of reflections compared 
with the total number that were collected, and may result from weak diffraction,
or partial obstruction by the beamstop.
;
####################################################################### 
# 
# 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_cu_jnm130
_database_code_depnum_ccdc_archive 'CCDC 2237933'
loop_
_audit_author_name
_audit_author_address
'Jennifer Murphy'
;University of Guelph
Canada
;
_audit_update_record             
;
2023-01-25 deposited with the CCDC.	2024-04-11 downloaded from the CCDC.
;
_audit_creation_date             2023-01-24
_audit_creation_method           
;
Olex2 1.5
(compiled 2022.04.07 svn.rca3783a0 for OlexSys, GUI svn.r6498)
;
_shelx_SHELXL_version_number     2018/3
_chemical_name_common            ?
_chemical_name_systematic        ?
_chemical_formula_moiety         'C40 H38 Cl4 N6 O4 Zn, C2 H6 O'
_chemical_formula_sum            'C42 H44 Cl4 N6 O5 Zn'
_chemical_formula_weight         920.00
_chemical_melting_point          ?
_chemical_oxdiff_formula         'C11 H10 N O'
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0181 0.0091 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Cl Cl 0.3639 0.7018 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0311 0.0180 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0492 0.0322 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Zn Zn -1.5491 0.6778 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_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/n 1'
_space_group_name_Hall           '-P 2yn'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x+1/2, y+1/2, -z+1/2'
'-x, -y, -z'
'x-1/2, -y-1/2, z-1/2'

_cell_length_a                   14.82310(10)
_cell_length_b                   14.77870(10)
_cell_length_c                   19.9676(2)
_cell_angle_alpha                90
_cell_angle_beta                 96.8790(10)
_cell_angle_gamma                90
_cell_volume                     4342.74(6)
_cell_formula_units_Z            4
_cell_measurement_reflns_used    34458
_cell_measurement_temperature    298
_cell_measurement_theta_max      77.0040
_cell_measurement_theta_min      2.2120
_shelx_estimated_absorpt_T_max   0.625
_shelx_estimated_absorpt_T_min   0.423
_exptl_absorpt_coefficient_mu    3.464
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.67049
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
;
CrysAlisPro 1.171.41.93a (Rigaku Oxford Diffraction, 2020)
Empirical absorption correction using spherical harmonics,
implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_absorpt_special_details   ?
_exptl_crystal_colour            'clear colourless'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.407
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       prism
_exptl_crystal_F_000             1904
_exptl_crystal_size_max          0.3
_exptl_crystal_size_mid          0.15
_exptl_crystal_size_min          0.15
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0652
_diffrn_reflns_av_unetI/netI     0.0252
_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       -17
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_limit_l_min       -24
_diffrn_reflns_number            93894
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 1.000
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         74.497
_diffrn_reflns_theta_min         3.519
_diffrn_ambient_environment      air
_diffrn_ambient_temperature      298
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean ?
_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   -136.76 -25.76   1.00   55.00    -- -105.12  83.74 -29.95  111
  2  ω    176.08 272.08   1.00   55.00    -- -105.12 -59.25  20.08   96
  3  ω   -136.76 -25.76   1.00   55.00    -- -105.12  83.74 130.05  111
  4  ω    176.08 272.08   1.00   55.00    -- -105.12 -59.25 -59.92   96
  5  ω    176.08 272.08   1.00   55.00    -- -105.12 -59.25-179.92   96
  6  ω      3.93  99.93   1.00   30.00    --   20.69  59.25 159.92   96
  7  ω    -26.23  72.77   1.00   32.50    --   50.69 -83.74  80.95   99
  8  ω   -136.76 -25.76   1.00   55.00    -- -105.12  83.74-109.95  111
  9  ω    176.08 272.08   1.00   55.00    -- -105.12 -59.25 -19.92   96
 10  ω    176.08 272.08   1.00   55.00    -- -105.12 -59.25  60.08   96
 11  φ   -339.92  20.08   1.00   45.70 -72.79 -90.12 -59.25    --   360
 12  ω    176.08 272.08   1.00   55.00    -- -105.12 -59.25 140.08   96
 13  ω   -136.76 -25.76   1.00   55.00    -- -105.12  83.74  90.05  111
 14  ω      3.93  99.93   1.00   30.00    --   20.69  59.25  69.92   96
 15  ω   -136.76 -25.76   1.00   55.00    -- -105.12  83.74 170.05  111
 16  ω    176.08 272.08   1.00   55.00    -- -105.12 -59.25 -99.92   96
 17  ω    176.08 272.08   1.00   55.00    -- -105.12 -59.25 100.08   96
 18  ω      3.93  99.93   1.00   30.00    --   20.69  59.25 -20.08   96
 19  ω    176.08 272.08   1.00   55.00    -- -105.12 -59.25-139.92   96
 20  ω    -26.23  72.77   1.00   32.50    --   50.69 -83.74-126.05   99
 21  ω   -136.76 -25.76   1.00   55.00    -- -105.12  83.74 -69.95  111
 22  ω    191.08 287.08   1.00   45.70    --  -90.12 -59.25 -69.92   96
 23  ω   -136.76 -25.76   1.00   55.00    -- -105.12  83.74-149.95  111
 24  ω   -136.76 -25.76   1.00   55.00    -- -105.12  83.74  50.05  111
 25  ω    191.08 287.08   1.00   45.70    --  -90.12 -59.25  20.08   96
 26  ω      3.93  99.93   1.00   30.00    --   20.69  59.25-110.08   96
;
_diffrn_measurement_device       'abstract diffractometer'
_diffrn_measurement_device_type  
'Saxi-CrysAlisPro-abstract goniometer imported SAXI images'
_diffrn_measurement_method       'ω and φ scans'
_diffrn_orient_matrix_type       
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      0.0248771000
_diffrn_orient_matrix_UB_12      0.0378053000
_diffrn_orient_matrix_UB_13      0.0717086000
_diffrn_orient_matrix_UB_21      0.0375538000
_diffrn_orient_matrix_UB_22      -0.0932353000
_diffrn_orient_matrix_UB_23      0.0238047000
_diffrn_orient_matrix_UB_31      0.0945804000
_diffrn_orient_matrix_UB_32      0.0271695000
_diffrn_orient_matrix_UB_33      -0.0180230000
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Cu K\a'
_diffrn_radiation_wavelength     1.54184
_diffrn_source                   'fine-focus sealed X-ray tube'
_diffrn_source_type              'Enhance (Cu) X-ray Source'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                7397
_reflns_number_total             8888
_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 1.171.41.93a (Rigaku OD, 2020)'
_computing_data_collection       'CrysAlisPro 1.171.41.93a (Rigaku OD, 2020)'
_computing_data_reduction        'CrysAlisPro 1.171.41.93a (Rigaku OD, 2020)'
_computing_molecular_graphics    'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2018/3 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT 2018/2 (Sheldrick, 2018)'
_refine_diff_density_max         0.333
_refine_diff_density_min         -0.453
_refine_diff_density_rms         0.064
_refine_ls_extinction_coef       0.00346(15)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4^
_refine_ls_extinction_method     'SHELXL-2018/3 (Sheldrick 2018)'
_refine_ls_goodness_of_fit_ref   1.044
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     573
_refine_ls_number_reflns         8888
_refine_ls_number_restraints     113
_refine_ls_R_factor_all          0.0566
_refine_ls_R_factor_gt           0.0486
_refine_ls_restrained_S_all      1.058
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0794P)²+1.7250P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1357
_refine_ls_wR_factor_ref         0.1454
_refine_special_details          ?
_olex2_refinement_description    
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups, All N(H) groups
 At 1.5 times of:
  All C(H,H,H) groups, All O(H) groups
2. Restrained distances
 O5-C41
 1.43 with sigma of 0.02
 C41-C42
 1.515 with sigma of 0.02
 C39A-C40A \\sim C39-C40
 with sigma of 0.02
 N4-C38 \\sim N4-C38A
 with sigma of 0.02
 N4-C38 \\sim N4A-C38
 with sigma of 0.02
 C38-C39 \\sim C38A-C39A
 with sigma of 0.02
 C39-C40 \\sim C39A-C40A
 with sigma of 0.02
 C35-C38 \\sim C35A-C38
 with sigma of 0.04
 C35-N4 \\sim C35A-N4A
 with sigma of 0.02
 N4-C37 \\sim N4A-C37
 with sigma of 0.02
 N4-C39 \\sim N4-C39A
 with sigma of 0.04
 C38-C40 \\sim C38A-C40A
 with sigma of 0.04
 N4-C38A \\sim N4A-C38A
 with sigma of 0.02
 N3-N4 \\sim N3-N4A
 with sigma of 0.04
 C35-C37 \\sim C35A-C37
 with sigma of 0.04
 C35-C38A \\sim C35A-C38A
 with sigma of 0.04
 N4-C38 \\sim N4A-C38A
 with sigma of 0.02
 N3-C35 \\sim C35-C35A
 with sigma of 0.02
 N3-C35 \\sim N3-C35A
 with sigma of 0.02
 N4-C35 \\sim N4A-C35A
 with sigma of 0.02
3. Rigid body (RIGU) restrains
 C40, C40A, C39A, C39, C38, C38A, N4A, N4, C35, C35A, N3, C36, C37
 with sigma for 1-2 distances of 0.001 and sigma for 1-3 distances of 0.001
 C42, C41, O5
 with sigma for 1-2 distances of 0.001 and sigma for 1-3 distances of 0.001
4. Others
 Sof(C38A)=Sof(H38C)=Sof(H38D)=Sof(C39A)=Sof(H39C)=Sof(H39D)=Sof(C40A)=
 Sof(H40C)=Sof(H40D)=1-FVAR(1)
 Sof(C38)=Sof(H38A)=Sof(H38B)=Sof(C39)=Sof(H39A)=Sof(H39B)=Sof(C40)=Sof(H40A)=
 Sof(H40B)=FVAR(1)
 Sof(N4A)=Sof(C35A)=Sof(H35A)=Sof(H37A)=1-FVAR(2)
 Sof(N4)=Sof(C35)=Sof(H35)=Sof(H37)=FVAR(2)
5.a Secondary CH2 refined with riding coordinates:
 C2(H2A,H2B), C16(H16A,H16B), C32(H32A,H32B), C33(H33A,H33B), C34(H34A,H34B),
 C38(H38A,H38B), C38A(H38C,H38D), C39(H39A,H39B), C39A(H39C,H39D), C40(H40A,
 H40B), C40A(H40C,H40D), C41(H41A,H41B)
5.b Aromatic/amide H refined with riding coordinates:
 N5(H5), N6(H6), C4(H4), C5(H5A), C6(H6A), C7(H7), C11(H11), C12(H12),
 C13(H13), C18(H18), C19(H19), C20(H20), C21(H21), C25(H25), C26(H26), C27(H27),
  C29(H29), C30(H30), C31(H31), C35(H35), C35A(H35A), C36(H36), C37(H37),
 C37(H37A)
5.c Idealised Me refined as rotating group:
 C42(H42A,H42B,H42C)
5.d Idealised tetrahedral OH refined as rotating group:
 O5(H5B)
;
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_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
Zn1 Zn 0.75577(2) 0.29001(2) 0.75751(2) 0.04945(12) Uani 1 1 d . . . . .
Cl1 Cl 0.42951(8) 0.04905(7) 0.75753(5) 0.1017(3) Uani 1 1 d . . . . .
Cl2 Cl 0.30437(7) 0.20135(7) 0.51846(5) 0.0979(3) Uani 1 1 d . . . . .
Cl3 Cl 0.73505(5) 0.29421(5) 0.54487(4) 0.0748(2) Uani 1 1 d . . . . .
Cl4 Cl 1.06885(6) 0.21688(6) 0.47759(5) 0.0927(3) Uani 1 1 d . . . . .
O1 O 0.65709(11) 0.32178(12) 0.68691(9) 0.0559(4) Uani 1 1 d . . . . .
O2 O 0.55016(13) 0.29095(14) 0.75211(10) 0.0700(5) Uani 1 1 d . . . . .
O3 O 0.85992(12) 0.28412(13) 0.70273(10) 0.0650(5) Uani 1 1 d . . . . .
O4 O 0.93999(18) 0.27923(18) 0.80238(13) 0.0956(8) Uani 1 1 d . . . . .
N1 N 0.76449(13) 0.40063(13) 0.81637(10) 0.0519(4) Uani 1 1 d . . . . .
N2 N 0.81982(13) 0.52982(13) 0.85643(10) 0.0516(4) Uani 1 1 d . . . . .
N3 N 0.74160(17) 0.17226(14) 0.80382(11) 0.0649(5) Uani 1 1 d D . . . .
N4 N 0.7193(4) 0.0843(3) 0.8878(3) 0.0605(13) Uani 0.511(8) 1 d D . P A 1
N4A N 0.6695(5) 0.0611(4) 0.8538(4) 0.0765(17) Uani 0.489(8) 1 d D . P A 2
N5 N 0.40013(15) 0.20299(13) 0.66140(14) 0.0659(6) Uani 1 1 d . . . . .
H5 H 0.456931 0.199918 0.676323 0.079 Uiso 1 1 calc R U . . .
N6 N 0.92651(16) 0.24043(15) 0.57408(12) 0.0664(6) Uani 1 1 d . . . . .
H6 H 0.915105 0.284883 0.599561 0.080 Uiso 1 1 calc R U . . .
C1 C 0.57543(15) 0.32013(15) 0.70004(12) 0.0491(5) Uani 1 1 d . . . . .
C2 C 0.50927(16) 0.35627(19) 0.64242(13) 0.0591(6) Uani 1 1 d . . . . .
H2A H 0.530636 0.415506 0.630529 0.071 Uiso 1 1 calc R U . . .
H2B H 0.512674 0.317174 0.603782 0.071 Uiso 1 1 calc R U . . .
C3 C 0.41056(16) 0.36535(16) 0.65249(13) 0.0543(5) Uani 1 1 d . . . . .
C4 C 0.3691(2) 0.44951(19) 0.65024(16) 0.0697(7) Uani 1 1 d . . . . .
H4 H 0.404126 0.501049 0.646423 0.084 Uiso 1 1 calc R U . . .
C5 C 0.2778(2) 0.4586(2) 0.6535(2) 0.0855(10) Uani 1 1 d . . . . .
H5A H 0.251344 0.515760 0.651901 0.103 Uiso 1 1 calc R U . . .
C6 C 0.2255(2) 0.3830(2) 0.6591(2) 0.0878(10) Uani 1 1 d . . . . .
H6A H 0.163407 0.388767 0.660905 0.105 Uiso 1 1 calc R U . . .
C7 C 0.2651(2) 0.2984(2) 0.6622(2) 0.0777(9) Uani 1 1 d . . . . .
H7 H 0.229612 0.247272 0.666456 0.093 Uiso 1 1 calc R U . . .
C8 C 0.35718(17) 0.28920(16) 0.65889(15) 0.0582(6) Uani 1 1 d . . . . .
C9 C 0.35484(18) 0.12336(17) 0.64092(16) 0.0643(7) Uani 1 1 d . . . . .
C10 C 0.3050(2) 0.1147(2) 0.57703(18) 0.0733(7) Uani 1 1 d . . . . .
C11 C 0.2593(3) 0.0354(2) 0.5563(2) 0.0920(10) Uani 1 1 d . . . . .
H11 H 0.223759 0.032603 0.514627 0.110 Uiso 1 1 calc R U . . .
C12 C 0.2671(3) -0.0377(2) 0.5975(3) 0.1021(13) Uani 1 1 d . . . . .
H12 H 0.236839 -0.090881 0.583773 0.122 Uiso 1 1 calc R U . . .
C13 C 0.3188(3) -0.0345(2) 0.6588(2) 0.0962(12) Uani 1 1 d . . . . .
H13 H 0.324803 -0.085527 0.686165 0.115 Uiso 1 1 calc R U . . .
C14 C 0.3623(2) 0.04565(19) 0.68006(17) 0.0742(8) Uani 1 1 d . . . . .
C15 C 0.93415(19) 0.27735(18) 0.74049(16) 0.0636(6) Uani 1 1 d . . . . .
C16 C 1.01895(18) 0.2654(2) 0.70603(18) 0.0730(7) Uani 1 1 d . . . . .
H16A H 1.022713 0.314137 0.673923 0.088 Uiso 1 1 calc R U . . .
H16B H 1.072038 0.268961 0.739426 0.088 Uiso 1 1 calc R U . . .
C17 C 1.01896(17) 0.17602(19) 0.66983(16) 0.0653(7) Uani 1 1 d . . . . .
C18 C 1.0624(2) 0.1013(2) 0.70223(19) 0.0831(9) Uani 1 1 d . . . . .
H18 H 1.091555 0.107709 0.745867 0.100 Uiso 1 1 calc R U . . .
C19 C 1.0628(3) 0.0185(3) 0.6709(2) 0.0946(11) Uani 1 1 d . . . . .
H19 H 1.092541 -0.030403 0.693034 0.114 Uiso 1 1 calc R U . . .
C20 C 1.0192(3) 0.0088(2) 0.60694(19) 0.0869(10) Uani 1 1 d . . . . .
H20 H 1.019466 -0.047171 0.585610 0.104 Uiso 1 1 calc R U . . .
C21 C 0.9745(2) 0.08121(19) 0.57350(16) 0.0719(7) Uani 1 1 d . . . . .
H21 H 0.944768 0.073772 0.530117 0.086 Uiso 1 1 calc R U . . .
C22 C 0.97429(17) 0.16525(17) 0.60528(15) 0.0612(6) Uani 1 1 d . . . . .
C23 C 0.89693(19) 0.24770(16) 0.50595(14) 0.0632(6) Uani 1 1 d . . . . .
C24 C 0.9533(2) 0.23633(19) 0.45488(17) 0.0736(8) Uani 1 1 d . . . . .
C25 C 0.9223(3) 0.2444(2) 0.38755(18) 0.0879(10) Uani 1 1 d . . . . .
H25 H 0.961147 0.233624 0.355179 0.105 Uiso 1 1 calc R U . . .
C26 C 0.8330(3) 0.2687(2) 0.36817(19) 0.0920(11) Uani 1 1 d . . . . .
H26 H 0.811544 0.273978 0.322641 0.110 Uiso 1 1 calc R U . . .
C27 C 0.7757(3) 0.2850(2) 0.41654(18) 0.0791(8) Uani 1 1 d . . . . .
H27 H 0.716145 0.303439 0.403763 0.095 Uiso 1 1 calc R U . . .
C28 C 0.8070(2) 0.27390(17) 0.48337(15) 0.0653(7) Uani 1 1 d . . . . .
C29 C 0.69715(17) 0.44725(18) 0.84248(14) 0.0608(6) Uani 1 1 d . . . . .
H29 H 0.637640 0.427455 0.842775 0.073 Uiso 1 1 calc R U . . .
C30 C 0.73096(18) 0.52682(18) 0.86782(14) 0.0621(6) Uani 1 1 d . . . . .
H30 H 0.699680 0.570956 0.888931 0.075 Uiso 1 1 calc R U . . .
C31 C 0.83728(16) 0.45267(16) 0.82596(12) 0.0536(5) Uani 1 1 d . . . . .
H31 H 0.893583 0.437413 0.813089 0.064 Uiso 1 1 calc R U . . .
C32 C 0.88618(18) 0.60130(16) 0.87660(14) 0.0608(6) Uani 1 1 d . . . . .
H32A H 0.856321 0.659669 0.870886 0.073 Uiso 1 1 calc R U . . .
H32B H 0.933694 0.599597 0.847174 0.073 Uiso 1 1 calc R U . . .
C33 C 0.92843(18) 0.59190(17) 0.94851(14) 0.0615(6) Uani 1 1 d . . . . .
H33A H 0.881349 0.599125 0.977899 0.074 Uiso 1 1 calc R U . . .
H33B H 0.971986 0.640440 0.958567 0.074 Uiso 1 1 calc R U . . .
C34 C 0.97614(18) 0.50226(17) 0.96444(13) 0.0595(6) Uani 1 1 d . . . . .
H34A H 0.931812 0.453798 0.958009 0.071 Uiso 1 1 calc R U . . .
H34B H 1.020300 0.492676 0.933012 0.071 Uiso 1 1 calc R U . . .
C35 C 0.7108(5) 0.1676(4) 0.8623(3) 0.0611(16) Uani 0.511(8) 1 d D . P A 1
H35 H 0.686080 0.216246 0.883469 0.073 Uiso 0.511(8) 1 calc R U P A 1
C35A C 0.6614(5) 0.1456(4) 0.8295(4) 0.0712(18) Uani 0.489(8) 1 d D . P A 2
H35A H 0.610007 0.181649 0.829624 0.085 Uiso 0.489(8) 1 calc R U P A 2
C36 C 0.7864(2) 0.09275(18) 0.80057(15) 0.0684(6) Uani 1 1 d . . . . .
H36 H 0.831241 0.082325 0.772653 0.082 Uiso 1 1 calc R U . . .
C37 C 0.7585(3) 0.0318(2) 0.84198(17) 0.0811(8) Uani 1 1 d D . . . .
H37 H 0.763947 -0.030801 0.840575 0.097 Uiso 0.511(8) 1 calc R U P A 1
H37A H 0.789813 -0.018998 0.859631 0.097 Uiso 0.489(8) 1 calc R U P A 2
C38 C 0.6842(4) 0.0529(4) 0.9496(3) 0.0786(16) Uani 0.555(7) 1 d D . P A 1
H38A H 0.692746 0.099784 0.983716 0.094 Uiso 0.555(7) 1 calc R U P A 1
H38B H 0.717808 -0.000201 0.966775 0.094 Uiso 0.555(7) 1 calc R U P A 1
C38A C 0.6013(7) 0.0132(7) 0.8899(5) 0.107(3) Uani 0.445(7) 1 d D . P A 2
H38C H 0.541342 0.036295 0.873770 0.129 Uiso 0.445(7) 1 calc R U P A 2
H38D H 0.602189 -0.050625 0.878635 0.129 Uiso 0.445(7) 1 calc R U P A 2
C39 C 0.5841(5) 0.0298(6) 0.9354(4) 0.0786(19) Uani 0.555(7) 1 d D . P A 1
H39A H 0.575928 -0.008183 0.895566 0.094 Uiso 0.555(7) 1 calc R U P A 1
H39B H 0.551167 0.085613 0.924337 0.094 Uiso 0.555(7) 1 calc R U P A 1
C39A C 0.6160(8) 0.0226(10) 0.9617(6) 0.101(3) Uani 0.445(7) 1 d D . P A 2
H39C H 0.639919 0.083153 0.970056 0.121 Uiso 0.445(7) 1 calc R U P A 2
H39D H 0.665242 -0.018516 0.976854 0.121 Uiso 0.445(7) 1 calc R U P A 2
C40 C 0.5386(12) -0.0185(10) 0.9918(7) 0.137(6) Uani 0.555(7) 1 d D . P A 1
H40A H 0.525826 -0.080467 0.977757 0.164 Uiso 0.555(7) 1 calc R U P A 1
H40B H 0.582162 -0.020507 1.032085 0.164 Uiso 0.555(7) 1 calc R U P A 1
C40A C 0.5487(10) 0.0103(11) 1.0084(6) 0.086(3) Uani 0.445(7) 1 d D . P A 2
H40C H 0.551012 0.065185 1.035157 0.103 Uiso 0.445(7) 1 calc R U P A 2
H40D H 0.572558 -0.037435 1.038877 0.103 Uiso 0.445(7) 1 calc R U P A 2
O5 O 1.0500(3) 0.1659(4) 0.8852(2) 0.1595(16) Uani 1 1 d D . . . .
H5B H 1.034838 0.211161 0.862830 0.239 Uiso 1 1 calc R U . . .
C41 C 1.0089(7) 0.1674(8) 0.9455(4) 0.217(4) Uani 1 1 d D . . . .
H41A H 1.056671 0.156800 0.982313 0.260 Uiso 1 1 calc R U . . .
H41B H 0.987131 0.228570 0.950966 0.260 Uiso 1 1 calc R U . . .
C42 C 0.9428(7) 0.1133(8) 0.9543(5) 0.244(5) Uani 1 1 d D . . . .
H42A H 0.899574 0.112867 0.914452 0.367 Uiso 1 1 calc R U . . .
H42B H 0.913634 0.133542 0.992007 0.367 Uiso 1 1 calc R U . . .
H42C H 0.966147 0.053290 0.962941 0.367 Uiso 1 1 calc R U . . .


_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
Zn1 O1 1.9628(17) . ?
Zn1 O3 1.9980(18) . ?
Zn1 N1 2.0085(19) . ?
Zn1 N3 1.994(2) . ?
Cl1 C14 1.737(4) . ?
Cl2 C10 1.733(3) . ?
Cl3 C28 1.747(3) . ?
Cl4 C24 1.742(4) . ?
O1 C1 1.269(3) . ?
O2 C1 1.225(3) . ?
O3 C15 1.261(4) . ?
O4 C15 1.229(4) . ?
N1 C29 1.367(3) . ?
N1 C31 1.320(3) . ?
N2 C30 1.364(3) . ?
N2 C31 1.332(3) . ?
N2 C32 1.467(3) . ?
N3 C35 1.306(5) . ?
N3 C35A 1.406(7) . ?
N3 C36 1.355(3) . ?
N4 C35 1.333(6) . ?
N4 C37 1.380(5) . ?
N4 C38 1.469(6) . ?
N4A C35A 1.341(7) . ?
N4A C37 1.434(7) . ?
N4A C38A 1.488(9) . ?
N5 H5 0.8600 . ?
N5 C8 1.423(3) . ?
N5 C9 1.392(3) . ?
N6 H6 0.8600 . ?
N6 C22 1.421(3) . ?
N6 C23 1.383(4) . ?
C1 C2 1.517(3) . ?
C2 H2A 0.9700 . ?
C2 H2B 0.9700 . ?
C2 C3 1.507(3) . ?
C3 C4 1.386(4) . ?
C3 C8 1.390(3) . ?
C4 H4 0.9300 . ?
C4 C5 1.369(4) . ?
C5 H5A 0.9300 . ?
C5 C6 1.372(5) . ?
C6 H6A 0.9300 . ?
C6 C7 1.379(4) . ?
C7 H7 0.9300 . ?
C7 C8 1.381(4) . ?
C9 C10 1.401(5) . ?
C9 C14 1.386(4) . ?
C10 C11 1.393(4) . ?
C11 H11 0.9300 . ?
C11 C12 1.354(6) . ?
C12 H12 0.9300 . ?
C12 C13 1.365(6) . ?
C13 H13 0.9300 . ?
C13 C14 1.390(5) . ?
C15 C16 1.514(4) . ?
C16 H16A 0.9700 . ?
C16 H16B 0.9700 . ?
C16 C17 1.506(4) . ?
C17 C18 1.398(4) . ?
C17 C22 1.386(4) . ?
C18 H18 0.9300 . ?
C18 C19 1.374(5) . ?
C19 H19 0.9300 . ?
C19 C20 1.369(6) . ?
C20 H20 0.9300 . ?
C20 C21 1.388(5) . ?
C21 H21 0.9300 . ?
C21 C22 1.395(4) . ?
C23 C24 1.404(4) . ?
C23 C28 1.409(4) . ?
C24 C25 1.373(5) . ?
C25 H25 0.9300 . ?
C25 C26 1.380(6) . ?
C26 H26 0.9300 . ?
C26 C27 1.382(5) . ?
C27 H27 0.9300 . ?
C27 C28 1.369(5) . ?
C29 H29 0.9300 . ?
C29 C30 1.353(4) . ?
C30 H30 0.9300 . ?
C31 H31 0.9300 . ?
C32 H32A 0.9700 . ?
C32 H32B 0.9700 . ?
C32 C33 1.503(4) . ?
C33 H33A 0.9700 . ?
C33 H33B 0.9700 . ?
C33 C34 1.517(4) . ?
C34 C34 1.510(5) 3_767 ?
C34 H34A 0.9700 . ?
C34 H34B 0.9700 . ?
C35 H35 0.9300 . ?
C35A H35A 0.9300 . ?
C36 H36 0.9300 . ?
C36 C37 1.322(4) . ?
C37 H37 0.9300 . ?
C37 H37A 0.9300 . ?
C38 H38A 0.9700 . ?
C38 H38B 0.9700 . ?
C38 C39 1.516(9) . ?
C38A H38C 0.9700 . ?
C38A H38D 0.9700 . ?
C38A C39A 1.432(12) . ?
C39 H39A 0.9700 . ?
C39 H39B 0.9700 . ?
C39 C40 1.553(10) . ?
C39A H39C 0.9700 . ?
C39A H39D 0.9700 . ?
C39A C40A 1.456(12) . ?
C40 C40 1.34(3) 3_657 ?
C40 H40A 0.9700 . ?
C40 H40B 0.9700 . ?
C40A C40A 1.47(3) 3_657 ?
C40A H40C 0.9700 . ?
C40A H40D 0.9700 . ?
O5 H5B 0.8200 . ?
O5 C41 1.414(8) . ?
C41 H41A 0.9700 . ?
C41 H41B 0.9700 . ?
C41 C42 1.293(10) . ?
C42 H42A 0.9600 . ?
C42 H42B 0.9600 . ?
C42 H42C 0.9600 . ?

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
O1 Zn1 O3 100.11(8) . . ?
O1 Zn1 N1 102.46(8) . . ?
O1 Zn1 N3 115.54(9) . . ?
O3 Zn1 N1 110.86(8) . . ?
N3 Zn1 O3 110.31(8) . . ?
N3 Zn1 N1 116.23(9) . . ?
C1 O1 Zn1 119.62(15) . . ?
C15 O3 Zn1 110.62(18) . . ?
C29 N1 Zn1 129.41(16) . . ?
C31 N1 Zn1 123.59(15) . . ?
C31 N1 C29 105.8(2) . . ?
C30 N2 C32 127.4(2) . . ?
C31 N2 C30 107.0(2) . . ?
C31 N2 C32 125.5(2) . . ?
C35 N3 Zn1 121.9(3) . . ?
C35 N3 C36 102.9(3) . . ?
C35A N3 Zn1 123.7(3) . . ?
C36 N3 Zn1 130.94(19) . . ?
C36 N3 C35A 102.4(3) . . ?
C35 N4 C37 107.1(4) . . ?
C35 N4 C38 125.9(4) . . ?
C37 N4 C38 126.8(4) . . ?
C35A N4A C37 105.4(5) . . ?
C35A N4A C38A 125.6(7) . . ?
C37 N4A C38A 128.9(6) . . ?
C8 N5 H5 118.4 . . ?
C9 N5 H5 118.4 . . ?
C9 N5 C8 123.3(2) . . ?
C22 N6 H6 117.5 . . ?
C23 N6 H6 117.5 . . ?
C23 N6 C22 125.1(2) . . ?
O1 C1 C2 112.5(2) . . ?
O2 C1 O1 125.3(2) . . ?
O2 C1 C2 122.2(2) . . ?
C1 C2 H2A 107.6 . . ?
C1 C2 H2B 107.6 . . ?
H2A C2 H2B 107.1 . . ?
C3 C2 C1 118.7(2) . . ?
C3 C2 H2A 107.6 . . ?
C3 C2 H2B 107.6 . . ?
C4 C3 C2 120.6(2) . . ?
C4 C3 C8 118.3(2) . . ?
C8 C3 C2 120.8(2) . . ?
C3 C4 H4 119.2 . . ?
C5 C4 C3 121.6(3) . . ?
C5 C4 H4 119.2 . . ?
C4 C5 H5A 120.2 . . ?
C4 C5 C6 119.6(3) . . ?
C6 C5 H5A 120.2 . . ?
C5 C6 H6A 120.0 . . ?
C5 C6 C7 120.1(3) . . ?
C7 C6 H6A 120.0 . . ?
C6 C7 H7 119.9 . . ?
C6 C7 C8 120.3(3) . . ?
C8 C7 H7 119.9 . . ?
C3 C8 N5 118.1(2) . . ?
C7 C8 N5 121.8(2) . . ?
C7 C8 C3 120.1(2) . . ?
N5 C9 C10 121.9(3) . . ?
C14 C9 N5 122.1(3) . . ?
C14 C9 C10 115.8(3) . . ?
C9 C10 Cl2 120.4(2) . . ?
C11 C10 Cl2 117.2(3) . . ?
C11 C10 C9 122.2(3) . . ?
C10 C11 H11 120.4 . . ?
C12 C11 C10 119.1(4) . . ?
C12 C11 H11 120.4 . . ?
C11 C12 H12 119.5 . . ?
C11 C12 C13 121.0(3) . . ?
C13 C12 H12 119.5 . . ?
C12 C13 H13 120.2 . . ?
C12 C13 C14 119.6(4) . . ?
C14 C13 H13 120.2 . . ?
C9 C14 Cl1 118.5(2) . . ?
C9 C14 C13 122.0(4) . . ?
C13 C14 Cl1 119.5(3) . . ?
O3 C15 C16 116.7(3) . . ?
O4 C15 O3 123.4(3) . . ?
O4 C15 C16 119.8(3) . . ?
C15 C16 H16A 109.3 . . ?
C15 C16 H16B 109.3 . . ?
H16A C16 H16B 108.0 . . ?
C17 C16 C15 111.6(2) . . ?
C17 C16 H16A 109.3 . . ?
C17 C16 H16B 109.3 . . ?
C18 C17 C16 119.8(3) . . ?
C22 C17 C16 121.3(3) . . ?
C22 C17 C18 118.8(3) . . ?
C17 C18 H18 119.3 . . ?
C19 C18 C17 121.3(4) . . ?
C19 C18 H18 119.3 . . ?
C18 C19 H19 120.3 . . ?
C20 C19 C18 119.4(3) . . ?
C20 C19 H19 120.3 . . ?
C19 C20 H20 119.6 . . ?
C19 C20 C21 120.8(3) . . ?
C21 C20 H20 119.6 . . ?
C20 C21 H21 120.2 . . ?
C20 C21 C22 119.7(3) . . ?
C22 C21 H21 120.2 . . ?
C17 C22 N6 118.4(2) . . ?
C17 C22 C21 119.9(3) . . ?
C21 C22 N6 121.7(3) . . ?
N6 C23 C24 124.0(3) . . ?
N6 C23 C28 120.8(2) . . ?
C24 C23 C28 115.0(3) . . ?
C23 C24 Cl4 118.9(3) . . ?
C25 C24 Cl4 118.2(2) . . ?
C25 C24 C23 122.8(3) . . ?
C24 C25 H25 120.2 . . ?
C24 C25 C26 119.7(3) . . ?
C26 C25 H25 120.2 . . ?
C25 C26 H26 120.1 . . ?
C25 C26 C27 119.9(4) . . ?
C27 C26 H26 120.1 . . ?
C26 C27 H27 120.2 . . ?
C28 C27 C26 119.7(4) . . ?
C28 C27 H27 120.2 . . ?
C23 C28 Cl3 117.1(2) . . ?
C27 C28 Cl3 120.0(3) . . ?
C27 C28 C23 122.8(3) . . ?
N1 C29 H29 125.5 . . ?
C30 C29 N1 109.0(2) . . ?
C30 C29 H29 125.5 . . ?
N2 C30 H30 126.6 . . ?
C29 C30 N2 106.7(2) . . ?
C29 C30 H30 126.6 . . ?
N1 C31 N2 111.4(2) . . ?
N1 C31 H31 124.3 . . ?
N2 C31 H31 124.3 . . ?
N2 C32 H32A 109.1 . . ?
N2 C32 H32B 109.1 . . ?
N2 C32 C33 112.6(2) . . ?
H32A C32 H32B 107.8 . . ?
C33 C32 H32A 109.1 . . ?
C33 C32 H32B 109.1 . . ?
C32 C33 H33A 108.7 . . ?
C32 C33 H33B 108.7 . . ?
C32 C33 C34 114.3(2) . . ?
H33A C33 H33B 107.6 . . ?
C34 C33 H33A 108.7 . . ?
C34 C33 H33B 108.7 . . ?
C33 C34 H34A 109.0 . . ?
C33 C34 H34B 109.0 . . ?
C34 C34 C33 112.9(3) 3_767 . ?
C34 C34 H34A 109.0 3_767 . ?
C34 C34 H34B 109.0 3_767 . ?
H34A C34 H34B 107.8 . . ?
N3 C35 N4 111.3(4) . . ?
N3 C35 H35 124.4 . . ?
N4 C35 H35 124.4 . . ?
N3 C35A H35A 124.8 . . ?
N4A C35A N3 110.5(5) . . ?
N4A C35A H35A 124.8 . . ?
N3 C36 H36 124.2 . . ?
C37 C36 N3 111.6(3) . . ?
C37 C36 H36 124.2 . . ?
N4 C37 H37 128.6 . . ?
N4A C37 H37A 127.4 . . ?
C36 C37 N4 102.8(3) . . ?
C36 C37 N4A 105.1(3) . . ?
C36 C37 H37 128.6 . . ?
C36 C37 H37A 127.4 . . ?
N4 C38 H38A 109.5 . . ?
N4 C38 H38B 109.5 . . ?
N4 C38 C39 110.6(5) . . ?
H38A C38 H38B 108.1 . . ?
C39 C38 H38A 109.5 . . ?
C39 C38 H38B 109.5 . . ?
N4A C38A H38C 108.7 . . ?
N4A C38A H38D 108.7 . . ?
H38C C38A H38D 107.6 . . ?
C39A C38A N4A 114.1(8) . . ?
C39A C38A H38C 108.7 . . ?
C39A C38A H38D 108.7 . . ?
C38 C39 H39A 107.8 . . ?
C38 C39 H39B 107.8 . . ?
C38 C39 C40 117.9(9) . . ?
H39A C39 H39B 107.2 . . ?
C40 C39 H39A 107.8 . . ?
C40 C39 H39B 107.8 . . ?
C38A C39A H39C 105.7 . . ?
C38A C39A H39D 105.7 . . ?
C38A C39A C40A 126.6(11) . . ?
H39C C39A H39D 106.1 . . ?
C40A C39A H39C 105.7 . . ?
C40A C39A H39D 105.7 . . ?
C39 C40 H40A 108.2 . . ?
C39 C40 H40B 108.2 . . ?
C40 C40 C39 116.5(18) 3_657 . ?
C40 C40 H40A 108.2 3_657 . ?
C40 C40 H40B 108.2 3_657 . ?
H40A C40 H40B 107.3 . . ?
C39A C40A C40A 127.4(14) . 3_657 ?
C39A C40A H40C 105.5 . . ?
C39A C40A H40D 105.5 . . ?
C40A C40A H40C 105.5 3_657 . ?
C40A C40A H40D 105.5 3_657 . ?
H40C C40A H40D 106.0 . . ?
C41 O5 H5B 109.5 . . ?
O5 C41 H41A 107.1 . . ?
O5 C41 H41B 107.1 . . ?
H41A C41 H41B 106.8 . . ?
C42 C41 O5 121.1(8) . . ?
C42 C41 H41A 107.1 . . ?
C42 C41 H41B 107.1 . . ?
C41 C42 H42A 109.5 . . ?
C41 C42 H42B 109.5 . . ?
C41 C42 H42C 109.5 . . ?
H42A C42 H42B 109.5 . . ?
H42A C42 H42C 109.5 . . ?
H42B C42 H42C 109.5 . . ?

loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
Zn1 O1 C1 O2 -8.1(3) . . . . ?
Zn1 O1 C1 C2 173.72(16) . . . . ?
Zn1 O3 C15 O4 -3.6(4) . . . . ?
Zn1 O3 C15 C16 175.76(19) . . . . ?
Zn1 N1 C29 C30 -168.02(19) . . . . ?
Zn1 N1 C31 N2 168.33(16) . . . . ?
Zn1 N3 C35 N4 -171.1(4) . . . . ?
Zn1 N3 C35A N4A 175.9(4) . . . . ?
Zn1 N3 C36 C37 177.2(2) . . . . ?
Cl2 C10 C11 C12 172.1(3) . . . . ?
Cl4 C24 C25 C26 -173.6(3) . . . . ?
O1 C1 C2 C3 -175.3(2) . . . . ?
O2 C1 C2 C3 6.4(4) . . . . ?
O3 C15 C16 C17 -66.4(4) . . . . ?
O4 C15 C16 C17 113.0(3) . . . . ?
N1 C29 C30 N2 0.8(3) . . . . ?
N2 C32 C33 C34 57.7(3) . . . . ?
N3 C36 C37 N4 -20.7(5) . . . . ?
N3 C36 C37 N4A 22.2(5) . . . . ?
N4 C38 C39 C40 170.7(8) . . . . ?
N4A C38A C39A C40A 158.7(13) . . . . ?
N5 C9 C10 Cl2 4.4(4) . . . . ?
N5 C9 C10 C11 -179.8(3) . . . . ?
N5 C9 C14 Cl1 0.8(4) . . . . ?
N5 C9 C14 C13 -178.4(3) . . . . ?
N6 C23 C24 Cl4 -3.0(4) . . . . ?
N6 C23 C24 C25 -179.6(3) . . . . ?
N6 C23 C28 Cl3 -1.3(3) . . . . ?
N6 C23 C28 C27 177.7(3) . . . . ?
C1 C2 C3 C4 116.8(3) . . . . ?
C1 C2 C3 C8 -68.4(3) . . . . ?
C2 C3 C4 C5 174.3(3) . . . . ?
C2 C3 C8 N5 5.2(4) . . . . ?
C2 C3 C8 C7 -174.3(3) . . . . ?
C3 C4 C5 C6 0.0(6) . . . . ?
C4 C3 C8 N5 -179.8(3) . . . . ?
C4 C3 C8 C7 0.6(4) . . . . ?
C4 C5 C6 C7 0.7(6) . . . . ?
C5 C6 C7 C8 -0.7(6) . . . . ?
C6 C7 C8 N5 -179.6(3) . . . . ?
C6 C7 C8 C3 0.0(5) . . . . ?
C8 N5 C9 C10 53.2(4) . . . . ?
C8 N5 C9 C14 -132.2(3) . . . . ?
C8 C3 C4 C5 -0.6(5) . . . . ?
C9 N5 C8 C3 -153.3(3) . . . . ?
C9 N5 C8 C7 26.3(5) . . . . ?
C9 C10 C11 C12 -3.8(5) . . . . ?
C10 C9 C14 Cl1 175.7(2) . . . . ?
C10 C9 C14 C13 -3.6(4) . . . . ?
C10 C11 C12 C13 0.2(6) . . . . ?
C11 C12 C13 C14 1.5(6) . . . . ?
C12 C13 C14 Cl1 -179.0(3) . . . . ?
C12 C13 C14 C9 0.3(5) . . . . ?
C14 C9 C10 Cl2 -170.5(2) . . . . ?
C14 C9 C10 C11 5.3(4) . . . . ?
C15 C16 C17 C18 -94.3(3) . . . . ?
C15 C16 C17 C22 83.8(3) . . . . ?
C16 C17 C18 C19 179.3(3) . . . . ?
C16 C17 C22 N6 -1.2(4) . . . . ?
C16 C17 C22 C21 -179.1(2) . . . . ?
C17 C18 C19 C20 -0.6(5) . . . . ?
C18 C17 C22 N6 176.9(2) . . . . ?
C18 C17 C22 C21 -1.0(4) . . . . ?
C18 C19 C20 C21 -0.1(5) . . . . ?
C19 C20 C21 C22 0.3(5) . . . . ?
C20 C21 C22 N6 -177.5(2) . . . . ?
C20 C21 C22 C17 0.3(4) . . . . ?
C22 N6 C23 C24 -53.3(4) . . . . ?
C22 N6 C23 C28 131.3(3) . . . . ?
C22 C17 C18 C19 1.2(4) . . . . ?
C23 N6 C22 C17 164.2(2) . . . . ?
C23 N6 C22 C21 -18.0(4) . . . . ?
C23 C24 C25 C26 3.0(5) . . . . ?
C24 C23 C28 Cl3 -177.11(19) . . . . ?
C24 C23 C28 C27 1.8(4) . . . . ?
C24 C25 C26 C27 0.3(5) . . . . ?
C25 C26 C27 C28 -2.3(5) . . . . ?
C26 C27 C28 Cl3 -179.9(2) . . . . ?
C26 C27 C28 C23 1.2(4) . . . . ?
C28 C23 C24 Cl4 172.6(2) . . . . ?
C28 C23 C24 C25 -3.9(4) . . . . ?
C29 N1 C31 N2 -0.3(3) . . . . ?
C30 N2 C31 N1 0.7(3) . . . . ?
C30 N2 C32 C33 82.5(3) . . . . ?
C31 N1 C29 C30 -0.3(3) . . . . ?
C31 N2 C30 C29 -0.9(3) . . . . ?
C31 N2 C32 C33 -94.0(3) . . . . ?
C32 N2 C30 C29 -177.9(2) . . . . ?
C32 N2 C31 N1 177.8(2) . . . . ?
C32 C33 C34 C34 175.6(3) . . . 3_767 ?
C35 N3 C36 C37 20.8(5) . . . . ?
C35 N4 C37 C36 12.4(5) . . . . ?
C35 N4 C38 C39 81.3(8) . . . . ?
C35A N3 C36 C37 -22.3(5) . . . . ?
C35A N4A C37 C36 -12.3(6) . . . . ?
C35A N4A C38A C39A -92.5(12) . . . . ?
C36 N3 C35 N4 -12.0(6) . . . . ?
C36 N3 C35A N4A 13.5(6) . . . . ?
C37 N4 C35 N3 0.0(7) . . . . ?
C37 N4 C38 C39 -91.6(8) . . . . ?
C37 N4A C35A N3 -1.0(7) . . . . ?
C37 N4A C38A C39A 82.4(13) . . . . ?
C38 N4 C35 N3 -174.0(6) . . . . ?
C38 N4 C37 C36 -173.7(6) . . . . ?
C38 C39 C40 C40 129(2) . . . 3_657 ?
C38A N4A C35A N3 174.8(8) . . . . ?
C38A N4A C37 C36 172.0(8) . . . . ?
C38A C39A C40A C40A -3(3) . . . 3_657 ?

_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
- Detector area scaling
;
_oxdiff_exptl_absorpt_empirical_full_max 1.611
_oxdiff_exptl_absorpt_empirical_full_min 0.640
_vrf_PLAT360_cu_jnm130           
;
PROBLEM: Short  C(sp3)-C(sp3) Bond  C41      - C42      .       1.29 Ang.  
RESPONSE: The data for this crystal was collected at room temperature.
This C-C bond is part of highly disordered EtOH solvent. It was chosen to 
to restrain the atoms with DFIX and RIGU as opposed to using a solvent
 mask or squeeze.
;
_vrf_PLAT260_cu_jnm130           
;
PROBLEM: Large Average Ueq of Residue Including        O5      0.207 Check 
RESPONSE: This atom is part of a disordered EtOH mentioned above that has
been restrained using RIGU with small esd. It was found to be
optimal as opposed to constraining the molecule with EADP or using 
Squeeze.
;
_vrf_PLAT414_cu_jnm130           
;
PROBLEM: Short Intra D-H..H-X       H5B      ..H41B     .       1.99 Ang.  
RESPONSE: These H atoms were introduced in calculated positions 
on atoms from a disordered EtOH molecule.
;
# end Validation Reply Form
####################################################################### 
# 
# 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_jnm43
_database_code_depnum_ccdc_archive 'CCDC 2237930'
loop_
_audit_author_name
_audit_author_address
'Jennifer Murphy'
;University of Guelph
Canada
;
_audit_update_record             
;
2023-01-25 deposited with the CCDC.	2024-04-11 downloaded from the CCDC.
;
_audit_creation_date             2023-01-24
_audit_creation_method           
;
Olex2 1.5
(compiled 2022.04.07 svn.rca3783a0 for OlexSys, GUI svn.r6498)
;
_shelx_SHELXL_version_number     2018/3
_chemical_name_common            ?
_chemical_name_systematic        ?
_chemical_formula_moiety         'C39 H36 Cl4 Cu N6 O4'
_chemical_formula_sum            'C39 H36 Cl4 Cu N6 O4'
_chemical_formula_weight         858.08
_chemical_melting_point          ?
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0181 0.0091 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Cl Cl 0.3639 0.7018 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Cu Cu -1.9646 0.5888 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0311 0.0180 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0492 0.0322 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_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                   21.7971(5)
_cell_length_b                   8.3133(2)
_cell_length_c                   21.5270(6)
_cell_angle_alpha                90
_cell_angle_beta                 90.584(2)
_cell_angle_gamma                90
_cell_volume                     3900.62(17)
_cell_formula_units_Z            4
_cell_measurement_reflns_used    35660
_cell_measurement_temperature    170
_cell_measurement_theta_max      75.5000
_cell_measurement_theta_min      1.9070
_shelx_estimated_absorpt_T_max   ?
_shelx_estimated_absorpt_T_min   ?
_exptl_absorpt_coefficient_mu    3.714
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.56777
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
;
CrysAlisPro 1.171.40.53 (Rigaku Oxford Diffraction, 2019)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_absorpt_special_details   ?
_exptl_crystal_colour            'light violet'
_exptl_crystal_colour_modifier   light
_exptl_crystal_colour_primary    violet
_exptl_crystal_density_diffrn    1.461
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       prism
_exptl_crystal_F_000             1764
_exptl_crystal_size_max          0.3
_exptl_crystal_size_mid          0.2
_exptl_crystal_size_min          0.1
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.1367
_diffrn_reflns_av_unetI/netI     0.0338
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 1.000
_diffrn_reflns_limit_h_max       25
_diffrn_reflns_limit_h_min       -25
_diffrn_reflns_limit_k_max       9
_diffrn_reflns_limit_k_min       -9
_diffrn_reflns_limit_l_max       25
_diffrn_reflns_limit_l_min       -24
_diffrn_reflns_number            183242
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 1.000
_diffrn_reflns_theta_full        66.597
_diffrn_reflns_theta_max         66.596
_diffrn_reflns_theta_min         4.056
_diffrn_ambient_temperature      170.00
_diffrn_detector_area_resol_mean ?
_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    176.08 269.88   1.40   10.00    -- -105.12 -59.25 -59.92   67
  2  ω    176.08 269.88   1.40   10.00    -- -105.12 -59.25  20.08   67
  3  φ   -339.92  19.88   1.40   10.00 -57.79 -75.12 -59.25    --   257
  4  ω   -136.76 -27.56   1.40   10.00    -- -105.12  83.74 130.05   78
  5  ω    176.08 269.88   1.40   10.00    -- -105.12 -59.25  60.08   67
  6  ω    176.08 269.88   1.40   10.00    -- -105.12 -59.25 100.08   67
  7  ω    -26.23  70.37   1.40   10.00    --   50.69 -83.74-177.05   69
  8  ω    176.08 269.88   1.40   10.00    -- -105.12 -59.25 -19.92   67
  9  ω   -136.76 -27.56   1.40   10.00    -- -105.12  83.74  50.05   78
 10  ω      3.93  99.13   1.40   10.00    --   20.69  59.25  69.92   68
 11  ω   -136.76 -27.56   1.40   10.00    -- -105.12  83.74  10.05   78
 12  φ   -339.92  19.88   1.40   10.00 -87.79-105.12 -59.25    --   257
 13  ω    176.08 269.88   1.40   10.00    -- -105.12 -59.25 -99.92   67
 14  ω     33.93 127.73   1.40   10.00    --   50.69  59.25 132.92   67
 15  ω    176.08 269.88   1.40   10.00    -- -105.12 -59.25-139.92   67
 16  ω   -136.76 -27.56   1.40   10.00    -- -105.12  83.74  90.05   78
 17  ω    176.08 269.88   1.40   10.00    -- -105.12 -59.25-179.92   67
 18  ω    176.08 269.88   1.40   10.00    -- -105.12 -59.25 140.08   67
 19  ω   -136.76 -27.56   1.40   10.00    -- -105.12  83.74 -69.95   78
 20  ω   -136.76 -27.56   1.40   10.00    -- -105.12  83.74-149.95   78
 21  φ    -14.27 216.73   1.40   10.00 -25.56-105.12  31.50    --   165
 22  φ   -339.92  19.88   1.40   10.00 -72.79 -90.12 -59.25    --   257
 23  φ   -349.73   8.67   1.40   10.00 -96.36-105.12 -31.50    --   256
 24  ω     43.36 137.16   1.40   10.00    --   60.12  59.25 159.92   67
 25  ω     43.36 137.16   1.40   10.00    --   60.12  59.25  69.92   67
 26  ω   -136.76 -27.56   1.40   10.00    -- -105.12  83.74 170.05   78
 27  ω   -136.76 -27.56   1.40   10.00    -- -105.12  83.74 -29.95   78
 28  ω   -136.76 -27.56   1.40   10.00    -- -105.12  83.74-109.95   78
 29  ω    -26.23  70.37   1.40   10.00    --   50.69 -83.74 131.95   69
 30  ω     18.93 114.13   1.40   10.00    --   35.69  59.25  69.92   68
 31  ω    -26.23  70.37   1.40   10.00    --   50.69 -83.74-126.05   69
 32  ω     18.93 114.13   1.40   10.00    --   35.69  59.25 159.92   68
 33  ω    191.08 284.88   1.40   10.00    --  -90.12 -59.25 110.08   67
 34  ω    191.08 284.88   1.40   10.00    --  -90.12 -59.25  20.08   67
 35  ω      3.93  99.13   1.40   10.00    --   20.69  59.25 159.92   68
 36  ω    206.08 299.88   1.40   10.00    --  -75.12 -59.25 110.08   67
 37  ω    206.08 299.88   1.40   10.00    --  -75.12 -59.25  20.08   67
 38  ω     33.93 127.73   1.40   10.00    --   50.69  59.25-176.08   67
 39  ω    -26.23  70.37   1.40   10.00    --   50.69 -83.74  80.95   69
 40  φ    -20.08 339.72   1.40   10.00  33.24  50.69  59.25    --   257
 41  ω    191.08 284.88   1.40   10.00    --  -90.12 -59.25 -69.92   67
 42  ω    191.08 284.88   1.40   10.00    --  -90.12 -59.25-159.92   67
 43  ω     33.93 127.73   1.40   10.00    --   50.69  59.25  81.92   67
 44  φ    -10.27 348.13   1.40   10.00  42.06  50.69  31.50    --   256
 45  ω    -26.23  70.37   1.40   10.00    --   50.69 -83.74 -75.05   69
 46  φ    -10.27 348.13   1.40   10.00  42.06  50.69  31.50    --   256
;
_diffrn_measurement_device       'abstract diffractometer'
_diffrn_measurement_device_type  
'Saxi-CrysAlisPro-abstract goniometer imported SAXI images'
_diffrn_measurement_method       'ω and φ scans'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_source                   ?
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                5683
_reflns_number_total             6885
_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
;
_reflns_threshold_expression     'I > 2σ(I)'
_computing_cell_refinement       'CrysAlisPro 1.171.40.53 (Rigaku OD, 2019)'
_computing_data_collection       'CrysAlisPro 1.171.40.53 (Rigaku OD, 2019)'
_computing_data_reduction        'CrysAlisPro 1.171.40.53 (Rigaku OD, 2019)'
_computing_molecular_graphics    'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2018/3 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT 2014/5 (Sheldrick, 2014)'
_refine_diff_density_max         0.959
_refine_diff_density_min         -0.658
_refine_diff_density_rms         0.086
_refine_ls_extinction_coef       0.00052(10)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4^
_refine_ls_extinction_method     'SHELXL-2018/3 (Sheldrick 2018)'
_refine_ls_goodness_of_fit_ref   1.080
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     489
_refine_ls_number_reflns         6885
_refine_ls_number_restraints     1
_refine_ls_R_factor_all          0.0717
_refine_ls_R_factor_gt           0.0608
_refine_ls_restrained_S_all      1.080
_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)+(0.1008P)²+3.1883P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1626
_refine_ls_wR_factor_ref         0.1750
_refine_special_details          ?
_olex2_refinement_description    
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups, All N(H) groups
2. Restrained distances
 H6-N6 \\sim H5-N5
 with sigma of 0.02
3. Uiso/Uaniso restraints and constraints
Uanis(O3) = Uanis(O4)
4.a Riding coordinates:
 N5(H5)
4.b Secondary CH2 refined with riding coordinates:
 C13(H13A,H13B), C18(H18A,H18B), C19(H19A,H19B), C20(H20A,H20B), C21(H21A,
 H21B), C22(H22A,H22B), C27(H27A,H27B)
4.c Aromatic/amide H refined with riding coordinates:
 C2(H2), C3(H3), C4(H4), C8(H8), C9(H9), C10(H10), C11(H11), C15(H15),
 C16(H16), C17(H17), C23(H23), C24(H24), C25(H25), C29(H29), C30(H30), C31(H31),
  C32(H32), C36(H36), C37(H37), C38(H38)
;
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     dual
_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
Cu1 Cu 0.000000 0.500000 0.500000 0.02732(19) Uani 1 2 d S . P . .
Cu2 Cu 0.500000 0.500000 0.500000 0.0393(2) Uani 1 2 d S . P . .
Cl1 Cl 0.02861(5) 0.14107(13) 0.38032(4) 0.0634(3) Uani 1 1 d . . . . .
Cl2 Cl 0.15316(4) 0.41686(12) 0.19316(4) 0.0530(3) Uani 1 1 d . . . . .
Cl3 Cl 0.68349(6) 0.48869(12) 0.46447(5) 0.0612(3) Uani 1 1 d . . . . .
Cl4 Cl 0.68794(8) 0.44325(17) 0.21509(6) 0.0894(5) Uani 1 1 d . . . . .
O1 O 0.04730(10) 0.5560(3) 0.42581(10) 0.0342(5) Uani 1 1 d . . . . .
O2 O 0.10579(11) 0.7083(3) 0.48782(11) 0.0425(5) Uani 1 1 d . . . . .
O3 O 0.52939(12) 0.5324(3) 0.41569(14) 0.0534(5) Uani 1 1 d . . . . .
O4 O 0.44004(11) 0.6590(3) 0.40281(13) 0.0534(5) Uani 1 1 d . . . . .
N1 N 0.05659(11) 0.3233(3) 0.51771(12) 0.0315(6) Uani 1 1 d . . . . .
N2 N 0.14133(12) 0.1824(3) 0.52417(14) 0.0422(7) Uani 1 1 d . . . . .
N3 N 0.42466(12) 0.0472(3) 0.48240(16) 0.0449(7) Uani 1 1 d . . . . .
N4 N 0.46585(12) 0.2876(4) 0.47497(14) 0.0441(7) Uani 1 1 d . . . . .
N5 N 0.10735(11) 0.3921(3) 0.32385(12) 0.0332(6) Uani 1 1 d D . . . .
H5 H 0.073966 0.398057 0.348912 0.040 Uiso 1 1 d DR U . . .
N6 N 0.63283(15) 0.5305(4) 0.33596(15) 0.0459(7) Uani 1 1 d D . . . .
C1 C 0.10914(15) 0.2608(4) 0.22217(15) 0.0402(7) Uani 1 1 d . . . . .
C2 C 0.09106(17) 0.1391(5) 0.18235(18) 0.0511(9) Uani 1 1 d . . . . .
H2 H 0.104721 0.138032 0.140590 0.061 Uiso 1 1 calc R U . . .
C3 C 0.05258(19) 0.0180(5) 0.2040(2) 0.0545(10) Uani 1 1 d . . . . .
H3 H 0.039498 -0.065448 0.176733 0.065 Uiso 1 1 calc R U . . .
C4 C 0.03359(19) 0.0192(5) 0.26452(19) 0.0509(9) Uani 1 1 d . . . . .
H4 H 0.007433 -0.063430 0.279375 0.061 Uiso 1 1 calc R U . . .
C5 C 0.05264(16) 0.1407(4) 0.30368(15) 0.0406(8) Uani 1 1 d . . . . .
C6 C 0.09150(13) 0.2653(4) 0.28453(14) 0.0336(7) Uani 1 1 d . . . . .
C7 C 0.16838(14) 0.4304(4) 0.34001(13) 0.0323(7) Uani 1 1 d . . . . .
C8 C 0.21647(15) 0.3248(4) 0.32943(15) 0.0388(7) Uani 1 1 d . . . . .
H8 H 0.208491 0.222607 0.311327 0.047 Uiso 1 1 calc R U . . .
C9 C 0.27585(16) 0.3676(5) 0.34508(16) 0.0469(9) Uani 1 1 d . . . . .
H9 H 0.308551 0.295541 0.336639 0.056 Uiso 1 1 calc R U . . .
C10 C 0.28816(17) 0.5130(5) 0.37269(18) 0.0531(10) Uani 1 1 d . . . . .
H10 H 0.329079 0.541758 0.383490 0.064 Uiso 1 1 calc R U . . .
C11 C 0.23998(15) 0.6175(5) 0.38465(16) 0.0464(9) Uani 1 1 d . . . . .
H11 H 0.248249 0.717004 0.404738 0.056 Uiso 1 1 calc R U . . .
C12 C 0.17992(14) 0.5797(4) 0.36787(14) 0.0348(7) Uani 1 1 d . . . . .
C13 C 0.12886(15) 0.6989(4) 0.37846(15) 0.0377(7) Uani 1 1 d . . . . .
H13A H 0.101359 0.701010 0.341589 0.045 Uiso 1 1 calc R U . . .
H13B H 0.146515 0.807832 0.383828 0.045 Uiso 1 1 calc R U . . .
C14 C 0.09176(14) 0.6551(3) 0.43590(15) 0.0343(7) Uani 1 1 d . . . . .
C15 C 0.11701(14) 0.3263(4) 0.51106(16) 0.0384(7) Uani 1 1 d . . . . .
H15 H 0.139853 0.418011 0.498699 0.046 Uiso 1 1 calc R U . . .
C16 C 0.04241(14) 0.1686(4) 0.53557(15) 0.0342(7) Uani 1 1 d . . . . .
H16 H 0.002363 0.130547 0.544497 0.041 Uiso 1 1 calc R U . . .
C17 C 0.09418(15) 0.0794(4) 0.53843(16) 0.0386(7) Uani 1 1 d . . . . .
H17 H 0.097339 -0.031697 0.548284 0.046 Uiso 1 1 calc R U . . .
C18 C 0.20727(15) 0.1454(4) 0.52327(19) 0.0470(9) Uani 1 1 d . . . . .
H18A H 0.219301 0.092192 0.562691 0.056 Uiso 1 1 calc R U . . .
H18B H 0.230898 0.246720 0.519917 0.056 Uiso 1 1 calc R U . . .
C19 C 0.22238(16) 0.0387(5) 0.47025(18) 0.0466(8) Uani 1 1 d . . . . .
H19A H 0.204169 0.083262 0.431612 0.056 Uiso 1 1 calc R U . . .
H19B H 0.204269 -0.068967 0.477225 0.056 Uiso 1 1 calc R U . . .
C20 C 0.29230(16) 0.0220(5) 0.46252(18) 0.0461(9) Uani 1 1 d . . . . .
H20A H 0.300559 -0.052073 0.427585 0.055 Uiso 1 1 calc R U . . .
H20B H 0.309649 0.128372 0.451785 0.055 Uiso 1 1 calc R U . . .
C21 C 0.32400(15) -0.0400(4) 0.51983(19) 0.0457(9) Uani 1 1 d . . . . .
H21A H 0.301148 -0.134429 0.535416 0.055 Uiso 1 1 calc R U . . .
H21B H 0.322745 0.044185 0.552316 0.055 Uiso 1 1 calc R U . . .
C22 C 0.39085(16) -0.0887(4) 0.5096(2) 0.0512(9) Uani 1 1 d . . . . .
H22A H 0.410050 -0.119869 0.549659 0.061 Uiso 1 1 calc R U . . .
H22B H 0.392506 -0.182464 0.481269 0.061 Uiso 1 1 calc R U . . .
C23 C 0.43964(14) 0.1812(4) 0.51255(18) 0.0434(8) Uani 1 1 d . . . . .
H23 H 0.432559 0.198837 0.555486 0.052 Uiso 1 1 calc R U . . .
C24 C 0.44159(17) 0.0651(5) 0.4222(2) 0.0538(10) Uani 1 1 d . . . . .
H24 H 0.436907 -0.011259 0.389659 0.065 Uiso 1 1 calc R U . . .
C25 C 0.46650(17) 0.2141(5) 0.41798(19) 0.0523(9) Uani 1 1 d . . . . .
H25 H 0.482086 0.260569 0.381045 0.063 Uiso 1 1 calc R U . . .
C26 C 0.49036(17) 0.6140(5) 0.38280(19) 0.0486(9) Uani 1 1 d . . . . .
C27 C 0.51107(19) 0.6560(6) 0.31829(19) 0.0591(10) Uani 1 1 d . . . . .
H27A H 0.477075 0.711458 0.296225 0.071 Uiso 1 1 calc R U . . .
H27B H 0.519721 0.555141 0.295543 0.071 Uiso 1 1 calc R U . . .
C28 C 0.56757(18) 0.7621(5) 0.31637(17) 0.0502(9) Uani 1 1 d . . . . .
C29 C 0.5622(2) 0.9273(6) 0.3064(2) 0.0612(11) Uani 1 1 d . . . . .
H29 H 0.522429 0.973474 0.303075 0.073 Uiso 1 1 calc R U . . .
C30 C 0.6130(2) 1.0263(5) 0.3013(2) 0.0631(12) Uani 1 1 d . . . . .
H30 H 0.608088 1.138604 0.294749 0.076 Uiso 1 1 calc R U . . .
C31 C 0.6707(2) 0.9604(5) 0.30579(19) 0.0558(10) Uani 1 1 d . . . . .
H31 H 0.705761 1.027107 0.301552 0.067 Uiso 1 1 calc R U . . .
C32 C 0.67801(18) 0.7960(4) 0.31655(17) 0.0482(9) Uani 1 1 d . . . . .
H32 H 0.718054 0.751387 0.319458 0.058 Uiso 1 1 calc R U . . .
C33 C 0.62687(16) 0.6970(4) 0.32304(15) 0.0432(8) Uani 1 1 d . . . . .
C34 C 0.69113(18) 0.4614(4) 0.34024(18) 0.0469(9) Uani 1 1 d . . . . .
C35 C 0.7229(2) 0.4126(5) 0.2869(2) 0.0581(11) Uani 1 1 d . . . . .
C36 C 0.7797(2) 0.3432(5) 0.2900(3) 0.0768(15) Uani 1 1 d . . . . .
H36 H 0.800033 0.313601 0.252945 0.092 Uiso 1 1 calc R U . . .
C37 C 0.8072(2) 0.3164(5) 0.3465(3) 0.0794(16) Uani 1 1 d . . . . .
H37 H 0.846644 0.267723 0.348417 0.095 Uiso 1 1 calc R U . . .
C38 C 0.7782(2) 0.3595(5) 0.4009(3) 0.0667(12) Uani 1 1 d . . . . .
H38 H 0.797276 0.340252 0.440057 0.080 Uiso 1 1 calc R U . . .
C39 C 0.72073(18) 0.4314(4) 0.39727(19) 0.0494(9) Uani 1 1 d . . . . .
H6 H 0.6076(19) 0.498(5) 0.3657(17) 0.070(15) Uiso 1 1 d 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
Cu1 O1 1.966(2) . ?
Cu1 O1 1.965(2) 3_566 ?
Cu1 N1 1.953(2) . ?
Cu1 N1 1.953(2) 3_566 ?
Cu2 O3 1.949(3) . ?
Cu2 O3 1.949(3) 3_666 ?
Cu2 N4 1.989(3) 3_666 ?
Cu2 N4 1.989(3) . ?
Cl1 C5 1.736(3) . ?
Cl2 C1 1.734(4) . ?
Cl3 C39 1.733(4) . ?
Cl4 C35 1.735(5) . ?
O1 C14 1.289(4) . ?
O2 C14 1.237(4) . ?
O3 C26 1.294(5) . ?
O4 C26 1.240(5) . ?
N1 C15 1.326(4) . ?
N1 C16 1.378(4) . ?
N2 C15 1.338(4) . ?
N2 C17 1.375(4) . ?
N2 C18 1.470(4) . ?
N3 C22 1.473(4) . ?
N3 C23 1.329(5) . ?
N3 C24 1.359(5) . ?
N4 C23 1.331(5) . ?
N4 C25 1.371(5) . ?
N5 H5 0.9115 . ?
N5 C6 1.393(4) . ?
N5 C7 1.408(4) . ?
N6 C33 1.418(5) . ?
N6 C34 1.397(5) . ?
N6 H6 0.889(19) . ?
C1 C2 1.381(5) . ?
C1 C6 1.401(4) . ?
C2 H2 0.9500 . ?
C2 C3 1.393(6) . ?
C3 H3 0.9500 . ?
C3 C4 1.372(6) . ?
C4 H4 0.9500 . ?
C4 C5 1.377(5) . ?
C5 C6 1.403(4) . ?
C7 C8 1.388(5) . ?
C7 C12 1.400(5) . ?
C8 H8 0.9500 . ?
C8 C9 1.381(5) . ?
C9 H9 0.9500 . ?
C9 C10 1.372(5) . ?
C10 H10 0.9500 . ?
C10 C11 1.389(5) . ?
C11 H11 0.9500 . ?
C11 C12 1.390(5) . ?
C12 C13 1.509(4) . ?
C13 H13A 0.9900 . ?
C13 H13B 0.9900 . ?
C13 C14 1.528(4) . ?
C15 H15 0.9500 . ?
C16 H16 0.9500 . ?
C16 C17 1.351(4) . ?
C17 H17 0.9500 . ?
C18 H18A 0.9900 . ?
C18 H18B 0.9900 . ?
C18 C19 1.486(5) . ?
C19 H19A 0.9900 . ?
C19 H19B 0.9900 . ?
C19 C20 1.541(5) . ?
C20 H20A 0.9900 . ?
C20 H20B 0.9900 . ?
C20 C21 1.499(5) . ?
C21 H21A 0.9900 . ?
C21 H21B 0.9900 . ?
C21 C22 1.531(5) . ?
C22 H22A 0.9900 . ?
C22 H22B 0.9900 . ?
C23 H23 0.9500 . ?
C24 H24 0.9500 . ?
C24 C25 1.356(5) . ?
C25 H25 0.9500 . ?
C26 C27 1.506(6) . ?
C27 H27A 0.9900 . ?
C27 H27B 0.9900 . ?
C27 C28 1.516(5) . ?
C28 C29 1.395(6) . ?
C28 C33 1.407(5) . ?
C29 H29 0.9500 . ?
C29 C30 1.386(6) . ?
C30 H30 0.9500 . ?
C30 C31 1.373(6) . ?
C31 H31 0.9500 . ?
C31 C32 1.395(5) . ?
C32 H32 0.9500 . ?
C32 C33 1.394(5) . ?
C34 C35 1.406(5) . ?
C34 C39 1.403(6) . ?
C35 C36 1.367(7) . ?
C36 H36 0.9500 . ?
C36 C37 1.370(8) . ?
C37 H37 0.9500 . ?
C37 C38 1.383(8) . ?
C38 H38 0.9500 . ?
C38 C39 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
O1 Cu1 O1 180.0 3_566 . ?
N1 Cu1 O1 89.93(10) 3_566 . ?
N1 Cu1 O1 90.07(10) 3_566 3_566 ?
N1 Cu1 O1 89.93(10) . 3_566 ?
N1 Cu1 O1 90.07(10) . . ?
N1 Cu1 N1 180.0 3_566 . ?
O3 Cu2 O3 180.0 . 3_666 ?
O3 Cu2 N4 89.77(12) . . ?
O3 Cu2 N4 89.77(12) 3_666 3_666 ?
O3 Cu2 N4 90.23(12) . 3_666 ?
O3 Cu2 N4 90.23(12) 3_666 . ?
N4 Cu2 N4 180.00(7) 3_666 . ?
C14 O1 Cu1 114.5(2) . . ?
C26 O3 Cu2 111.2(2) . . ?
C15 N1 Cu1 126.2(2) . . ?
C15 N1 C16 105.9(3) . . ?
C16 N1 Cu1 127.8(2) . . ?
C15 N2 C17 108.0(3) . . ?
C15 N2 C18 124.7(3) . . ?
C17 N2 C18 127.3(3) . . ?
C23 N3 C22 124.8(3) . . ?
C23 N3 C24 107.8(3) . . ?
C24 N3 C22 127.2(3) . . ?
C23 N4 Cu2 125.9(3) . . ?
C23 N4 C25 104.8(3) . . ?
C25 N4 Cu2 129.1(2) . . ?
C6 N5 H5 101.9 . . ?
C6 N5 C7 123.3(3) . . ?
C7 N5 H5 126.8 . . ?
C33 N6 H6 112(3) . . ?
C34 N6 C33 119.7(3) . . ?
C34 N6 H6 113(3) . . ?
C2 C1 Cl2 118.7(3) . . ?
C2 C1 C6 122.4(3) . . ?
C6 C1 Cl2 118.9(3) . . ?
C1 C2 H2 120.3 . . ?
C1 C2 C3 119.4(4) . . ?
C3 C2 H2 120.3 . . ?
C2 C3 H3 120.0 . . ?
C4 C3 C2 120.0(3) . . ?
C4 C3 H3 120.0 . . ?
C3 C4 H4 120.2 . . ?
C3 C4 C5 119.7(4) . . ?
C5 C4 H4 120.2 . . ?
C4 C5 Cl1 119.4(3) . . ?
C4 C5 C6 122.8(3) . . ?
C6 C5 Cl1 117.8(3) . . ?
N5 C6 C1 122.3(3) . . ?
N5 C6 C5 121.8(3) . . ?
C1 C6 C5 115.7(3) . . ?
C8 C7 N5 121.9(3) . . ?
C8 C7 C12 119.9(3) . . ?
C12 C7 N5 118.1(3) . . ?
C7 C8 H8 119.9 . . ?
C9 C8 C7 120.3(3) . . ?
C9 C8 H8 119.9 . . ?
C8 C9 H9 119.6 . . ?
C10 C9 C8 120.8(3) . . ?
C10 C9 H9 119.6 . . ?
C9 C10 H10 120.5 . . ?
C9 C10 C11 119.1(3) . . ?
C11 C10 H10 120.5 . . ?
C10 C11 H11 119.3 . . ?
C10 C11 C12 121.5(3) . . ?
C12 C11 H11 119.3 . . ?
C7 C12 C13 121.2(3) . . ?
C11 C12 C7 118.4(3) . . ?
C11 C12 C13 120.4(3) . . ?
C12 C13 H13A 109.4 . . ?
C12 C13 H13B 109.4 . . ?
C12 C13 C14 111.3(3) . . ?
H13A C13 H13B 108.0 . . ?
C14 C13 H13A 109.4 . . ?
C14 C13 H13B 109.4 . . ?
O1 C14 C13 114.8(3) . . ?
O2 C14 O1 124.0(3) . . ?
O2 C14 C13 121.2(3) . . ?
N1 C15 N2 110.6(3) . . ?
N1 C15 H15 124.7 . . ?
N2 C15 H15 124.7 . . ?
N1 C16 H16 125.2 . . ?
C17 C16 N1 109.6(3) . . ?
C17 C16 H16 125.2 . . ?
N2 C17 H17 127.1 . . ?
C16 C17 N2 105.9(3) . . ?
C16 C17 H17 127.1 . . ?
N2 C18 H18A 109.4 . . ?
N2 C18 H18B 109.4 . . ?
N2 C18 C19 111.1(3) . . ?
H18A C18 H18B 108.0 . . ?
C19 C18 H18A 109.4 . . ?
C19 C18 H18B 109.4 . . ?
C18 C19 H19A 109.4 . . ?
C18 C19 H19B 109.4 . . ?
C18 C19 C20 111.3(3) . . ?
H19A C19 H19B 108.0 . . ?
C20 C19 H19A 109.4 . . ?
C20 C19 H19B 109.4 . . ?
C19 C20 H20A 109.0 . . ?
C19 C20 H20B 109.0 . . ?
H20A C20 H20B 107.8 . . ?
C21 C20 C19 113.0(3) . . ?
C21 C20 H20A 109.0 . . ?
C21 C20 H20B 109.0 . . ?
C20 C21 H21A 108.8 . . ?
C20 C21 H21B 108.8 . . ?
C20 C21 C22 113.8(3) . . ?
H21A C21 H21B 107.7 . . ?
C22 C21 H21A 108.8 . . ?
C22 C21 H21B 108.8 . . ?
N3 C22 C21 109.6(3) . . ?
N3 C22 H22A 109.7 . . ?
N3 C22 H22B 109.7 . . ?
C21 C22 H22A 109.7 . . ?
C21 C22 H22B 109.7 . . ?
H22A C22 H22B 108.2 . . ?
N3 C23 N4 111.4(3) . . ?
N3 C23 H23 124.3 . . ?
N4 C23 H23 124.3 . . ?
N3 C24 H24 127.0 . . ?
C25 C24 N3 106.1(3) . . ?
C25 C24 H24 127.0 . . ?
N4 C25 H25 125.1 . . ?
C24 C25 N4 109.8(4) . . ?
C24 C25 H25 125.1 . . ?
O3 C26 C27 115.1(3) . . ?
O4 C26 O3 123.2(4) . . ?
O4 C26 C27 121.7(4) . . ?
C26 C27 H27A 108.7 . . ?
C26 C27 H27B 108.7 . . ?
C26 C27 C28 114.3(3) . . ?
H27A C27 H27B 107.6 . . ?
C28 C27 H27A 108.7 . . ?
C28 C27 H27B 108.7 . . ?
C29 C28 C27 120.7(4) . . ?
C29 C28 C33 118.0(4) . . ?
C33 C28 C27 121.3(4) . . ?
C28 C29 H29 119.0 . . ?
C30 C29 C28 122.1(4) . . ?
C30 C29 H29 119.0 . . ?
C29 C30 H30 120.4 . . ?
C31 C30 C29 119.3(4) . . ?
C31 C30 H30 120.4 . . ?
C30 C31 H31 119.8 . . ?
C30 C31 C32 120.4(4) . . ?
C32 C31 H31 119.8 . . ?
C31 C32 H32 119.8 . . ?
C33 C32 C31 120.3(4) . . ?
C33 C32 H32 119.8 . . ?
C28 C33 N6 118.5(3) . . ?
C32 C33 N6 121.6(3) . . ?
C32 C33 C28 119.8(3) . . ?
N6 C34 C35 121.3(4) . . ?
N6 C34 C39 122.7(3) . . ?
C39 C34 C35 116.0(4) . . ?
C34 C35 Cl4 118.1(3) . . ?
C36 C35 Cl4 119.7(4) . . ?
C36 C35 C34 122.3(5) . . ?
C35 C36 H36 119.9 . . ?
C35 C36 C37 120.1(5) . . ?
C37 C36 H36 119.9 . . ?
C36 C37 H37 119.7 . . ?
C36 C37 C38 120.6(4) . . ?
C38 C37 H37 119.7 . . ?
C37 C38 H38 120.5 . . ?
C37 C38 C39 119.0(5) . . ?
C39 C38 H38 120.5 . . ?
C34 C39 Cl3 117.8(3) . . ?
C38 C39 Cl3 120.1(4) . . ?
C38 C39 C34 122.1(4) . . ?

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
Cu1 O1 C14 O2 2.3(4) . . . . ?
Cu1 O1 C14 C13 179.85(19) . . . . ?
Cu1 N1 C15 N2 -176.7(2) . . . . ?
Cu1 N1 C16 C17 175.1(2) . . . . ?
Cu2 O3 C26 O4 -2.6(4) . . . . ?
Cu2 O3 C26 C27 175.6(3) . . . . ?
Cu2 N4 C23 N3 -176.5(2) . . . . ?
Cu2 N4 C25 C24 176.0(3) . . . . ?
Cl1 C5 C6 N5 -4.4(4) . . . . ?
Cl1 C5 C6 C1 -179.4(2) . . . . ?
Cl2 C1 C2 C3 -176.1(3) . . . . ?
Cl2 C1 C6 N5 0.9(4) . . . . ?
Cl2 C1 C6 C5 176.0(2) . . . . ?
Cl4 C35 C36 C37 -179.0(3) . . . . ?
O3 C26 C27 C28 -62.2(5) . . . . ?
O4 C26 C27 C28 116.0(4) . . . . ?
N1 C16 C17 N2 2.1(4) . . . . ?
N2 C18 C19 C20 170.6(3) . . . . ?
N3 C24 C25 N4 0.7(4) . . . . ?
N5 C7 C8 C9 179.1(3) . . . . ?
N5 C7 C12 C11 179.2(3) . . . . ?
N5 C7 C12 C13 -2.0(4) . . . . ?
N6 C34 C35 Cl4 0.9(5) . . . . ?
N6 C34 C35 C36 -179.3(4) . . . . ?
N6 C34 C39 Cl3 -1.8(5) . . . . ?
N6 C34 C39 C38 178.6(3) . . . . ?
C1 C2 C3 C4 -0.8(6) . . . . ?
C2 C1 C6 N5 -176.9(3) . . . . ?
C2 C1 C6 C5 -1.8(5) . . . . ?
C2 C3 C4 C5 0.1(6) . . . . ?
C3 C4 C5 Cl1 -179.8(3) . . . . ?
C3 C4 C5 C6 -0.4(6) . . . . ?
C4 C5 C6 N5 176.2(3) . . . . ?
C4 C5 C6 C1 1.2(5) . . . . ?
C6 N5 C7 C8 -14.6(5) . . . . ?
C6 N5 C7 C12 165.7(3) . . . . ?
C6 C1 C2 C3 1.7(5) . . . . ?
C7 N5 C6 C1 -63.2(4) . . . . ?
C7 N5 C6 C5 122.1(3) . . . . ?
C7 C8 C9 C10 1.6(5) . . . . ?
C7 C12 C13 C14 79.4(4) . . . . ?
C8 C7 C12 C11 -0.4(5) . . . . ?
C8 C7 C12 C13 178.4(3) . . . . ?
C8 C9 C10 C11 -0.2(6) . . . . ?
C9 C10 C11 C12 -1.6(6) . . . . ?
C10 C11 C12 C7 1.9(5) . . . . ?
C10 C11 C12 C13 -176.9(3) . . . . ?
C11 C12 C13 C14 -101.8(3) . . . . ?
C12 C7 C8 C9 -1.3(5) . . . . ?
C12 C13 C14 O1 -87.1(3) . . . . ?
C12 C13 C14 O2 90.5(3) . . . . ?
C15 N1 C16 C17 -1.1(4) . . . . ?
C15 N2 C17 C16 -2.3(4) . . . . ?
C15 N2 C18 C19 -109.7(4) . . . . ?
C16 N1 C15 N2 -0.4(4) . . . . ?
C17 N2 C15 N1 1.7(4) . . . . ?
C17 N2 C18 C19 70.6(5) . . . . ?
C18 N2 C15 N1 -178.1(3) . . . . ?
C18 N2 C17 C16 177.5(3) . . . . ?
C18 C19 C20 C21 57.2(4) . . . . ?
C19 C20 C21 C22 168.6(3) . . . . ?
C20 C21 C22 N3 54.8(4) . . . . ?
C22 N3 C23 N4 -175.2(3) . . . . ?
C22 N3 C24 C25 174.6(3) . . . . ?
C23 N3 C22 C21 70.8(5) . . . . ?
C23 N3 C24 C25 -0.4(4) . . . . ?
C23 N4 C25 C24 -0.7(4) . . . . ?
C24 N3 C22 C21 -103.4(4) . . . . ?
C24 N3 C23 N4 0.0(4) . . . . ?
C25 N4 C23 N3 0.5(4) . . . . ?
C26 C27 C28 C29 -99.9(5) . . . . ?
C26 C27 C28 C33 81.7(5) . . . . ?
C27 C28 C29 C30 -176.7(4) . . . . ?
C27 C28 C33 N6 -4.3(5) . . . . ?
C27 C28 C33 C32 175.3(3) . . . . ?
C28 C29 C30 C31 0.3(7) . . . . ?
C29 C28 C33 N6 177.2(3) . . . . ?
C29 C28 C33 C32 -3.2(5) . . . . ?
C29 C30 C31 C32 -1.2(7) . . . . ?
C30 C31 C32 C33 -0.2(6) . . . . ?
C31 C32 C33 N6 -178.0(3) . . . . ?
C31 C32 C33 C28 2.4(5) . . . . ?
C33 N6 C34 C35 -82.9(5) . . . . ?
C33 N6 C34 C39 99.2(4) . . . . ?
C33 C28 C29 C30 1.9(6) . . . . ?
C34 N6 C33 C28 177.3(3) . . . . ?
C34 N6 C33 C32 -2.3(5) . . . . ?
C34 C35 C36 C37 1.1(7) . . . . ?
C35 C34 C39 Cl3 -179.8(3) . . . . ?
C35 C34 C39 C38 0.7(5) . . . . ?
C35 C36 C37 C38 -0.3(7) . . . . ?
C36 C37 C38 C39 -0.4(6) . . . . ?
C37 C38 C39 Cl3 -179.4(3) . . . . ?
C37 C38 C39 C34 0.2(6) . . . . ?
C39 C34 C35 Cl4 178.9(3) . . . . ?
C39 C34 C35 C36 -1.3(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
- Detector area scaling
;
_vrf_PLAT978_jnm43               
;
PROBLEM: Number C-C Bonds with Positive Residual Density.          0 Info  
RESPONSE: No problem here! This is where we would like to see the
calculated residual electron density at the "end" of a refinement.
;
# start Validation Reply Form
_vrf_RINTA01_jnm43               
;
PROBLEM: The value of Rint is greater than 0.12
RESPONSE: These were low quality crystals that did not result in
super satisfactory results despite many attempts to grow better crystals.
;
####################################################################### 
# 
# 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_mo_jlk052_0m
_database_code_depnum_ccdc_archive 'CCDC 2237934'
loop_
_audit_author_name
_audit_author_address
'Jennifer Murphy'
;University of Guelph
Canada
;
_audit_update_record             
;
2023-01-25 deposited with the CCDC.	2024-04-11 downloaded from the CCDC.
;
_audit_creation_date             2023-01-09
_audit_creation_method           
;
Olex2 1.5
(compiled 2022.04.07 svn.rca3783a0 for OlexSys, GUI svn.r6498)
;
_shelx_SHELXL_version_number     2018/3
_chemical_name_common            ?
_chemical_name_systematic        ?
_chemical_formula_moiety         'C42 H46 Cl4 Mn N6 O6'
_chemical_formula_sum            'C42 H46 Cl4 Mn N6 O6'
_chemical_formula_weight         927.59
_chemical_melting_point          ?
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'
Mn Mn 0.3368 0.7283 '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'

_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/n 1'
_space_group_name_Hall           '-P 2yn'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x+1/2, y+1/2, -z+1/2'
'-x, -y, -z'
'x-1/2, -y-1/2, z-1/2'

_cell_length_a                   8.5133(2)
_cell_length_b                   20.8959(7)
_cell_length_c                   12.8879(4)
_cell_angle_alpha                90
_cell_angle_beta                 107.4090(10)
_cell_angle_gamma                90
_cell_volume                     2187.65(11)
_cell_formula_units_Z            2
_cell_measurement_reflns_used    9623
_cell_measurement_temperature    170.0(1)
_cell_measurement_theta_max      28.29
_cell_measurement_theta_min      2.56
_shelx_estimated_absorpt_T_max   0.920
_shelx_estimated_absorpt_T_min   0.832
_exptl_absorpt_coefficient_mu    0.599
_exptl_absorpt_correction_T_max  0.7457
_exptl_absorpt_correction_T_min  0.7083
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
;
SADABS-2016/2 (Bruker,2016/2) was used for absorption correction.
wR2(int) was 0.0568 before and 0.0529 after correction.
The Ratio of minimum to maximum transmission is 0.9498.
The λ/2 correction factor is Not present.
;
_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    1.408
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       block
_exptl_crystal_F_000             962
_exptl_crystal_recrystallization_method 
'Crystallized in 1 day by slow evaporation at room temperature.'
_exptl_crystal_size_max          0.319
_exptl_crystal_size_mid          0.282
_exptl_crystal_size_min          0.142
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0417
_diffrn_reflns_av_unetI/netI     0.0120
_diffrn_reflns_Laue_measured_fraction_full 0.992
_diffrn_reflns_Laue_measured_fraction_max 0.991
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       27
_diffrn_reflns_limit_k_min       -27
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            137306
_diffrn_reflns_point_group_measured_fraction_full 0.992
_diffrn_reflns_point_group_measured_fraction_max 0.991
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         28.356
_diffrn_reflns_theta_min         3.177
_diffrn_ambient_temperature      170.00(10)
_diffrn_detector_area_resol_mean ?
_diffrn_measured_fraction_theta_full 0.992
_diffrn_measured_fraction_theta_max 0.991
_diffrn_measurement_device_type  'Bruker D8 Venture'
_diffrn_measurement_method       'φ and ω scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_source                   ?
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                4810
_reflns_number_total             5427
_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       'SAINT V8.40B (?, 2016)'
_computing_data_collection       ?
_computing_data_reduction        'SAINT V8.40B (?, 2016)'
_computing_molecular_graphics    'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2018/3 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT 2018/2 (Sheldrick, 2018)'
_refine_diff_density_max         0.390
_refine_diff_density_min         -0.334
_refine_diff_density_rms         0.061
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.075
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     276
_refine_ls_number_reflns         5427
_refine_ls_number_restraints     3
_refine_ls_R_factor_all          0.0369
_refine_ls_R_factor_gt           0.0311
_refine_ls_restrained_S_all      1.080
_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)+(0.0391P)²+1.0256P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0802
_refine_ls_wR_factor_ref         0.0852
_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, All O(H) groups
2. Restrained distances
 O3-H3
 0.87 with sigma of 0.01
 Mn1-H3
 2.758822 with sigma of 0.02
 C15-H3
 1.8802 with sigma of 0.02
3.a Secondary CH2 refined with riding coordinates:
 C13(H13A,H13B), C19(H19A,H19B), C20(H20A,H20B), C21(H21A,H21B)
3.b Aromatic/amide H refined with riding coordinates:
 C3(H3A), C4(H4), C5(H5), C9(H9), C10(H10), C11(H11), C12(H12), C16(H16),
 C17(H17), C18(H18)
3.c Idealised Me refined as rotating group:
 C15(H15A,H15B,H15C)
;
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     dual
_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
Mn1 Mn 0.500000 0.500000 0.500000 0.02318(8) Uani 1 2 d DS . P . .
Cl1 Cl 0.45214(6) 0.35104(2) -0.16389(3) 0.04417(11) Uani 1 1 d . . . . .
Cl2 Cl 0.32452(5) 0.26589(2) 0.19948(3) 0.03551(9) Uani 1 1 d . . . . .
O1 O 0.42504(13) 0.41931(5) 0.26096(8) 0.0319(2) Uani 1 1 d . . . . .
O2 O 0.58669(13) 0.49570(5) 0.35873(8) 0.0286(2) Uani 1 1 d . . . . .
O3 O 0.61052(14) 0.59669(5) 0.54545(9) 0.0339(2) Uani 1 1 d D . . . .
H3 H 0.623(2) 0.6014(8) 0.6160(8) 0.051 Uiso 1 1 d D U . . .
N1 N 0.46343(13) 0.35842(5) 0.07154(9) 0.0244(2) Uani 1 1 d . . . . .
H1 H 0.421(2) 0.3708(9) 0.1234(15) 0.035(5) Uiso 1 1 d . . . . .
N2 N 0.73144(14) 0.45318(6) 0.60156(9) 0.0274(2) Uani 1 1 d . . . . .
N3 N 0.90129(14) 0.40303(6) 0.74176(9) 0.0256(2) Uani 1 1 d . . . . .
C1 C 0.38279(15) 0.30489(6) 0.01418(11) 0.0242(2) Uani 1 1 d . . . . .
C2 C 0.36871(17) 0.29506(7) -0.09564(12) 0.0305(3) Uani 1 1 d . . . . .
C3 C 0.2858(2) 0.24278(8) -0.15344(13) 0.0402(4) Uani 1 1 d . . . . .
H3A H 0.281366 0.236716 -0.227320 0.048 Uiso 1 1 calc R U . . .
C4 C 0.2099(2) 0.19972(8) -0.10269(15) 0.0434(4) Uani 1 1 d . . . . .
H4 H 0.151510 0.164327 -0.142250 0.052 Uiso 1 1 calc R U . . .
C5 C 0.21839(19) 0.20779(7) 0.00495(14) 0.0372(3) Uani 1 1 d . . . . .
H5 H 0.164577 0.178618 0.039544 0.045 Uiso 1 1 calc R U . . .
C6 C 0.30644(16) 0.25902(7) 0.06206(11) 0.0276(3) Uani 1 1 d . . . . .
C7 C 0.63625(15) 0.36316(6) 0.10345(10) 0.0214(2) Uani 1 1 d . . . . .
C8 C 0.71033(16) 0.41730(6) 0.16328(10) 0.0225(2) Uani 1 1 d . . . . .
C9 C 0.88134(17) 0.41968(7) 0.20281(11) 0.0284(3) Uani 1 1 d . . . . .
H9 H 0.932200 0.455008 0.246406 0.034 Uiso 1 1 calc R U . . .
C10 C 0.97977(17) 0.37183(8) 0.18029(12) 0.0322(3) Uani 1 1 d . . . . .
H10 H 1.096254 0.374306 0.208479 0.039 Uiso 1 1 calc R U . . .
C11 C 0.90583(17) 0.32048(7) 0.11621(12) 0.0303(3) Uani 1 1 d . . . . .
H11 H 0.971955 0.288270 0.098161 0.036 Uiso 1 1 calc R U . . .
C12 C 0.73520(16) 0.31589(6) 0.07821(11) 0.0257(3) Uani 1 1 d . . . . .
H12 H 0.685460 0.280360 0.034740 0.031 Uiso 1 1 calc R U . . .
C13 C 0.60845(17) 0.47298(6) 0.18223(11) 0.0256(3) Uani 1 1 d . . . . .
H13A H 0.518371 0.481346 0.114492 0.031 Uiso 1 1 calc R U . . .
H13B H 0.678725 0.511656 0.198732 0.031 Uiso 1 1 calc R U . . .
C14 C 0.53419(16) 0.46170(6) 0.27468(10) 0.0226(2) Uani 1 1 d . . . . .
C15 C 0.7435(3) 0.62712(12) 0.52442(17) 0.0620(6) Uani 1 1 d D . . . .
H15A H 0.724874 0.629298 0.445696 0.093 Uiso 1 1 calc R U . . .
H15B H 0.844455 0.602923 0.558263 0.093 Uiso 1 1 calc R U . . .
H15C H 0.754625 0.670534 0.554519 0.093 Uiso 1 1 calc R U . . .
C16 C 0.87961(18) 0.44324(7) 0.58130(11) 0.0309(3) Uani 1 1 d . . . . .
H16 H 0.904139 0.455863 0.517039 0.037 Uiso 1 1 calc R U . . .
C17 C 0.98553(17) 0.41259(7) 0.66733(12) 0.0308(3) Uani 1 1 d . . . . .
H17 H 1.095673 0.400273 0.674437 0.037 Uiso 1 1 calc R U . . .
C18 C 0.75046(17) 0.42825(7) 0.69861(11) 0.0270(3) Uani 1 1 d . . . . .
H18 H 0.667222 0.428140 0.733935 0.032 Uiso 1 1 calc R U . . .
C19 C 0.96568(18) 0.37498(7) 0.85063(11) 0.0290(3) Uani 1 1 d . . . . .
H19A H 1.039633 0.338906 0.847741 0.035 Uiso 1 1 calc R U . . .
H19B H 0.872975 0.357741 0.873592 0.035 Uiso 1 1 calc R U . . .
C20 C 1.05993(16) 0.42357(7) 0.93448(11) 0.0272(3) Uani 1 1 d . . . . .
H20A H 1.147366 0.443025 0.908532 0.033 Uiso 1 1 calc R U . . .
H20B H 1.114038 0.400966 1.003437 0.033 Uiso 1 1 calc R U . . .
C21 C 0.95143(16) 0.47674(7) 0.95681(10) 0.0255(3) Uani 1 1 d . . . . .
H21A H 0.900025 0.500469 0.888589 0.031 Uiso 1 1 calc R U . . .
H21B H 0.862158 0.457478 0.981103 0.031 Uiso 1 1 calc R U . . .


_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
Mn1 O2 2.1614(10) . ?
Mn1 O2 2.1615(10) 3_666 ?
Mn1 O3 2.2318(10) 3_666 ?
Mn1 O3 2.2318(10) . ?
Mn1 N2 2.2382(12) 3_666 ?
Mn1 N2 2.2382(12) . ?
Cl1 C2 1.7379(16) . ?
Cl2 C6 1.7371(15) . ?
O1 C14 1.2574(16) . ?
O2 C14 1.2602(15) . ?
O3 H3 0.889(9) . ?
O3 C15 1.394(2) . ?
N1 H1 0.887(19) . ?
N1 C1 1.4019(16) . ?
N1 C7 1.4077(16) . ?
N2 C16 1.3783(18) . ?
N2 C18 1.3193(18) . ?
N3 C17 1.3733(18) . ?
N3 C18 1.3448(17) . ?
N3 C19 1.4671(17) . ?
C1 C2 1.3993(19) . ?
C1 C6 1.401(2) . ?
C2 C3 1.390(2) . ?
C3 H3A 0.9500 . ?
C3 C4 1.381(3) . ?
C4 H4 0.9500 . ?
C4 C5 1.378(3) . ?
C5 H5 0.9500 . ?
C5 C6 1.385(2) . ?
C7 C8 1.4075(17) . ?
C7 C12 1.3982(17) . ?
C8 C9 1.3920(19) . ?
C8 C13 1.5141(18) . ?
C9 H9 0.9500 . ?
C9 C10 1.390(2) . ?
C10 H10 0.9500 . ?
C10 C11 1.385(2) . ?
C11 H11 0.9500 . ?
C11 C12 1.3905(19) . ?
C12 H12 0.9500 . ?
C13 H13A 0.9900 . ?
C13 H13B 0.9900 . ?
C13 C14 1.5251(17) . ?
C15 H15A 0.9800 . ?
C15 H15B 0.9800 . ?
C15 H15C 0.9800 . ?
C16 H16 0.9500 . ?
C16 C17 1.362(2) . ?
C17 H17 0.9500 . ?
C18 H18 0.9500 . ?
C19 H19A 0.9900 . ?
C19 H19B 0.9900 . ?
C19 C20 1.5244(19) . ?
C20 H20A 0.9900 . ?
C20 H20B 0.9900 . ?
C20 C21 1.5262(18) . ?
C21 C21 1.522(3) 3_767 ?
C21 H21A 0.9900 . ?
C21 H21B 0.9900 . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
O2 Mn1 O2 179.998(17) . 3_666 ?
O2 Mn1 O3 87.98(4) 3_666 . ?
O2 Mn1 O3 92.02(4) . . ?
O2 Mn1 O3 92.02(4) 3_666 3_666 ?
O2 Mn1 O3 87.98(4) . 3_666 ?
O2 Mn1 N2 90.67(4) 3_666 3_666 ?
O2 Mn1 N2 89.32(4) . 3_666 ?
O2 Mn1 N2 90.67(4) . . ?
O2 Mn1 N2 89.33(4) 3_666 . ?
O3 Mn1 O3 180.00(2) 3_666 . ?
O3 Mn1 N2 90.80(4) 3_666 3_666 ?
O3 Mn1 N2 90.80(4) . . ?
O3 Mn1 N2 89.20(4) . 3_666 ?
O3 Mn1 N2 89.20(4) 3_666 . ?
N2 Mn1 N2 180.0 3_666 . ?
C14 O2 Mn1 128.67(9) . . ?
Mn1 O3 H3 106.3(10) . . ?
C15 O3 Mn1 131.69(12) . . ?
C15 O3 H3 107.0(10) . . ?
C1 N1 H1 112.6(12) . . ?
C1 N1 C7 120.95(10) . . ?
C7 N1 H1 112.6(12) . . ?
C16 N2 Mn1 130.58(9) . . ?
C18 N2 Mn1 124.33(9) . . ?
C18 N2 C16 105.10(11) . . ?
C17 N3 C19 127.04(12) . . ?
C18 N3 C17 106.72(11) . . ?
C18 N3 C19 126.11(12) . . ?
C2 C1 N1 122.05(13) . . ?
C2 C1 C6 115.76(12) . . ?
C6 C1 N1 122.16(12) . . ?
C1 C2 Cl1 119.26(11) . . ?
C3 C2 Cl1 118.46(12) . . ?
C3 C2 C1 122.25(15) . . ?
C2 C3 H3A 120.2 . . ?
C4 C3 C2 119.52(15) . . ?
C4 C3 H3A 120.2 . . ?
C3 C4 H4 119.8 . . ?
C5 C4 C3 120.40(14) . . ?
C5 C4 H4 119.8 . . ?
C4 C5 H5 120.4 . . ?
C4 C5 C6 119.11(15) . . ?
C6 C5 H5 120.4 . . ?
C1 C6 Cl2 118.77(10) . . ?
C5 C6 Cl2 118.32(12) . . ?
C5 C6 C1 122.90(14) . . ?
C8 C7 N1 118.32(11) . . ?
C12 C7 N1 122.15(11) . . ?
C12 C7 C8 119.52(12) . . ?
C7 C8 C13 121.44(11) . . ?
C9 C8 C7 118.52(12) . . ?
C9 C8 C13 120.02(12) . . ?
C8 C9 H9 119.1 . . ?
C10 C9 C8 121.85(13) . . ?
C10 C9 H9 119.1 . . ?
C9 C10 H10 120.4 . . ?
C11 C10 C9 119.14(13) . . ?
C11 C10 H10 120.4 . . ?
C10 C11 H11 119.9 . . ?
C10 C11 C12 120.26(13) . . ?
C12 C11 H11 119.9 . . ?
C7 C12 H12 119.7 . . ?
C11 C12 C7 120.53(12) . . ?
C11 C12 H12 119.7 . . ?
C8 C13 H13A 108.9 . . ?
C8 C13 H13B 108.9 . . ?
C8 C13 C14 113.49(10) . . ?
H13A C13 H13B 107.7 . . ?
C14 C13 H13A 108.9 . . ?
C14 C13 H13B 108.9 . . ?
O1 C14 O2 125.11(12) . . ?
O1 C14 C13 117.43(11) . . ?
O2 C14 C13 117.46(12) . . ?
O3 C15 H15A 109.5 . . ?
O3 C15 H15B 109.5 . . ?
O3 C15 H15C 109.5 . . ?
H15A C15 H15B 109.5 . . ?
H15A C15 H15C 109.5 . . ?
H15B C15 H15C 109.5 . . ?
N2 C16 H16 125.1 . . ?
C17 C16 N2 109.70(12) . . ?
C17 C16 H16 125.1 . . ?
N3 C17 H17 126.9 . . ?
C16 C17 N3 106.27(12) . . ?
C16 C17 H17 126.9 . . ?
N2 C18 N3 112.21(12) . . ?
N2 C18 H18 123.9 . . ?
N3 C18 H18 123.9 . . ?
N3 C19 H19A 109.2 . . ?
N3 C19 H19B 109.2 . . ?
N3 C19 C20 112.26(11) . . ?
H19A C19 H19B 107.9 . . ?
C20 C19 H19A 109.2 . . ?
C20 C19 H19B 109.2 . . ?
C19 C20 H20A 108.9 . . ?
C19 C20 H20B 108.9 . . ?
C19 C20 C21 113.49(11) . . ?
H20A C20 H20B 107.7 . . ?
C21 C20 H20A 108.9 . . ?
C21 C20 H20B 108.9 . . ?
C20 C21 H21A 109.2 . . ?
C20 C21 H21B 109.2 . . ?
C21 C21 C20 112.07(13) 3_767 . ?
C21 C21 H21A 109.2 3_767 . ?
C21 C21 H21B 109.2 3_767 . ?
H21A C21 H21B 107.9 . . ?

loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
Mn1 O2 C14 O1 -5.4(2) . . . . ?
Mn1 O2 C14 C13 174.36(8) . . . . ?
Mn1 N2 C16 C17 179.94(10) . . . . ?
Mn1 N2 C18 N3 179.84(9) . . . . ?
Cl1 C2 C3 C4 -176.11(13) . . . . ?
N1 C1 C2 Cl1 -0.48(18) . . . . ?
N1 C1 C2 C3 -178.57(13) . . . . ?
N1 C1 C6 Cl2 -4.49(17) . . . . ?
N1 C1 C6 C5 176.27(13) . . . . ?
N1 C7 C8 C9 174.70(12) . . . . ?
N1 C7 C8 C13 -7.05(18) . . . . ?
N1 C7 C12 C11 -176.43(13) . . . . ?
N2 C16 C17 N3 0.37(16) . . . . ?
N3 C19 C20 C21 66.72(15) . . . . ?
C1 N1 C7 C8 -178.39(12) . . . . ?
C1 N1 C7 C12 1.20(19) . . . . ?
C1 C2 C3 C4 2.0(2) . . . . ?
C2 C1 C6 Cl2 177.59(10) . . . . ?
C2 C1 C6 C5 -1.65(19) . . . . ?
C2 C3 C4 C5 -1.1(2) . . . . ?
C3 C4 C5 C6 -1.1(2) . . . . ?
C4 C5 C6 Cl2 -176.68(12) . . . . ?
C4 C5 C6 C1 2.6(2) . . . . ?
C6 C1 C2 Cl1 177.44(10) . . . . ?
C6 C1 C2 C3 -0.7(2) . . . . ?
C7 N1 C1 C2 -73.92(17) . . . . ?
C7 N1 C1 C6 108.29(15) . . . . ?
C7 C8 C9 C10 3.2(2) . . . . ?
C7 C8 C13 C14 80.69(15) . . . . ?
C8 C7 C12 C11 3.2(2) . . . . ?
C8 C9 C10 C11 0.4(2) . . . . ?
C8 C13 C14 O1 -67.40(16) . . . . ?
C8 C13 C14 O2 112.78(13) . . . . ?
C9 C8 C13 C14 -101.09(14) . . . . ?
C9 C10 C11 C12 -2.2(2) . . . . ?
C10 C11 C12 C7 0.5(2) . . . . ?
C12 C7 C8 C9 -4.90(18) . . . . ?
C12 C7 C8 C13 173.35(12) . . . . ?
C13 C8 C9 C10 -175.09(13) . . . . ?
C16 N2 C18 N3 0.02(16) . . . . ?
C17 N3 C18 N2 0.21(16) . . . . ?
C17 N3 C19 C20 81.92(17) . . . . ?
C18 N2 C16 C17 -0.25(16) . . . . ?
C18 N3 C17 C16 -0.35(16) . . . . ?
C18 N3 C19 C20 -93.36(16) . . . . ?
C19 N3 C17 C16 -176.36(13) . . . . ?
C19 N3 C18 N2 176.27(12) . . . . ?
C19 C20 C21 C21 178.36(14) . . . 3_767 ?

_olex2_submission_special_instructions 'No special instructions were received'
# start Validation Reply Form
_vrf_PLAT910_mo_jlk052_0m        
;
PROBLEM: Missing # of FCF Reflection(s) Below Theta(Min).          6 Note  
RESPONSE: This represents only a very small number of reflections compared 
with the total number that were collected, and may result from full 
or partial obstruction by the beamstop.
;
_vrf_PLAT911_mo_jlk052_0m        
;
PROBLEM: Missing FCF Refl Between Thmin & STh/L=    0.600         25 Report
RESPONSE: This represents only a very small number of reflections compared 
with the total number that were collected, and may result from weak diffraction,
or partial obstruction by the beamstop
;
_vrf_PLAT913_mo_jlk052_0m        
;
PROBLEM: Missing # of Very Strong Reflections in FCF ....         12 Note  
RESPONSE: This represents only a very small number of reflections compared 
with the total number that were collected, and may result from weak diffraction,
or partial obstruction by the beamstop
;
# end Validation Reply Form
####################################################################### 
# 
# 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_cu_jnm106
_database_code_depnum_ccdc_archive 'CCDC 2237928'
loop_
_audit_author_name
_audit_author_address
'Jennifer Murphy'
;University of Guelph
Canada
;
_audit_update_record             
;
2023-01-25 deposited with the CCDC.	2024-04-11 downloaded from the CCDC.
;
_audit_creation_date             2021-02-16
_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         'C44 H50 Cl4 Mg N6 O6'
_chemical_formula_sum            'C44 H50 Cl4 Mg N6 O6'
_chemical_formula_weight         925.01
_chemical_melting_point          ?
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0181 0.0091 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Cl Cl 0.3639 0.7018 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Mg Mg 0.1719 0.1771 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0311 0.0180 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0492 0.0322 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_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/n 1'
_space_group_name_Hall           '-P 2yn'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x+1/2, y+1/2, -z+1/2'
'-x, -y, -z'
'x-1/2, -y-1/2, z-1/2'

_cell_length_a                   8.50360(10)
_cell_length_b                   21.7792(3)
_cell_length_c                   12.8123(2)
_cell_angle_alpha                90
_cell_angle_beta                 108.489(2)
_cell_angle_gamma                90
_cell_volume                     2250.38(6)
_cell_formula_units_Z            2
_cell_measurement_reflns_used    12645
_cell_measurement_temperature    170
_cell_measurement_theta_max      78.6990
_cell_measurement_theta_min      4.0560
_shelx_estimated_absorpt_T_max   0.756
_shelx_estimated_absorpt_T_min   0.588
_exptl_absorpt_coefficient_mu    2.970
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.75800
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
;
CrysAlisPro 1.171.40.53 (Rigaku Oxford Diffraction, 2019)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_absorpt_special_details   ?
_exptl_crystal_colour            'clear colourless'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.365
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       prism
_exptl_crystal_F_000             968
_exptl_crystal_size_max          0.2
_exptl_crystal_size_mid          0.2
_exptl_crystal_size_min          0.1
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0675
_diffrn_reflns_av_unetI/netI     0.0293
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 1.000
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_k_max       26
_diffrn_reflns_limit_k_min       -26
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_number            45917
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 1.000
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         68.232
_diffrn_reflns_theta_min         4.060
_diffrn_ambient_temperature      170
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean ?
_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    191.08 286.08   1.00   21.30    --  -90.12 -59.25 110.08   95
  2  ω   -136.76 -25.76   1.00   25.00    -- -105.12  83.74 130.05  111
  3  ω   -136.76 -25.76   1.00   25.00    -- -105.12  83.74 -29.95  111
  4  ω    191.08 286.08   1.00   21.30    --  -90.12 -59.25  20.08   95
  5  ω    176.08 272.08   1.00   25.00    -- -105.12 -59.25-139.92   96
  6  ω      3.93  99.93   1.00   15.00    --   20.69  59.25 159.92   96
  7  ω    176.08 271.08   1.00   25.00    -- -105.12 -59.25 -59.92   95
  8  ω      3.93  99.93   1.00   15.00    --   20.69  59.25  69.92   96
  9  ω   -136.76 -25.76   1.00   25.00    -- -105.12  83.74-109.95  111
 10  ω    176.08 271.08   1.00   25.00    -- -105.12 -59.25 -19.92   95
 11  ω    -26.23  72.77   1.00   16.00    --   50.69 -83.74 -75.05   99
 12  ω   -136.76 -25.76   1.00   25.00    -- -105.12  83.74 -69.95  111
 13  ω   -136.76 -25.76   1.00   25.00    -- -105.12  83.74  90.05  111
 14  ω    -26.23  72.77   1.00   16.00    --   50.69 -83.74  29.95   99
 15  φ   -160.88 148.13   1.00   25.00 -25.56-105.12  31.50    --   309
 16  ω      3.93  99.93   1.00   15.00    --   20.69  59.25 -20.08   96
 17  ω   -136.76 -26.76   1.00   25.00    -- -105.12  83.74  50.05  110
 18  ω    191.08 286.08   1.00   21.30    --  -90.12 -59.25-159.92   95
 19  ω   -136.76 -25.76   1.00   25.00    -- -105.12  83.74-149.95  111
 20  ω    176.08 271.08   1.00   25.00    -- -105.12 -59.25 100.08   95
 21  ω    -26.23  72.77   1.00   16.00    --   50.69 -83.74 131.95   99
 22  ω    176.08 271.08   1.00   25.00    -- -105.12 -59.25  20.08   95
 23  ω   -136.76 -25.76   1.00   25.00    -- -105.12  83.74  10.05  111
;
_diffrn_measurement_device       'abstract diffractometer'
_diffrn_measurement_device_type  
'Saxi-CrysAlisPro-abstract goniometer imported SAXI images'
_diffrn_measurement_method       'ω and φ scans'
_diffrn_orient_matrix_type       
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      0.0297865000
_diffrn_orient_matrix_UB_12      0.0687946000
_diffrn_orient_matrix_UB_13      0.0267621000
_diffrn_orient_matrix_UB_21      0.1010983000
_diffrn_orient_matrix_UB_22      -0.0161324000
_diffrn_orient_matrix_UB_23      0.1194725000
_diffrn_orient_matrix_UB_31      0.1594282000
_diffrn_orient_matrix_UB_32      -0.0026933000
_diffrn_orient_matrix_UB_33      -0.0327142000
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_source                   'fine-focus sealed X-ray tube'
_diffrn_source_type              'Enhance (Cu) X-ray Source'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                3539
_reflns_number_total             4132
_reflns_odcompleteness_completeness 99.32
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     78.82
_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
;
_reflns_threshold_expression     'I > 2σ(I)'
_computing_cell_refinement       'CrysAlisPro 1.171.40.53 (Rigaku OD, 2019)'
_computing_data_collection       'CrysAlisPro 1.171.40.53 (Rigaku OD, 2019)'
_computing_data_reduction        'CrysAlisPro 1.171.40.53 (Rigaku OD, 2019)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'XL (Sheldrick, 2008)'
_computing_structure_solution    'XT (Sheldrick, 2015)'
_refine_diff_density_max         0.217
_refine_diff_density_min         -0.286
_refine_diff_density_rms         0.050
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.048
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     285
_refine_ls_number_reflns         4132
_refine_ls_number_restraints     9
_refine_ls_R_factor_all          0.0421
_refine_ls_R_factor_gt           0.0346
_refine_ls_restrained_S_all      1.055
_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)+(0.0489P)²+0.7698P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0893
_refine_ls_wR_factor_ref         0.0942
_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, All O(H) groups
2. Restrained distances
 O3-H3
 0.87 with sigma of 0.01
 C21-H3
 1.905966 with sigma of 0.02
 Mg1-H3
 2.667649 with sigma of 0.02
3. Uiso/Uaniso restraints and constraints
C21 \\sim C22: within 1.7A with sigma of 0.02 and sigma for terminal atoms of
0.04
4.a Secondary CH2 refined with riding coordinates:
 C2(H2A,H2B), C18(H18A,H18B), C19(H19A,H19B), C20(H20A,H20B), C21(H21A,H21B)
4.b Aromatic/amide H refined with riding coordinates:
 C4(H4), C5(H5), C6(H6), C7(H7), C11(H11), C12(H12), C13(H13), C15(H15),
 C16(H16), C17(H17)
4.c Idealised Me refined as rotating group:
 C22(H22A,H22B,H22C)
;
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     dual
_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
Cl1 Cl 0.68931(6) 0.26575(2) 0.30135(4) 0.03570(14) Uani 1 1 d . . . . .
Cl2 Cl 0.56397(6) 0.35472(2) 0.66174(4) 0.04050(14) Uani 1 1 d . . . . .
Mg1 Mg 0.500000 0.500000 0.000000 0.01688(17) Uani 1 2 d DS T P . .
O1 O 0.42705(14) 0.49107(5) 0.13754(9) 0.0220(3) Uani 1 1 d . . . . .
O2 O 0.58467(16) 0.41506(6) 0.23239(10) 0.0299(3) Uani 1 1 d . . . . .
O3 O 0.37723(15) 0.58394(5) -0.03644(10) 0.0235(3) Uani 1 1 d D . . . .
H3 H 0.371(2) 0.5950(8) -0.1040(10) 0.035 Uiso 1 1 d DR . . . .
N1 N 0.72239(17) 0.54917(6) 0.10000(11) 0.0216(3) Uani 1 1 d . . . . .
N2 N 0.88896(17) 0.59794(6) 0.24381(11) 0.0215(3) Uani 1 1 d . . . . .
N3 N 0.55219(17) 0.35790(6) 0.42449(12) 0.0223(3) Uani 1 1 d . . . . .
C1 C 0.4819(2) 0.45811(7) 0.22158(13) 0.0189(3) Uani 1 1 d . . . . .
C2 C 0.4185(2) 0.47101(7) 0.31824(14) 0.0231(4) Uani 1 1 d . . . . .
H2A H 0.514290 0.476683 0.385718 0.028 Uiso 1 1 calc R . . . .
H2B H 0.354157 0.509729 0.304240 0.028 Uiso 1 1 calc R . . . .
C3 C 0.3101(2) 0.41985(7) 0.33708(13) 0.0198(3) Uani 1 1 d . . . . .
C4 C 0.1384(2) 0.42563(8) 0.29880(14) 0.0256(4) Uani 1 1 d . . . . .
H4 H 0.090429 0.461016 0.257581 0.031 Uiso 1 1 calc R . . . .
C5 C 0.0352(2) 0.38099(9) 0.31930(15) 0.0288(4) Uani 1 1 d . . . . .
H5 H -0.081811 0.385430 0.291149 0.035 Uiso 1 1 calc R . . . .
C6 C 0.1045(2) 0.33024(9) 0.38086(15) 0.0274(4) Uani 1 1 d . . . . .
H6 H 0.035079 0.300240 0.397689 0.033 Uiso 1 1 calc R . . . .
C7 C 0.2758(2) 0.32275(8) 0.41849(14) 0.0232(4) Uani 1 1 d . . . . .
H7 H 0.322633 0.287653 0.461057 0.028 Uiso 1 1 calc R . . . .
C8 C 0.3790(2) 0.36618(7) 0.39433(13) 0.0189(3) Uani 1 1 d . . . . .
C9 C 0.6295(2) 0.30622(7) 0.48477(14) 0.0223(4) Uani 1 1 d . . . . .
C10 C 0.6432(2) 0.29862(8) 0.59567(15) 0.0285(4) Uani 1 1 d . . . . .
C11 C 0.7227(3) 0.24844(10) 0.65687(18) 0.0391(5) Uani 1 1 d . . . . .
H11 H 0.727318 0.244105 0.731563 0.047 Uiso 1 1 calc R . . . .
C12 C 0.7951(3) 0.20486(9) 0.6082(2) 0.0426(5) Uani 1 1 d . . . . .
H12 H 0.850245 0.170586 0.649768 0.051 Uiso 1 1 calc R . . . .
C13 C 0.7875(2) 0.21094(9) 0.49976(19) 0.0366(5) Uani 1 1 d . . . . .
H13 H 0.838917 0.181398 0.466674 0.044 Uiso 1 1 calc R . . . .
C14 C 0.7040(2) 0.26064(8) 0.43918(16) 0.0270(4) Uani 1 1 d . . . . .
C15 C 0.7387(2) 0.57284(8) 0.19748(14) 0.0225(4) Uani 1 1 d . . . . .
H15 H 0.653947 0.572225 0.231124 0.027 Uiso 1 1 calc R . . . .
C16 C 0.8717(2) 0.56014(8) 0.08280(14) 0.0250(4) Uani 1 1 d . . . . .
H16 H 0.898100 0.548664 0.018765 0.030 Uiso 1 1 calc R . . . .
C17 C 0.9755(2) 0.58979(8) 0.17094(15) 0.0259(4) Uani 1 1 d . . . . .
H17 H 1.086131 0.602405 0.180328 0.031 Uiso 1 1 calc R . . . .
C18 C 0.9535(2) 0.62303(8) 0.35573(14) 0.0272(4) Uani 1 1 d . . . . .
H18A H 0.859715 0.637379 0.379455 0.033 Uiso 1 1 calc R . . . .
H18B H 1.024931 0.658882 0.355392 0.033 Uiso 1 1 calc R . . . .
C19 C 1.0529(2) 0.57578(8) 0.43736(14) 0.0260(4) Uani 1 1 d . . . . .
H19A H 1.107375 0.596437 0.508518 0.031 Uiso 1 1 calc R . . . .
H19B H 1.141255 0.559309 0.410169 0.031 Uiso 1 1 calc R . . . .
C20 C 0.9495(2) 0.52235(8) 0.45677(14) 0.0248(4) Uani 1 1 d . . . . .
H20A H 0.857601 0.538742 0.480428 0.030 Uiso 1 1 calc R . . . .
H20B H 0.900113 0.500056 0.386640 0.030 Uiso 1 1 calc R . . . .
C21 C 0.2234(2) 0.59950(8) -0.02127(16) 0.0290(4) Uani 1 1 d D U . . .
H21A H 0.217585 0.580328 0.047462 0.035 Uiso 1 1 calc R . . . .
H21B H 0.131555 0.582714 -0.083170 0.035 Uiso 1 1 calc R . . . .
C22 C 0.2020(3) 0.66730(10) -0.0151(2) 0.0490(6) Uani 1 1 d . U . . .
H22A H 0.200009 0.686149 -0.084994 0.073 Uiso 1 1 calc GR . . . .
H22B H 0.294481 0.684278 0.044687 0.073 Uiso 1 1 calc GR . . . .
H22C H 0.097435 0.675965 -0.001069 0.073 Uiso 1 1 calc GR . . . .
H3A H 0.595(3) 0.3685(10) 0.3712(18) 0.031(5) Uiso 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
Cl1 C14 1.734(2) . ?
Cl2 C10 1.739(2) . ?
Mg1 O1 2.0546(11) . ?
Mg1 O1 2.0547(11) 3_665 ?
Mg1 O3 2.0834(11) 3_665 ?
Mg1 O3 2.0834(11) . ?
Mg1 N1 2.1972(14) 3_665 ?
Mg1 N1 2.1972(14) . ?
O1 C1 1.254(2) . ?
O2 C1 1.259(2) . ?
O3 H3 0.884(9) . ?
O3 C21 1.423(2) . ?
N1 C15 1.317(2) . ?
N1 C16 1.377(2) . ?
N2 C15 1.343(2) . ?
N2 C17 1.372(2) . ?
N2 C18 1.469(2) . ?
N3 C8 1.411(2) . ?
N3 C9 1.405(2) . ?
N3 H3A 0.90(2) . ?
C1 C2 1.525(2) . ?
C2 H2A 0.9900 . ?
C2 H2B 0.9900 . ?
C2 C3 1.513(2) . ?
C3 C4 1.391(2) . ?
C3 C8 1.405(2) . ?
C4 H4 0.9500 . ?
C4 C5 1.389(3) . ?
C5 H5 0.9500 . ?
C5 C6 1.377(3) . ?
C6 H6 0.9500 . ?
C6 C7 1.391(2) . ?
C7 H7 0.9500 . ?
C7 C8 1.391(2) . ?
C9 C10 1.398(3) . ?
C9 C14 1.401(3) . ?
C10 C11 1.389(3) . ?
C11 H11 0.9500 . ?
C11 C12 1.383(3) . ?
C12 H12 0.9500 . ?
C12 C13 1.377(3) . ?
C13 H13 0.9500 . ?
C13 C14 1.389(3) . ?
C15 H15 0.9500 . ?
C16 H16 0.9500 . ?
C16 C17 1.356(3) . ?
C17 H17 0.9500 . ?
C18 H18A 0.9900 . ?
C18 H18B 0.9900 . ?
C18 C19 1.519(3) . ?
C19 H19A 0.9900 . ?
C19 H19B 0.9900 . ?
C19 C20 1.526(2) . ?
C20 C20 1.519(3) 3_766 ?
C20 H20A 0.9900 . ?
C20 H20B 0.9900 . ?
C21 H21A 0.9900 . ?
C21 H21B 0.9900 . ?
C21 C22 1.493(3) . ?
C22 H22A 0.9800 . ?
C22 H22B 0.9800 . ?
C22 H22C 0.9800 . ?

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
O1 Mg1 O1 180.0 . 3_665 ?
O1 Mg1 O3 89.48(5) 3_665 . ?
O1 Mg1 O3 90.52(5) . . ?
O1 Mg1 O3 90.52(5) 3_665 3_665 ?
O1 Mg1 O3 89.48(5) . 3_665 ?
O1 Mg1 N1 90.91(5) 3_665 . ?
O1 Mg1 N1 89.09(5) . . ?
O1 Mg1 N1 90.91(5) . 3_665 ?
O1 Mg1 N1 89.09(5) 3_665 3_665 ?
O3 Mg1 O3 180.0 3_665 . ?
O3 Mg1 N1 91.12(5) 3_665 . ?
O3 Mg1 N1 91.12(5) . 3_665 ?
O3 Mg1 N1 88.88(5) . . ?
O3 Mg1 N1 88.88(5) 3_665 3_665 ?
N1 Mg1 N1 180.0 . 3_665 ?
C1 O1 Mg1 131.24(11) . . ?
Mg1 O3 H3 109.2(10) . . ?
C21 O3 Mg1 126.54(10) . . ?
C21 O3 H3 107.3(10) . . ?
C15 N1 Mg1 123.78(11) . . ?
C15 N1 C16 104.99(14) . . ?
C16 N1 Mg1 131.17(11) . . ?
C15 N2 C17 106.70(14) . . ?
C15 N2 C18 126.29(15) . . ?
C17 N2 C18 126.70(14) . . ?
C8 N3 H3A 113.6(13) . . ?
C9 N3 C8 121.26(14) . . ?
C9 N3 H3A 112.9(13) . . ?
O1 C1 O2 125.21(15) . . ?
O1 C1 C2 117.43(14) . . ?
O2 C1 C2 117.36(14) . . ?
C1 C2 H2A 109.1 . . ?
C1 C2 H2B 109.1 . . ?
H2A C2 H2B 107.8 . . ?
C3 C2 C1 112.58(13) . . ?
C3 C2 H2A 109.1 . . ?
C3 C2 H2B 109.1 . . ?
C4 C3 C2 120.09(15) . . ?
C4 C3 C8 118.47(15) . . ?
C8 C3 C2 121.43(15) . . ?
C3 C4 H4 119.2 . . ?
C5 C4 C3 121.68(16) . . ?
C5 C4 H4 119.2 . . ?
C4 C5 H5 120.4 . . ?
C6 C5 C4 119.28(16) . . ?
C6 C5 H5 120.4 . . ?
C5 C6 H6 119.9 . . ?
C5 C6 C7 120.22(16) . . ?
C7 C6 H6 119.9 . . ?
C6 C7 H7 119.7 . . ?
C8 C7 C6 120.56(16) . . ?
C8 C7 H7 119.7 . . ?
C3 C8 N3 118.40(14) . . ?
C7 C8 N3 122.00(15) . . ?
C7 C8 C3 119.60(15) . . ?
C10 C9 N3 121.82(16) . . ?
C10 C9 C14 115.90(16) . . ?
C14 C9 N3 122.21(16) . . ?
C9 C10 Cl2 119.42(14) . . ?
C11 C10 Cl2 118.17(16) . . ?
C11 C10 C9 122.39(19) . . ?
C10 C11 H11 120.3 . . ?
C12 C11 C10 119.5(2) . . ?
C12 C11 H11 120.3 . . ?
C11 C12 H12 119.9 . . ?
C13 C12 C11 120.27(18) . . ?
C13 C12 H12 119.9 . . ?
C12 C13 H13 120.3 . . ?
C12 C13 C14 119.4(2) . . ?
C14 C13 H13 120.3 . . ?
C9 C14 Cl1 118.88(13) . . ?
C13 C14 Cl1 118.58(16) . . ?
C13 C14 C9 122.53(18) . . ?
N1 C15 N2 112.20(15) . . ?
N1 C15 H15 123.9 . . ?
N2 C15 H15 123.9 . . ?
N1 C16 H16 125.1 . . ?
C17 C16 N1 109.83(15) . . ?
C17 C16 H16 125.1 . . ?
N2 C17 H17 126.9 . . ?
C16 C17 N2 106.27(15) . . ?
C16 C17 H17 126.9 . . ?
N2 C18 H18A 109.2 . . ?
N2 C18 H18B 109.2 . . ?
N2 C18 C19 111.98(14) . . ?
H18A C18 H18B 107.9 . . ?
C19 C18 H18A 109.2 . . ?
C19 C18 H18B 109.2 . . ?
C18 C19 H19A 108.8 . . ?
C18 C19 H19B 108.8 . . ?
C18 C19 C20 113.90(14) . . ?
H19A C19 H19B 107.7 . . ?
C20 C19 H19A 108.8 . . ?
C20 C19 H19B 108.8 . . ?
C19 C20 H20A 109.1 . . ?
C19 C20 H20B 109.1 . . ?
C20 C20 C19 112.67(18) 3_766 . ?
C20 C20 H20A 109.1 3_766 . ?
C20 C20 H20B 109.1 3_766 . ?
H20A C20 H20B 107.8 . . ?
O3 C21 H21A 109.2 . . ?
O3 C21 H21B 109.2 . . ?
O3 C21 C22 112.07(16) . . ?
H21A C21 H21B 107.9 . . ?
C22 C21 H21A 109.2 . . ?
C22 C21 H21B 109.2 . . ?
C21 C22 H22A 109.5 . . ?
C21 C22 H22B 109.5 . . ?
C21 C22 H22C 109.5 . . ?
H22A C22 H22B 109.5 . . ?
H22A C22 H22C 109.5 . . ?
H22B C22 H22C 109.5 . . ?

_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
- Detector area scaling
;
_oxdiff_exptl_absorpt_empirical_full_max 1.247
_oxdiff_exptl_absorpt_empirical_full_min 0.757
####################################################################### 
# 
# 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_cu_jnm034
_database_code_depnum_ccdc_archive 'CCDC 2237929'
loop_
_audit_author_name
_audit_author_address
'Jennifer Murphy'
;University of Guelph
Canada
;
_audit_update_record             
;
2023-01-25 deposited with the CCDC.	2024-04-11 downloaded from the CCDC.
;
_audit_creation_date             2020-03-25
_audit_creation_method           
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_shelx_SHELXL_version_number     2017/1
_chemical_name_common            ?
_chemical_name_systematic        ?
_chemical_formula_moiety         'C40 H38 Cl4 Cu N6 O4, 2(C H4 O)'
_chemical_formula_sum            'C42 H46 Cl4 Cu N6 O6'
_chemical_formula_weight         936.19
_chemical_melting_point          ?
_chemical_oxdiff_formula         'C42Cl4CuN6O6H40 '
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0181 0.0091 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Cl Cl 0.3639 0.7018 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Cu Cu -1.9646 0.5888 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0311 0.0180 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0492 0.0322 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_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/n 1'
_space_group_name_Hall           '-P 2yn'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x+1/2, y+1/2, -z+1/2'
'-x, -y, -z'
'x-1/2, -y-1/2, z-1/2'

_cell_length_a                   8.1316(3)
_cell_length_b                   10.8394(3)
_cell_length_c                   24.3849(7)
_cell_angle_alpha                90
_cell_angle_beta                 97.503(3)
_cell_angle_gamma                90
_cell_volume                     2130.92(12)
_cell_formula_units_Z            2
_cell_measurement_reflns_used    20320
_cell_measurement_temperature    170
_cell_measurement_theta_max      78.4060
_cell_measurement_theta_min      3.5480
_shelx_estimated_absorpt_T_max   0.845
_shelx_estimated_absorpt_T_min   0.421
_exptl_absorpt_coefficient_mu    3.482
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.44744
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
;
CrysAlisPro 1.171.40.53 (Rigaku Oxford Diffraction, 2019)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_absorpt_special_details   ?
_exptl_crystal_colour            'clear blue'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_primary    blue
_exptl_crystal_density_diffrn    1.459
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       prism
_exptl_crystal_F_000             970
_exptl_crystal_size_max          0.3
_exptl_crystal_size_mid          0.2
_exptl_crystal_size_min          0.05
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.1038
_diffrn_reflns_av_unetI/netI     0.0290
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 1.000
_diffrn_reflns_limit_h_max       8
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       29
_diffrn_reflns_limit_l_min       -29
_diffrn_reflns_number            79116
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 1.000
_diffrn_reflns_theta_full        66.595
_diffrn_reflns_theta_max         66.595
_diffrn_reflns_theta_min         3.657
_diffrn_ambient_temperature      170
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean ?
_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    176.08 270.68   1.10   10.00    -- -105.12 -59.25 -99.92   86
  2  ω   -136.76 -26.76   1.10   10.00    -- -105.12  83.74  10.05  100
  3  ω   -136.76 -26.76   1.10   10.00    -- -105.12  83.74 170.05  100
  4  ω      3.93  99.63   1.10   10.00    --   20.69  59.25 159.92   87
  5  ω    176.08 270.68   1.10   10.00    -- -105.12 -59.25 100.08   86
  6  ω    176.08 270.68   1.10   10.00    -- -105.12 -59.25-139.92   86
  7  ω    -26.23  72.77   1.10   10.00    --   50.69 -83.74  29.95   90
  8  ω   -136.76 -26.76   1.10   10.00    -- -105.12  83.74 -69.95  100
  9  ω    176.08 270.68   1.10   10.00    -- -105.12 -59.25  20.08   86
 10  ω    176.08 270.68   1.10   10.00    -- -105.12 -59.25 -59.92   86
 11  ω      3.93  99.63   1.10   10.00    --   20.69  59.25  69.92   87
 12  ω   -136.76 -26.76   1.10   10.00    -- -105.12  83.74-149.95  100
 13  ω   -136.76 -26.76   1.10   10.00    -- -105.12  83.74  90.05  100
 14  ω   -136.76 -26.76   1.10   10.00    -- -105.12  83.74 -29.95  100
 15  ω    176.08 270.68   1.10   10.00    -- -105.12 -59.25 140.08   86
 16  ω    176.08 271.78   1.10   10.00    -- -105.12 -59.25 -19.92   87
 17  ω    176.08 270.68   1.10   10.00    -- -105.12 -59.25-179.92   86
 18  ω   -136.76 -26.76   1.10   10.00    -- -105.12  83.74 130.05  100
 19  ω   -136.76 -26.76   1.10   10.00    -- -105.12  83.74-109.95  100
 20  ω   -136.76 -25.66   1.10   10.00    -- -105.12  83.74  50.05  101
 21  ω    -26.23  72.77   1.10   10.00    --   50.69 -83.74 131.95   90
 22  φ   -174.27   9.43   1.10   10.00 -25.56-105.12  31.50    --   167
 23  ω    191.08 285.68   1.10   10.00    --  -90.12 -59.25 -69.92   86
 24  ω    -26.23  72.77   1.10   10.00    --   50.69 -83.74-126.05   90
 25  φ    -64.08 118.52   1.10   10.00  33.24  50.69  59.25    --   166
 26  φ   -135.28 195.82   1.10   10.00 -96.36-105.12 -31.50    --   301
 27  ω      3.93  99.63   1.10   10.00    --   20.69  59.25-110.08   87
 28  φ    -47.92 135.78   1.10   10.00 -87.79-105.12 -59.25    --   167
 29  ω    191.08 285.68   1.10   10.00    --  -90.12 -59.25-159.92   86
 30  ω    191.08 285.68   1.10   10.00    --  -90.12 -59.25 110.08   86
 31  ω    -26.23  71.67   1.10   10.00    --   50.69 -83.74 -24.05   89
 32  φ   -339.92  19.78   1.10   10.00 -72.79 -90.12 -59.25    --   327
 33  ω     33.93 128.53   1.10   10.00    --   50.69  59.25 132.92   86
 34  ω    206.08 300.68   1.10   10.00    --  -75.12 -59.25 -69.92   86
 35  ω    -26.23  72.77   1.10   10.00    --   50.69 -83.74 -75.05   90
 36  ω    191.08 285.68   1.10   10.00    --  -90.12 -59.25  20.08   86
 37  φ   -339.92  19.78   1.10   10.00 -57.79 -75.12 -59.25    --   327
 38  φ   -339.92  19.78   1.10   10.00 -19.37  60.12 -59.25    --   327
;
_diffrn_measurement_device       'abstract diffractometer'
_diffrn_measurement_device_type  
'Saxi-CrysAlisPro-abstract goniometer imported SAXI images'
_diffrn_measurement_method       'ω and φ scans'
_diffrn_orient_matrix_type       
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      -0.0413081000
_diffrn_orient_matrix_UB_12      -0.0029148000
_diffrn_orient_matrix_UB_13      -0.0634490000
_diffrn_orient_matrix_UB_21      0.0051030000
_diffrn_orient_matrix_UB_22      -0.1420925000
_diffrn_orient_matrix_UB_23      0.0011856000
_diffrn_orient_matrix_UB_31      -0.1865055000
_diffrn_orient_matrix_UB_32      -0.0032149000
_diffrn_orient_matrix_UB_33      0.0055767000
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_source                   'fine-focus sealed X-ray tube'
_diffrn_source_type              'Enhance (Cu) X-ray Source'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                3237
_reflns_number_total             3763
_reflns_odcompleteness_completeness 98.56
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     78.73
_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
;
_reflns_threshold_expression     'I > 2σ(I)'
_computing_cell_refinement       'CrysAlisPro 1.171.40.53 (Rigaku OD, 2019)'
_computing_data_collection       'CrysAlisPro 1.171.40.53 (Rigaku OD, 2019)'
_computing_data_reduction        'CrysAlisPro 1.171.40.53 (Rigaku OD, 2019)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_computing_structure_solution    'ShelXT (Sheldrick, 2015)'
_refine_diff_density_max         0.391
_refine_diff_density_min         -0.571
_refine_diff_density_rms         0.084
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.072
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     277
_refine_ls_number_reflns         3763
_refine_ls_number_restraints     1
_refine_ls_R_factor_all          0.0595
_refine_ls_R_factor_gt           0.0526
_refine_ls_restrained_S_all      1.073
_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)+(0.0934P)²+1.4214P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1443
_refine_ls_wR_factor_ref         0.1532
_refine_special_details          ?
_olex2_refinement_description    
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups, All N(H) groups
 At 1.5 times of:
  All C(H,H,H) groups, All O(H) groups
2. Restrained distances
 O3A-C21A \\sim O3-C21
 with sigma of 0.02
3. Uiso/Uaniso restraints and constraints
Uanis(O3A) = Uanis(O3)
Uanis(C21A) = Uanis(C21)
4. Others
 Sof(O3A)=Sof(H3AA)=Sof(C21A)=Sof(H21D)=Sof(H21E)=Sof(H21F)=1-FVAR(1)
 Sof(O3)=Sof(H3A)=Sof(C21)=Sof(H21A)=Sof(H21B)=Sof(H21C)=FVAR(1)
5.a Riding coordinates:
 N3(H3)
5.b Secondary CH2 refined with riding coordinates:
 C2(H2A,H2B), C18(H18A,H18B), C19(H19A,H19B), C20(H20A,H20B)
5.c Aromatic/amide H refined with riding coordinates:
 C4(H4), C5(H5), C6(H6), C7(H7), C11(H11), C12(H12), C13(H13), C15(H15),
 C16(H16), C17(H17)
5.d Tetrahedral OH refined with riding coordinates:
 O3(H3A), O3A(H3AA)
5.e Idealised Me refined as rotating group:
 C21(H21A,H21B,H21C), C21A(H21D,H21E,H21F)
;
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     dual
_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
Cu1 Cu 0.500000 -0.500000 0.500000 0.0292(2) Uani 1 2 d S T P . .
Cl1 Cl 0.49743(11) -0.83537(8) 0.45739(3) 0.0520(3) Uani 1 1 d . . . . .
Cl2 Cl 0.34365(10) -0.84844(6) 0.23547(3) 0.0432(2) Uani 1 1 d . . . . .
O1 O 0.4955(2) -0.52958(18) 0.42069(8) 0.0349(4) Uani 1 1 d . . . . .
O2 O 0.6041(3) -0.34279(18) 0.41310(9) 0.0452(5) Uani 1 1 d . . . . .
N1 N 0.2740(3) -0.4297(2) 0.48569(9) 0.0327(5) Uani 1 1 d . . . . .
N2 N 0.0412(3) -0.3419(2) 0.50072(11) 0.0363(6) Uani 1 1 d . . . . .
N3 N 0.4688(3) -0.7285(2) 0.34258(9) 0.0323(5) Uani 1 1 d . . . . .
H3 H 0.449062 -0.686276 0.370861 0.039 Uiso 1 1 d R . . . .
C1 C 0.5550(4) -0.4427(3) 0.39309(11) 0.0345(6) Uani 1 1 d . . . . .
C2 C 0.5644(4) -0.4743(3) 0.33239(12) 0.0406(7) Uani 1 1 d . . . . .
H2A H 0.452057 -0.495775 0.314149 0.049 Uiso 1 1 calc R . . . .
H2B H 0.602486 -0.400801 0.313504 0.049 Uiso 1 1 calc R . . . .
C3 C 0.6811(4) -0.5809(3) 0.32601(11) 0.0376(7) Uani 1 1 d . . . . .
C4 C 0.8423(4) -0.5572(3) 0.31588(14) 0.0522(9) Uani 1 1 d . . . . .
H4 H 0.878164 -0.474158 0.313798 0.063 Uiso 1 1 calc R . . . .
C5 C 0.9520(5) -0.6518(4) 0.30876(17) 0.0610(10) Uani 1 1 d . . . . .
H5 H 1.062312 -0.633659 0.302496 0.073 Uiso 1 1 calc R . . . .
C6 C 0.8995(4) -0.7729(4) 0.31083(15) 0.0550(9) Uani 1 1 d . . . . .
H6 H 0.973205 -0.838056 0.304755 0.066 Uiso 1 1 calc R . . . .
C7 C 0.7397(4) -0.8002(3) 0.32175(13) 0.0430(7) Uani 1 1 d . . . . .
H7 H 0.704877 -0.883590 0.323577 0.052 Uiso 1 1 calc R . . . .
C8 C 0.6306(3) -0.7041(3) 0.33002(11) 0.0340(6) Uani 1 1 d . . . . .
C9 C 0.4155(3) -0.8517(2) 0.34669(11) 0.0314(6) Uani 1 1 d . . . . .
C10 C 0.4199(4) -0.9137(3) 0.39715(12) 0.0386(7) Uani 1 1 d . . . . .
C11 C 0.3639(4) -1.0325(3) 0.40126(14) 0.0461(8) Uani 1 1 d . . . . .
H11 H 0.368237 -1.071175 0.436383 0.055 Uiso 1 1 calc R . . . .
C12 C 0.3009(4) -1.0956(3) 0.35339(14) 0.0482(8) Uani 1 1 d . . . . .
H12 H 0.262687 -1.178002 0.355740 0.058 Uiso 1 1 calc R . . . .
C13 C 0.2938(4) -1.0384(3) 0.30225(13) 0.0410(7) Uani 1 1 d . . . . .
H13 H 0.250065 -1.080712 0.269450 0.049 Uiso 1 1 calc R . . . .
C14 C 0.3513(3) -0.9186(3) 0.29975(11) 0.0333(6) Uani 1 1 d . . . . .
C15 C 0.1725(4) -0.4178(3) 0.43622(12) 0.0391(7) Uani 1 1 d . . . . .
H15 H 0.199287 -0.443656 0.401228 0.047 Uiso 1 1 calc R . . . .
C16 C 0.0287(4) -0.3634(3) 0.44520(13) 0.0428(7) Uani 1 1 d . . . . .
H16 H -0.062810 -0.344048 0.418225 0.051 Uiso 1 1 calc R . . . .
C17 C 0.1893(3) -0.3825(3) 0.52358(12) 0.0356(6) Uani 1 1 d . . . . .
H17 H 0.228829 -0.378160 0.561954 0.043 Uiso 1 1 calc R . . . .
C18 C -0.0790(4) -0.2770(3) 0.53078(15) 0.0450(7) Uani 1 1 d . . . . .
H18A H -0.088288 -0.320715 0.565895 0.054 Uiso 1 1 calc R . . . .
H18B H -0.189437 -0.277792 0.508249 0.054 Uiso 1 1 calc R . . . .
C19 C -0.0258(5) -0.1451(3) 0.54308(16) 0.0512(8) Uani 1 1 d . . . . .
H19A H -0.099709 -0.108262 0.567849 0.061 Uiso 1 1 calc R . . . .
H19B H 0.088221 -0.145166 0.563095 0.061 Uiso 1 1 calc R . . . .
C20 C -0.0294(5) -0.0667(3) 0.49313(16) 0.0555(9) Uani 1 1 d . . . . .
H20A H -0.143902 -0.064511 0.473535 0.067 Uiso 1 1 calc R . . . .
H20B H 0.042702 -0.104098 0.467899 0.067 Uiso 1 1 calc R . . . .
O3 O 0.7147(8) -0.1175(5) 0.3577(3) 0.1051(18) Uani 0.799(7) 1 d D . . A 1
H3A H 0.646215 -0.175766 0.356654 0.158 Uiso 0.799(7) 1 calc R . . A 1
C21 C 0.8285(7) -0.1452(4) 0.3284(2) 0.0580(12) Uani 0.799(7) 1 d D . . A 1
H21A H 0.779146 -0.159749 0.290119 0.087 Uiso 0.799(7) 1 calc GR . . A 1
H21B H 0.885805 -0.219983 0.343206 0.087 Uiso 0.799(7) 1 calc GR . . A 1
H21C H 0.908142 -0.077065 0.329461 0.087 Uiso 0.799(7) 1 calc GR . . A 1
O3A O 0.769(4) -0.153(2) 0.3782(11) 0.1051(18) Uani 0.201(7) 1 d D . . A 2
H3AA H 0.668155 -0.155371 0.381923 0.158 Uiso 0.201(7) 1 calc R . . A 2
C21A C 0.801(3) -0.2374(17) 0.3483(8) 0.0580(12) Uani 0.201(7) 1 d D . . A 2
H21D H 0.834571 -0.203540 0.314238 0.087 Uiso 0.201(7) 1 calc GR . . A 2
H21E H 0.702272 -0.289087 0.339264 0.087 Uiso 0.201(7) 1 calc GR . . A 2
H21F H 0.891414 -0.287254 0.367400 0.087 Uiso 0.201(7) 1 calc GR . . 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
Cu1 O1 1.9558(19) 3_646 ?
Cu1 O1 1.9559(19) . ?
Cu1 N1 1.978(2) . ?
Cu1 N1 1.978(2) 3_646 ?
Cl1 C10 1.742(3) . ?
Cl2 C14 1.736(3) . ?
O1 C1 1.288(4) . ?
O2 C1 1.233(3) . ?
N1 C15 1.376(4) . ?
N1 C17 1.325(4) . ?
N2 C16 1.364(4) . ?
N2 C17 1.334(4) . ?
N2 C18 1.474(4) . ?
N3 C8 1.414(4) . ?
N3 C9 1.411(3) . ?
C1 C2 1.531(4) . ?
C2 C3 1.516(4) . ?
C3 C4 1.390(4) . ?
C3 C8 1.404(4) . ?
C4 C5 1.384(5) . ?
C5 C6 1.384(5) . ?
C6 C7 1.392(5) . ?
C7 C8 1.400(4) . ?
C9 C10 1.398(4) . ?
C9 C14 1.397(4) . ?
C10 C11 1.374(4) . ?
C11 C12 1.392(5) . ?
C12 C13 1.387(4) . ?
C13 C14 1.384(4) . ?
C15 C16 1.353(4) . ?
C18 C19 1.513(4) . ?
C19 C20 1.482(5) . ?
C20 C20 1.546(7) 3_556 ?
O3 C21 1.276(6) . ?
O3A C21A 1.213(17) . ?

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
O1 Cu1 O1 180.0 3_646 . ?
O1 Cu1 N1 89.52(9) 3_646 3_646 ?
O1 Cu1 N1 90.48(9) 3_646 . ?
O1 Cu1 N1 90.48(9) . 3_646 ?
O1 Cu1 N1 89.52(9) . . ?
N1 Cu1 N1 180.00(11) . 3_646 ?
C1 O1 Cu1 115.92(17) . . ?
C15 N1 Cu1 128.9(2) . . ?
C17 N1 Cu1 125.53(19) . . ?
C17 N1 C15 105.6(2) . . ?
C16 N2 C18 127.3(3) . . ?
C17 N2 C16 107.8(2) . . ?
C17 N2 C18 124.8(3) . . ?
C9 N3 C8 119.7(2) . . ?
O1 C1 C2 114.3(2) . . ?
O2 C1 O1 124.0(3) . . ?
O2 C1 C2 121.7(3) . . ?
C3 C2 C1 112.4(2) . . ?
C4 C3 C2 119.7(3) . . ?
C4 C3 C8 118.6(3) . . ?
C8 C3 C2 121.7(3) . . ?
C5 C4 C3 121.6(3) . . ?
C6 C5 C4 119.4(3) . . ?
C5 C6 C7 120.6(3) . . ?
C6 C7 C8 119.7(3) . . ?
C3 C8 N3 118.8(3) . . ?
C7 C8 N3 121.2(3) . . ?
C7 C8 C3 120.1(3) . . ?
C10 C9 N3 123.0(2) . . ?
C14 C9 N3 121.2(2) . . ?
C14 C9 C10 115.8(3) . . ?
C9 C10 Cl1 118.2(2) . . ?
C11 C10 Cl1 118.8(2) . . ?
C11 C10 C9 123.0(3) . . ?
C10 C11 C12 119.2(3) . . ?
C13 C12 C11 120.1(3) . . ?
C14 C13 C12 119.0(3) . . ?
C9 C14 Cl2 118.6(2) . . ?
C13 C14 Cl2 118.6(2) . . ?
C13 C14 C9 122.9(3) . . ?
C16 C15 N1 109.3(3) . . ?
C15 C16 N2 106.3(3) . . ?
N1 C17 N2 111.0(3) . . ?
N2 C18 C19 111.0(3) . . ?
C20 C19 C18 113.9(3) . . ?
C19 C20 C20 112.7(4) . 3_556 ?

_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
- Detector area scaling
;
_oxdiff_exptl_absorpt_empirical_full_max 1.824
_oxdiff_exptl_absorpt_empirical_full_min 0.668

# start Validation Reply Form
_vrf_PLAT977_cu_jnm034           
;
PROBLEM: Check Negative Difference Density on H21A             -0.31 eA-3  
RESPONSE: This H atom was introduced in a calculated position after the
methanol solvent was modeled using MSplit. It is not the result of an 
incorrect AFIX. There are also many G-level alerts about close contacts
that arose from modelling the disordered methanol.
;
_vrf_PLAT978_cu_jnm034           
;
PROBLEM: Number C-C Bonds with Positive Residual Density.          0 Info  
RESPONSE: This is exactly were we would like to the calculated residual 
density at the ?end? of refinement.
;
# end Validation Reply Form
####################################################################### 
# 
# 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_cu_jnm044
_database_code_depnum_ccdc_archive 'CCDC 2237931'
loop_
_audit_author_name
_audit_author_address
'Jennifer Murphy'
;University of Guelph
Canada
;
_audit_update_record             
;
2023-01-25 deposited with the CCDC.	2024-04-11 downloaded from the CCDC.
;
_audit_creation_date             2022-02-01
_audit_creation_method           
;
Olex2 1.5
(compiled 2021.12.09 svn.r5202d8cf for OlexSys, GUI svn.r6439)
;
_shelx_SHELXL_version_number     2017/1
_chemical_name_common            ?
_chemical_name_systematic        ?
_chemical_formula_moiety         'C39 H36 Cl4 N6 O4 Zn'
_chemical_formula_sum            'C39 H36 Cl4 N6 O4 Zn'
_chemical_formula_weight         859.91
_chemical_melting_point          ?
_chemical_oxdiff_formula         C39H36Cl4N6O4Zn
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0181 0.0091 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Cl Cl 0.3639 0.7018 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0311 0.0180 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0492 0.0322 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Zn Zn -1.5491 0.6778 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_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/n 1'
_space_group_name_Hall           '-P 2yn'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x+1/2, y+1/2, -z+1/2'
'-x, -y, -z'
'x-1/2, -y-1/2, z-1/2'

_cell_length_a                   15.7556(3)
_cell_length_b                   15.5699(3)
_cell_length_c                   16.1773(3)
_cell_angle_alpha                90
_cell_angle_beta                 109.828(2)
_cell_angle_gamma                90
_cell_volume                     3733.23(13)
_cell_formula_units_Z            4
_cell_measurement_reflns_used    81492
_cell_measurement_temperature    170
_cell_measurement_theta_max      78.2190
_cell_measurement_theta_min      2.8600
_shelx_estimated_absorpt_T_max   0.692
_shelx_estimated_absorpt_T_min   0.504
_exptl_absorpt_coefficient_mu    3.968
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.45619
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
;
CrysAlisPro 1.171.40.53 (Rigaku Oxford Diffraction, 2019)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_absorpt_special_details   ?
_exptl_crystal_colour            'clear colourless'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.530
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       plate
_exptl_crystal_F_000             1768
_exptl_crystal_size_max          0.2
_exptl_crystal_size_mid          0.2
_exptl_crystal_size_min          0.1
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.1289
_diffrn_reflns_av_unetI/netI     0.0268
_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       18
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            222774
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 1.000
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         68.249
_diffrn_reflns_theta_min         3.384
_diffrn_ambient_temperature      170.00
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean ?
_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  φ    -10.27 349.73   1.00   10.00 -25.56-105.12  31.50    --   360
  2  φ   -339.92  20.08   1.00   10.00 -57.79 -75.12 -59.25    --   360
  3  ω   -136.76 -25.76   1.00   10.00    -- -105.12  83.74  50.05  111
  4  ω   -136.76 -25.76   1.00   10.00    -- -105.12  83.74-109.95  111
  5  ω    -26.23  72.77   1.00   10.00    --   50.69 -83.74-126.05   99
  6  φ   -349.73  10.27   1.00   10.00 -96.36-105.12 -31.50    --   360
  7  ω      3.93  99.93   1.00   10.00    --   20.69  59.25 -20.08   96
  8  ω   -136.76 -25.76   1.00   10.00    -- -105.12  83.74 130.05  111
  9  ω    -26.23  72.77   1.00   10.00    --   50.69 -83.74  80.95   99
 10  ω      3.93  99.93   1.00   10.00    --   20.69  59.25 159.92   96
 11  φ   -339.92  20.08   1.00   10.00 -72.79 -90.12 -59.25    --   360
 12  ω   -136.76 -25.76   1.00   10.00    -- -105.12  83.74 -29.95  111
 13  ω   -136.76 -25.76   1.00   10.00    -- -105.12  83.74-149.95  111
 14  ω     33.93 129.93   1.00   10.00    --   50.69  59.25-125.08   96
 15  ω   -136.76 -25.76   1.00   10.00    -- -105.12  83.74  10.05  111
 16  ω   -136.76 -25.76   1.00   10.00    -- -105.12  83.74 170.05  111
 17  ω   -136.76 -25.76   1.00   10.00    -- -105.12  83.74  90.05  111
 18  ω   -136.76 -25.76   1.00   10.00    -- -105.12  83.74 -69.95  111
 19  ω     33.93 129.93   1.00   10.00    --   50.69  59.25  30.92   96
 20  ω     33.93 129.93   1.00   10.00    --   50.69  59.25 132.92   96
 21  ω     33.93 129.93   1.00   10.00    --   50.69  59.25-176.08   96
 22  ω     33.93 129.93   1.00   10.00    --   50.69  59.25 -20.08   96
 23  ω     33.94 129.94   1.00   10.00    --   50.69  59.25  81.92   96
 24  ω     33.93 129.93   1.00   10.00    --   50.69  59.25 -74.08   96
 25  ω    176.08 271.08   1.00   10.00    -- -105.12 -59.25 140.08   95
 26  ω    176.08 271.08   1.00   10.00    -- -105.12 -59.25  20.08   95
 27  φ   -339.92  20.08   1.00   10.00 -87.79-105.12 -59.25    --   360
 28  ω    176.08 271.08   1.00   10.00    -- -105.12 -59.25-139.92   95
 29  ω    176.08 271.08   1.00   10.00    -- -105.12 -59.25 -59.92   95
 30  ω    176.08 271.08   1.00   10.00    -- -105.12 -59.25  60.08   95
 31  ω    176.08 271.08   1.00   10.00    -- -105.12 -59.25 100.08   95
 32  ω      3.93  99.93   1.00   10.00    --   20.69  59.25  69.92   96
 33  ω    -26.23  72.77   1.00   10.00    --   50.69 -83.74 -24.05   99
 34  ω    176.08 271.08   1.00   10.00    -- -105.12 -59.25 -99.92   95
 35  ω      3.93  99.93   1.00   10.00    --   20.69  59.25-110.08   96
 36  ω    176.08 271.08   1.00   10.00    -- -105.12 -59.25-179.92   95
 37  ω     43.36 138.36   1.00   10.00    --   60.12  59.25 -20.08   95
 38  ω     43.36 138.36   1.00   10.00    --   60.12  59.25-110.08   95
 39  ω     18.93 114.93   1.00   10.00    --   35.69  59.25 159.92   96
 40  ω     43.36 138.36   1.00   10.00    --   60.12  59.25  69.92   95
 41  φ    -20.08 339.92   1.00   10.00  33.24  50.69  59.25    --   360
 42  ω    176.08 271.08   1.00   10.00    -- -105.12 -59.25 -19.92   95
 43  ω    191.08 286.08   1.00   10.00    --  -90.12 -59.25  20.08   95
 44  ω    191.08 286.08   1.00   10.00    --  -90.12 -59.25 110.08   95
 45  ω    191.08 286.08   1.00   10.00    --  -90.12 -59.25 -69.92   95
 46  ω    191.08 286.08   1.00   10.00    --  -90.12 -59.25-159.92   95
 47  ω    -26.23  72.77   1.00   10.00    --   50.69 -83.74 131.95   99
 48  ω     18.93 114.93   1.00   10.00    --   35.69  59.25-110.08   96
 49  ω    206.08 301.08   1.00   10.00    --  -75.12 -59.25 110.08   95
 50  ω    206.08 301.08   1.00   10.00    --  -75.12 -59.25-159.92   95
 51  ω     18.93 114.93   1.00   10.00    --   35.69  59.25  69.92   96
 52  ω    206.08 301.08   1.00   10.00    --  -75.12 -59.25 -69.92   95
 53  ω     43.36 138.36   1.00   10.00    --   60.12  59.25 159.92   95
 54  ω    206.08 301.08   1.00   10.00    --  -75.12 -59.25  20.08   95
 55  ω     18.93 114.93   1.00   10.00    --   35.69  59.25 -20.08   96
 56  ω    -26.23  72.77   1.00   10.00    --   50.69 -83.74 -75.05   99
 57  ω    -26.23  72.77   1.00   10.00    --   50.69 -83.74-177.05   99
 58  φ    -10.27 349.73   1.00   10.00  42.06  50.69  31.50    --   360
 59  ω    -26.23  72.77   1.00   10.00    --   50.69 -83.74  29.95   99
 60  φ    -10.27 349.73   1.00   10.00  42.06  50.69  31.50    --   360
;
_diffrn_measurement_device       'abstract diffractometer'
_diffrn_measurement_device_type  
'Saxi-CrysAlisPro-abstract goniometer imported SAXI images'
_diffrn_measurement_method       'ω and φ scans'
_diffrn_orient_matrix_type       
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      0.0687129000
_diffrn_orient_matrix_UB_12      -0.0032373000
_diffrn_orient_matrix_UB_13      -0.0486486000
_diffrn_orient_matrix_UB_21      0.0655383000
_diffrn_orient_matrix_UB_22      -0.0509855000
_diffrn_orient_matrix_UB_23      0.0767750000
_diffrn_orient_matrix_UB_31      -0.0421813000
_diffrn_orient_matrix_UB_32      -0.0848059000
_diffrn_orient_matrix_UB_33      -0.0445103000
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_source                   'fine-focus sealed X-ray tube'
_diffrn_source_type              'Enhance (Cu) X-ray Source'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                6186
_reflns_number_total             6828
_reflns_odcompleteness_completeness 99.57
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     78.94
_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
;
_reflns_threshold_expression     'I > 2σ(I)'
_computing_cell_refinement       'CrysAlisPro 1.171.40.53 (Rigaku OD, 2019)'
_computing_data_collection       'CrysAlisPro 1.171.40.53 (Rigaku OD, 2019)'
_computing_data_reduction        'CrysAlisPro 1.171.40.53 (Rigaku OD, 2019)'
_computing_molecular_graphics    'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL n/a (Sheldrick, 2015)'
_computing_structure_solution    'SHELXS  (Sheldrick, 2008)'
_refine_diff_density_max         0.801
_refine_diff_density_min         -0.577
_refine_diff_density_rms         0.095
_refine_ls_extinction_coef       0.00048(10)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4^
_refine_ls_extinction_method     'SHELXL-2017/1 (Sheldrick 2017)'
_refine_ls_goodness_of_fit_ref   1.059
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     496
_refine_ls_number_reflns         6828
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0580
_refine_ls_R_factor_gt           0.0542
_refine_ls_restrained_S_all      1.059
_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)+(0.1020P)²+2.5820P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1465
_refine_ls_wR_factor_ref         0.1519
_refine_special_details          ?
_olex2_refinement_description    
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
2.a Secondary CH2 refined with riding coordinates:
 C2(H2A,H2B), C16(H16A,H16B), C32(H32A,H32B), C33(H33A,H33B), C34(H34A,H34B),
 C35(H35A,H35B), C36(H36A,H36B)
2.b Aromatic/amide H refined with riding coordinates:
 C5(H5A), C6(H6A), C7(H7), C8(H8), C11(H11), C12(H12), C13(H13), C19(H19),
 C20(H20), C21(H21), C22(H22), C25(H25), C26(H26), C27(H27), C29(H29), C30(H30),
  C31(H31), C37(H37), C38(H38), C39(H39)
;
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     direct
_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
Zn1 Zn 0.56798(2) 0.26954(2) 0.50583(2) 0.02615(15) Uani 1 1 d . . . . .
Cl1 Cl 0.40658(4) 0.27754(4) 0.25980(4) 0.03414(19) Uani 1 1 d . . . . .
Cl2 Cl 0.57963(4) 0.41620(5) 0.05363(5) 0.03710(19) Uani 1 1 d . . . . .
Cl3 Cl 0.31221(5) 0.12238(5) 0.65918(5) 0.0445(2) Uani 1 1 d . . . . .
Cl4 Cl 0.59295(5) -0.06781(5) 0.86296(5) 0.0457(2) Uani 1 1 d . . . . .
O1 O 0.62712(12) 0.28362(12) 0.41411(13) 0.0320(4) Uani 1 1 d . . . . .
O2 O 0.70232(14) 0.37971(13) 0.51307(12) 0.0371(5) Uani 1 1 d . . . . .
O3 O 0.64338(13) 0.23898(13) 0.62549(13) 0.0333(4) Uani 1 1 d . . . . .
O4 O 0.51980(13) 0.23583(13) 0.66278(13) 0.0340(4) Uani 1 1 d . . . . .
N1 N 0.47955(14) 0.36654(14) 0.47668(14) 0.0271(5) Uani 1 1 d . . . . .
N2 N 0.39896(14) 0.47274(14) 0.39957(14) 0.0268(5) Uani 1 1 d . . . . .
N3 N 0.10406(14) 0.55446(14) 0.06030(14) 0.0264(5) Uani 1 1 d . . . . .
N4 N 0.00660(14) 0.66023(14) 0.03801(14) 0.0278(5) Uani 1 1 d . . . . .
N5 N 0.56202(15) 0.36478(15) 0.22750(16) 0.0298(5) Uani 1 1 d . . . . .
H5 H 0.568(3) 0.336(3) 0.272(3) 0.050(11) Uiso 1 1 d . . . . .
N6 N 0.50544(15) 0.09073(16) 0.76144(15) 0.0307(5) Uani 1 1 d . . . . .
H6 H 0.477(3) 0.130(3) 0.720(3) 0.057(11) Uiso 1 1 d . . . . .
C1 C 0.68441(17) 0.34563(17) 0.44068(17) 0.0294(6) Uani 1 1 d . . . . .
C2 C 0.72609(17) 0.37993(19) 0.37479(18) 0.0314(6) Uani 1 1 d . . . . .
H2A H 0.789783 0.396005 0.405863 0.038 Uiso 1 1 calc R . . . .
H2B H 0.724932 0.334637 0.331473 0.038 Uiso 1 1 calc R . . . .
C3 C 0.67415(17) 0.45747(18) 0.32780(17) 0.0289(5) Uani 1 1 d . . . . .
C4 C 0.59340(17) 0.44858(17) 0.25561(17) 0.0284(5) Uani 1 1 d . . . . .
C5 C 0.54690(19) 0.52143(18) 0.21434(19) 0.0318(6) Uani 1 1 d . . . . .
H5A H 0.493579 0.515320 0.164681 0.038 Uiso 1 1 calc R . . . .
C6 C 0.5777(2) 0.60316(19) 0.2451(2) 0.0370(6) Uani 1 1 d . . . . .
H6A H 0.544974 0.652516 0.217112 0.044 Uiso 1 1 calc R . . . .
C7 C 0.6563(2) 0.6122(2) 0.3166(2) 0.0421(7) Uani 1 1 d . . . . .
H7 H 0.677927 0.667738 0.337867 0.050 Uiso 1 1 calc R . . . .
C8 C 0.7030(2) 0.5401(2) 0.35673(19) 0.0371(6) Uani 1 1 d . . . . .
H8 H 0.756658 0.547072 0.405832 0.044 Uiso 1 1 calc R . . . .
C9 C 0.48626(17) 0.35064(16) 0.15257(17) 0.0278(5) Uani 1 1 d . . . . .
C10 C 0.48436(18) 0.37169(17) 0.06797(17) 0.0287(5) Uani 1 1 d . . . . .
C11 C 0.40941(19) 0.35758(19) -0.00615(18) 0.0328(6) Uani 1 1 d . . . . .
H11 H 0.410040 0.374298 -0.062416 0.039 Uiso 1 1 calc R . . . .
C12 C 0.33354(19) 0.31897(19) 0.00226(18) 0.0349(6) Uani 1 1 d . . . . .
H12 H 0.281693 0.309632 -0.048205 0.042 Uiso 1 1 calc R . . . .
C13 C 0.33346(18) 0.29401(18) 0.08438(19) 0.0320(6) Uani 1 1 d . . . . .
H13 H 0.282315 0.266018 0.090450 0.038 Uiso 1 1 calc R . . . .
C14 C 0.40832(17) 0.31017(16) 0.15727(17) 0.0280(5) Uani 1 1 d . . . . .
C15 C 0.60117(18) 0.22379(15) 0.67903(17) 0.0266(5) Uani 1 1 d . . . . .
C16 C 0.66095(18) 0.18530(18) 0.76640(17) 0.0308(6) Uani 1 1 d . . . . .
H16A H 0.674949 0.125469 0.754770 0.037 Uiso 1 1 calc R . . . .
H16B H 0.718653 0.217331 0.785211 0.037 Uiso 1 1 calc R . . . .
C17 C 0.62739(18) 0.18326(17) 0.84314(17) 0.0306(6) Uani 1 1 d . . . . .
C18 C 0.55306(18) 0.13390(17) 0.84102(17) 0.0301(6) Uani 1 1 d . . . . .
C19 C 0.5261(2) 0.1276(2) 0.9141(2) 0.0445(7) Uani 1 1 d . . . . .
H19 H 0.474642 0.094332 0.911502 0.053 Uiso 1 1 calc R . . . .
C20 C 0.5749(3) 0.1703(2) 0.9914(2) 0.0552(9) Uani 1 1 d . . . . .
H20 H 0.557013 0.166150 1.041696 0.066 Uiso 1 1 calc R . . . .
C21 C 0.6486(3) 0.2182(2) 0.9945(2) 0.0521(9) Uani 1 1 d . . . . .
H21 H 0.682012 0.246787 1.047432 0.063 Uiso 1 1 calc R . . . .
C22 C 0.6751(2) 0.22542(18) 0.9218(2) 0.0408(7) Uani 1 1 d . . . . .
H22 H 0.726233 0.259366 0.925121 0.049 Uiso 1 1 calc R . . . .
C23 C 0.44777(18) 0.02210(18) 0.75869(17) 0.0317(6) Uani 1 1 d . . . . .
C24 C 0.3563(2) 0.0247(2) 0.70818(18) 0.0349(6) Uani 1 1 d . . . . .
C25 C 0.2991(2) -0.0453(2) 0.6961(2) 0.0431(7) Uani 1 1 d . . . . .
H25 H 0.237453 -0.041053 0.660360 0.052 Uiso 1 1 calc R . . . .
C26 C 0.3341(2) -0.1216(2) 0.7375(2) 0.0461(8) Uani 1 1 d . . . . .
H26 H 0.296166 -0.170459 0.729957 0.055 Uiso 1 1 calc R . . . .
C27 C 0.4237(2) -0.1273(2) 0.7896(2) 0.0414(7) Uani 1 1 d . . . . .
H27 H 0.446951 -0.179903 0.818139 0.050 Uiso 1 1 calc R . . . .
C28 C 0.4799(2) -0.05681(19) 0.80027(18) 0.0355(6) Uani 1 1 d . . . . .
C29 C 0.47723(17) 0.43016(16) 0.42141(17) 0.0273(5) Uani 1 1 d . . . . .
H29 H 0.524897 0.443706 0.400133 0.033 Uiso 1 1 calc R . . . .
C30 C 0.39818(19) 0.36935(18) 0.49015(19) 0.0333(6) Uani 1 1 d . . . . .
H30 H 0.379982 0.331317 0.526927 0.040 Uiso 1 1 calc R . . . .
C31 C 0.34765(19) 0.43480(19) 0.4429(2) 0.0355(6) Uani 1 1 d . . . . .
H31 H 0.288695 0.451004 0.440382 0.043 Uiso 1 1 calc R . . . .
C32 C 0.37176(19) 0.54297(17) 0.33512(17) 0.0304(6) Uani 1 1 d . . . . .
H32A H 0.425750 0.575975 0.335929 0.036 Uiso 1 1 calc R . . . .
H32B H 0.330649 0.582449 0.351244 0.036 Uiso 1 1 calc R . . . .
C33 C 0.32447(19) 0.50772(17) 0.24323(17) 0.0317(6) Uani 1 1 d . . . . .
H33A H 0.364248 0.465405 0.228834 0.038 Uiso 1 1 calc R . . . .
H33B H 0.268615 0.477655 0.241777 0.038 Uiso 1 1 calc R . . . .
C34 C 0.30082(17) 0.57870(17) 0.17471(17) 0.0289(6) Uani 1 1 d . . . . .
H34A H 0.354703 0.615117 0.183565 0.035 Uiso 1 1 calc R . . . .
H34B H 0.253123 0.615265 0.183381 0.035 Uiso 1 1 calc R . . . .
C35 C 0.26814(17) 0.54478(18) 0.08055(17) 0.0305(6) Uani 1 1 d . . . . .
H35A H 0.314006 0.504537 0.073806 0.037 Uiso 1 1 calc R . . . .
H35B H 0.263977 0.593606 0.040163 0.037 Uiso 1 1 calc R . . . .
C36 C 0.17704(17) 0.49879(17) 0.05228(17) 0.0300(6) Uani 1 1 d . . . . .
H36A H 0.161409 0.479858 -0.009527 0.036 Uiso 1 1 calc R . . . .
H36B H 0.181914 0.446985 0.089093 0.036 Uiso 1 1 calc R . . . .
C37 C 0.06066(18) 0.54525(18) 0.12051(17) 0.0304(6) Uani 1 1 d . . . . .
H37 H 0.070799 0.501576 0.163794 0.036 Uiso 1 1 calc R . . . .
C38 C 0.00073(18) 0.61043(18) 0.10613(17) 0.0312(6) Uani 1 1 d . . . . .
H38 H -0.039107 0.620290 0.137991 0.037 Uiso 1 1 calc R . . . .
C39 C 0.06963(17) 0.62443(17) 0.01214(16) 0.0281(6) Uani 1 1 d . . . . .
H39 H 0.088007 0.645449 -0.034283 0.034 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
Zn1 O1 2.0138(19) . ?
Zn1 O3 1.9558(19) . ?
Zn1 N1 2.000(2) . ?
Zn1 N4 2.053(2) 2_545 ?
Cl1 C14 1.744(3) . ?
Cl2 C10 1.739(3) . ?
Cl3 C24 1.747(3) . ?
Cl4 C28 1.734(3) . ?
O1 C1 1.292(3) . ?
O2 C1 1.228(3) . ?
O3 C15 1.280(3) . ?
O4 C15 1.233(3) . ?
N1 C29 1.327(3) . ?
N1 C30 1.372(3) . ?
N2 C29 1.338(3) . ?
N2 C31 1.370(4) . ?
N2 C32 1.471(3) . ?
N3 C36 1.480(3) . ?
N3 C37 1.374(3) . ?
N3 C39 1.342(3) . ?
N4 C38 1.376(4) . ?
N4 C39 1.324(3) . ?
N5 H5 0.83(4) . ?
N5 C4 1.415(3) . ?
N5 C9 1.400(3) . ?
N6 H6 0.91(4) . ?
N6 C18 1.420(3) . ?
N6 C23 1.394(4) . ?
C1 C2 1.526(4) . ?
C2 H2A 0.9900 . ?
C2 H2B 0.9900 . ?
C2 C3 1.511(4) . ?
C3 C4 1.412(4) . ?
C3 C8 1.392(4) . ?
C4 C5 1.392(4) . ?
C5 H5A 0.9500 . ?
C5 C6 1.392(4) . ?
C6 H6A 0.9500 . ?
C6 C7 1.387(5) . ?
C7 H7 0.9500 . ?
C7 C8 1.377(5) . ?
C8 H8 0.9500 . ?
C9 C10 1.398(4) . ?
C9 C14 1.405(4) . ?
C10 C11 1.386(4) . ?
C11 H11 0.9500 . ?
C11 C12 1.385(4) . ?
C12 H12 0.9500 . ?
C12 C13 1.385(4) . ?
C13 H13 0.9500 . ?
C13 C14 1.379(4) . ?
C15 C16 1.530(4) . ?
C16 H16A 0.9900 . ?
C16 H16B 0.9900 . ?
C16 C17 1.506(4) . ?
C17 C18 1.391(4) . ?
C17 C22 1.403(4) . ?
C18 C19 1.389(4) . ?
C19 H19 0.9500 . ?
C19 C20 1.395(5) . ?
C20 H20 0.9500 . ?
C20 C21 1.365(6) . ?
C21 H21 0.9500 . ?
C21 C22 1.379(5) . ?
C22 H22 0.9500 . ?
C23 C24 1.395(4) . ?
C23 C28 1.410(4) . ?
C24 C25 1.385(4) . ?
C25 H25 0.9500 . ?
C25 C26 1.382(5) . ?
C26 H26 0.9500 . ?
C26 C27 1.380(5) . ?
C27 H27 0.9500 . ?
C27 C28 1.384(4) . ?
C29 H29 0.9500 . ?
C30 H30 0.9500 . ?
C30 C31 1.358(4) . ?
C31 H31 0.9500 . ?
C32 H32A 0.9900 . ?
C32 H32B 0.9900 . ?
C32 C33 1.521(4) . ?
C33 H33A 0.9900 . ?
C33 H33B 0.9900 . ?
C33 C34 1.519(4) . ?
C34 H34A 0.9900 . ?
C34 H34B 0.9900 . ?
C34 C35 1.527(4) . ?
C35 H35A 0.9900 . ?
C35 H35B 0.9900 . ?
C35 C36 1.529(4) . ?
C36 H36A 0.9900 . ?
C36 H36B 0.9900 . ?
C37 H37 0.9500 . ?
C37 C38 1.351(4) . ?
C38 H38 0.9500 . ?
C39 H39 0.9500 . ?

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
O1 Zn1 N4 100.92(8) . 2_545 ?
O3 Zn1 O1 118.57(8) . . ?
O3 Zn1 N1 123.91(9) . . ?
O3 Zn1 N4 102.98(8) . 2_545 ?
N1 Zn1 O1 101.74(8) . . ?
N1 Zn1 N4 105.86(9) . 2_545 ?
C1 O1 Zn1 106.38(17) . . ?
C15 O3 Zn1 115.72(16) . . ?
C29 N1 Zn1 125.49(18) . . ?
C29 N1 C30 105.6(2) . . ?
C30 N1 Zn1 126.90(18) . . ?
C29 N2 C31 107.6(2) . . ?
C29 N2 C32 125.2(2) . . ?
C31 N2 C32 127.0(2) . . ?
C37 N3 C36 126.1(2) . . ?
C39 N3 C36 126.7(2) . . ?
C39 N3 C37 107.2(2) . . ?
C38 N4 Zn1 123.90(18) . 2 ?
C39 N4 Zn1 129.97(18) . 2 ?
C39 N4 C38 106.1(2) . . ?
C4 N5 H5 108(3) . . ?
C9 N5 H5 118(3) . . ?
C9 N5 C4 121.7(2) . . ?
C18 N6 H6 109(3) . . ?
C23 N6 H6 110(3) . . ?
C23 N6 C18 122.0(2) . . ?
O1 C1 C2 116.6(2) . . ?
O2 C1 O1 123.3(3) . . ?
O2 C1 C2 120.0(2) . . ?
C1 C2 H2A 109.6 . . ?
C1 C2 H2B 109.6 . . ?
H2A C2 H2B 108.2 . . ?
C3 C2 C1 110.1(2) . . ?
C3 C2 H2A 109.6 . . ?
C3 C2 H2B 109.6 . . ?
C4 C3 C2 121.3(2) . . ?
C8 C3 C2 120.7(2) . . ?
C8 C3 C4 117.9(3) . . ?
C3 C4 N5 118.4(2) . . ?
C5 C4 N5 121.9(2) . . ?
C5 C4 C3 119.8(2) . . ?
C4 C5 H5A 119.6 . . ?
C4 C5 C6 120.7(3) . . ?
C6 C5 H5A 119.6 . . ?
C5 C6 H6A 120.2 . . ?
C7 C6 C5 119.7(3) . . ?
C7 C6 H6A 120.2 . . ?
C6 C7 H7 120.2 . . ?
C8 C7 C6 119.6(3) . . ?
C8 C7 H7 120.2 . . ?
C3 C8 H8 118.9 . . ?
C7 C8 C3 122.3(3) . . ?
C7 C8 H8 118.9 . . ?
N5 C9 C14 121.8(2) . . ?
C10 C9 N5 122.7(2) . . ?
C10 C9 C14 115.4(2) . . ?
C9 C10 Cl2 119.4(2) . . ?
C11 C10 Cl2 117.9(2) . . ?
C11 C10 C9 122.6(2) . . ?
C10 C11 H11 120.2 . . ?
C12 C11 C10 119.6(3) . . ?
C12 C11 H11 120.2 . . ?
C11 C12 H12 120.1 . . ?
C13 C12 C11 119.8(2) . . ?
C13 C12 H12 120.1 . . ?
C12 C13 H13 120.3 . . ?
C14 C13 C12 119.4(2) . . ?
C14 C13 H13 120.3 . . ?
C9 C14 Cl1 118.6(2) . . ?
C13 C14 Cl1 118.4(2) . . ?
C13 C14 C9 123.1(2) . . ?
O3 C15 C16 113.5(2) . . ?
O4 C15 O3 124.7(2) . . ?
O4 C15 C16 121.8(2) . . ?
C15 C16 H16A 107.5 . . ?
C15 C16 H16B 107.5 . . ?
H16A C16 H16B 107.0 . . ?
C17 C16 C15 119.4(2) . . ?
C17 C16 H16A 107.5 . . ?
C17 C16 H16B 107.5 . . ?
C18 C17 C16 121.3(2) . . ?
C18 C17 C22 117.9(3) . . ?
C22 C17 C16 120.6(3) . . ?
C17 C18 N6 117.7(2) . . ?
C19 C18 N6 121.2(3) . . ?
C19 C18 C17 121.1(3) . . ?
C18 C19 H19 120.2 . . ?
C18 C19 C20 119.6(3) . . ?
C20 C19 H19 120.2 . . ?
C19 C20 H20 120.1 . . ?
C21 C20 C19 119.9(3) . . ?
C21 C20 H20 120.1 . . ?
C20 C21 H21 119.6 . . ?
C20 C21 C22 120.8(3) . . ?
C22 C21 H21 119.6 . . ?
C17 C22 H22 119.6 . . ?
C21 C22 C17 120.8(3) . . ?
C21 C22 H22 119.6 . . ?
N6 C23 C24 122.0(3) . . ?
N6 C23 C28 121.9(2) . . ?
C24 C23 C28 115.9(3) . . ?
C23 C24 Cl3 117.6(2) . . ?
C25 C24 Cl3 118.8(2) . . ?
C25 C24 C23 123.6(3) . . ?
C24 C25 H25 120.8 . . ?
C26 C25 C24 118.3(3) . . ?
C26 C25 H25 120.8 . . ?
C25 C26 H26 119.7 . . ?
C27 C26 C25 120.6(3) . . ?
C27 C26 H26 119.7 . . ?
C26 C27 H27 119.9 . . ?
C26 C27 C28 120.2(3) . . ?
C28 C27 H27 119.9 . . ?
C23 C28 Cl4 119.8(2) . . ?
C27 C28 Cl4 118.8(2) . . ?
C27 C28 C23 121.4(3) . . ?
N1 C29 N2 111.1(2) . . ?
N1 C29 H29 124.4 . . ?
N2 C29 H29 124.4 . . ?
N1 C30 H30 125.2 . . ?
C31 C30 N1 109.6(2) . . ?
C31 C30 H30 125.2 . . ?
N2 C31 H31 127.0 . . ?
C30 C31 N2 106.1(2) . . ?
C30 C31 H31 127.0 . . ?
N2 C32 H32A 109.5 . . ?
N2 C32 H32B 109.5 . . ?
N2 C32 C33 110.7(2) . . ?
H32A C32 H32B 108.1 . . ?
C33 C32 H32A 109.5 . . ?
C33 C32 H32B 109.5 . . ?
C32 C33 H33A 109.3 . . ?
C32 C33 H33B 109.3 . . ?
H33A C33 H33B 108.0 . . ?
C34 C33 C32 111.6(2) . . ?
C34 C33 H33A 109.3 . . ?
C34 C33 H33B 109.3 . . ?
C33 C34 H34A 109.0 . . ?
C33 C34 H34B 109.0 . . ?
C33 C34 C35 113.1(2) . . ?
H34A C34 H34B 107.8 . . ?
C35 C34 H34A 109.0 . . ?
C35 C34 H34B 109.0 . . ?
C34 C35 H35A 108.5 . . ?
C34 C35 H35B 108.5 . . ?
C34 C35 C36 115.2(2) . . ?
H35A C35 H35B 107.5 . . ?
C36 C35 H35A 108.5 . . ?
C36 C35 H35B 108.5 . . ?
N3 C36 C35 112.2(2) . . ?
N3 C36 H36A 109.2 . . ?
N3 C36 H36B 109.2 . . ?
C35 C36 H36A 109.2 . . ?
C35 C36 H36B 109.2 . . ?
H36A C36 H36B 107.9 . . ?
N3 C37 H37 126.7 . . ?
C38 C37 N3 106.6(2) . . ?
C38 C37 H37 126.7 . . ?
N4 C38 H38 125.4 . . ?
C37 C38 N4 109.2(2) . . ?
C37 C38 H38 125.4 . . ?
N3 C39 H39 124.5 . . ?
N4 C39 N3 110.9(2) . . ?
N4 C39 H39 124.5 . . ?

# end Validation Reply Form
_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
- Detector area scaling
;
_oxdiff_exptl_absorpt_empirical_full_max 1.799
_oxdiff_exptl_absorpt_empirical_full_min 0.610
# start Validation Reply Form
_vrf_RINTA01_cu_jnm044           
;
PROBLEM: The value of Rint is greater than 0.12
RESPONSE: These were low quality crystals that did not result in
super satisfactory results despite many attempts to grow better crystals.
;
####################################################################### 
# 
# 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_cu_jnm038
_database_code_depnum_ccdc_archive 'CCDC 2237932'
loop_
_audit_author_name
_audit_author_address
'Jennifer Murphy'
;University of Guelph
Canada
;
_audit_update_record             
;
2023-01-25 deposited with the CCDC.	2024-04-11 downloaded from the CCDC.
;
_audit_creation_date             2020-02-18
_audit_creation_method           
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_shelx_SHELXL_version_number     2017/1
_chemical_name_common            ?
_chemical_name_systematic        ?
_chemical_formula_moiety         'C40 H38 Cl4 N6 O4 Zn, C H4 O'
_chemical_formula_sum            'C41 H42 Cl4 N6 O5 Zn'
_chemical_formula_weight         905.97
_chemical_melting_point          ?
_chemical_oxdiff_formula         ZnC41H40Cl4N4O6
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0181 0.0091 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Cl Cl 0.3639 0.7018 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0311 0.0180 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0492 0.0322 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Zn Zn -1.5491 0.6778 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_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/n 1'
_space_group_name_Hall           '-P 2yn'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x+1/2, y+1/2, -z+1/2'
'-x, -y, -z'
'x-1/2, -y-1/2, z-1/2'

_cell_length_a                   14.7461(3)
_cell_length_b                   14.5959(3)
_cell_length_c                   19.2358(3)
_cell_angle_alpha                90
_cell_angle_beta                 97.599(2)
_cell_angle_gamma                90
_cell_volume                     4103.81(14)
_cell_formula_units_Z            4
_cell_measurement_reflns_used    75342
_cell_measurement_temperature    170
_cell_measurement_theta_max      78.7240
_cell_measurement_theta_min      2.3640
_shelx_estimated_absorpt_T_max   0.528
_shelx_estimated_absorpt_T_min   0.322
_exptl_absorpt_coefficient_mu    3.657
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.41151
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
;
CrysAlisPro 1.171.40.53 (Rigaku Oxford Diffraction, 2019)
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    1.466
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       prism
_exptl_crystal_F_000             1872
_exptl_crystal_size_max          0.4
_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  0.1159
_diffrn_reflns_av_unetI/netI     0.0259
_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       -17
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_limit_l_min       -24
_diffrn_reflns_number            226781
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 1.000
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         74.498
_diffrn_reflns_theta_min         3.559
_diffrn_ambient_temperature      170
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean ?
_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   -136.76 -25.76   1.00    8.00    -- -105.12  83.74-109.95  111
  2  ω    176.08 271.08   1.00    8.00    -- -105.12 -59.25 -59.92   95
  3  ω    176.08 271.08   1.00    8.00    -- -105.12 -59.25 140.08   95
  4  φ   -339.92  20.08   1.00    8.00 -57.79 -75.12 -59.25    --   360
  5  ω    176.08 271.08   1.00    8.00    -- -105.12 -59.25  60.08   95
  6  ω   -136.76 -25.76   1.00    8.00    -- -105.12  83.74  50.05  111
  7  ω    176.08 271.08   1.00    8.00    -- -105.12 -59.25 -19.92   95
  8  ω    -26.23  72.77   1.00    8.00    --   50.69 -83.74  29.95   99
  9  ω    176.08 271.08   1.00    8.00    -- -105.12 -59.25-179.92   95
 10  ω    176.08 271.08   1.00    8.00    -- -105.12 -59.25  20.08   95
 11  ω      3.93  99.93   1.00    8.00    --   20.69  59.25  69.92   96
 12  ω    176.08 271.08   1.00    8.00    -- -105.12 -59.25 100.08   95
 13  ω    176.08 272.08   1.00    8.00    -- -105.12 -59.25 -99.92   96
 14  ω    -26.23  72.77   1.00    8.00    --   50.69 -83.74-126.05   99
 15  ω   -136.76 -25.76   1.00    8.00    -- -105.12  83.74 170.05  111
 16  ω     18.93 114.93   1.00    8.00    --   35.69  59.25 159.92   96
 17  ω   -136.76 -25.76   1.00    8.00    -- -105.12  83.74  10.05  111
 18  φ   -339.92  20.08   1.00    8.00 -87.79-105.12 -59.25    --   360
 19  ω   -136.76 -25.76   1.00    8.00    -- -105.12  83.74 130.05  111
 20  ω   -136.76 -25.76   1.00    8.00    -- -105.12  83.74 -29.95  111
 21  ω     33.93 129.93   1.00    8.00    --   50.69  59.25 -74.08   96
 22  ω   -136.76 -25.76   1.00    8.00    -- -105.12  83.74  90.05  111
 23  ω   -136.76 -25.76   1.00    8.00    -- -105.12  83.74 -69.95  111
 24  ω   -136.76 -25.76   1.00    8.00    -- -105.12  83.74-149.95  111
 25  ω      3.93  99.93   1.00    8.00    --   20.69  59.25-110.08   96
 26  φ    -10.27 349.73   1.00    8.00 -25.56-105.12  31.50    --   360
 27  φ   -339.92  20.08   1.00    8.00 -72.79 -90.12 -59.25    --   360
 28  ω     33.93 129.93   1.00    8.00    --   50.69  59.25 -20.08   96
 29  φ   -349.73  10.27   1.00    8.00 -96.36-105.12 -31.50    --   360
 30  ω     33.93 129.93   1.00    8.00    --   50.69  59.25-176.08   96
 31  ω     33.93 129.93   1.00    8.00    --   50.69  59.25-125.08   96
 32  ω     33.93 129.93   1.00    8.00    --   50.69  59.25  30.92   96
 33  ω     33.93 129.93   1.00    8.00    --   50.69  59.25  81.92   96
 34  ω      3.93  99.93   1.00    8.00    --   20.69  59.25 -20.08   96
 35  ω     33.93 129.93   1.00    8.00    --   50.69  59.25 132.92   96
 36  ω     43.36 138.36   1.00    8.00    --   60.12  59.25-110.08   95
 37  ω     43.36 138.36   1.00    8.00    --   60.12  59.25 -20.08   95
 38  ω    -26.23  72.77   1.00    8.00    --   50.69 -83.74 131.95   99
 39  ω     43.36 138.36   1.00    8.00    --   60.12  59.25  69.92   95
 40  ω     18.93 114.93   1.00    8.00    --   35.69  59.25 -20.08   96
 41  ω    191.08 286.08   1.00    8.00    --  -90.12 -59.25-159.92   95
 42  ω    191.08 286.08   1.00    8.00    --  -90.12 -59.25 110.08   95
 43  ω    191.08 286.08   1.00    8.00    --  -90.12 -59.25  20.08   95
 44  ω    191.08 287.08   1.00    8.00    --  -90.12 -59.25 -69.92   96
 45  ω    -26.23  72.77   1.00    8.00    --   50.69 -83.74  80.95   99
 46  ω     18.93 114.93   1.00    8.00    --   35.69  59.25  69.92   96
 47  ω     18.93 114.93   1.00    8.00    --   35.69  59.25-110.08   96
 48  ω     43.36 138.36   1.00    8.00    --   60.12  59.25 159.92   95
 49  ω    206.08 301.08   1.00    8.00    --  -75.12 -59.25 110.08   95
 50  ω      3.93  99.93   1.00    8.00    --   20.69  59.25 159.92   96
 51  ω    206.08 301.08   1.00    8.00    --  -75.12 -59.25-159.92   95
 52  ω    206.08 301.08   1.00    8.00    --  -75.12 -59.25  20.08   95
 53  φ    -20.08 339.92   1.00    8.00  33.24  50.69  59.25    --   360
 54  ω    206.08 301.08   1.00    8.00    --  -75.12 -59.25 -69.92   95
 55  φ    -10.27 349.73   1.00    8.00  42.06  50.69  31.50    --   360
;
_diffrn_measurement_device       'abstract diffractometer'
_diffrn_measurement_device_type  
'Saxi-CrysAlisPro-abstract goniometer imported SAXI images'
_diffrn_measurement_method       'ω and φ scans'
_diffrn_orient_matrix_type       
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      -0.0161702000
_diffrn_orient_matrix_UB_12      -0.0328216000
_diffrn_orient_matrix_UB_13      -0.0767294000
_diffrn_orient_matrix_UB_21      0.0297899000
_diffrn_orient_matrix_UB_22      0.0945288000
_diffrn_orient_matrix_UB_23      -0.0244427000
_diffrn_orient_matrix_UB_31      0.0998480000
_diffrn_orient_matrix_UB_32      -0.0335742000
_diffrn_orient_matrix_UB_33      0.0061467000
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_source                   'fine-focus sealed X-ray tube'
_diffrn_source_type              'Enhance (Cu) X-ray Source'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                7625
_reflns_number_total             8387
_reflns_odcompleteness_completeness 99.55
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     78.98
_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
;
_reflns_threshold_expression     'I > 2σ(I)'
_computing_cell_refinement       'CrysAlisPro 1.171.40.53 (Rigaku OD, 2019)'
_computing_data_collection       'CrysAlisPro 1.171.40.53 (Rigaku OD, 2019)'
_computing_data_reduction        'CrysAlisPro 1.171.40.53 (Rigaku OD, 2019)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_computing_structure_solution    'ShelXT (Sheldrick, 2015)'
_refine_diff_density_max         0.454
_refine_diff_density_min         -0.831
_refine_diff_density_rms         0.109
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.027
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     524
_refine_ls_number_reflns         8387
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0561
_refine_ls_R_factor_gt           0.0524
_refine_ls_restrained_S_all      1.027
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0921P)²+3.1411P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1407
_refine_ls_wR_factor_ref         0.1450
_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, All O(H) groups
2.a Secondary CH2 refined with riding coordinates:
 C2(H2A,H2B), C16(H16A,H16B), C32(H32A,H32B), C33(H33A,H33B), C34(H34A,H34B),
 C38(H38A,H38B), C39(H39A,H39B), C40(H40A,H40B)
2.b Aromatic/amide H refined with riding coordinates:
 C3(H3), C4(H4), C5(H5A), C6(H6A), C11(H11), C12(H12), C13(H13), C18(H18),
 C19(H19), C20(H20), C21(H21), C25(H25), C26(H26), C27(H27), C29(H29), C30(H30),
  C31(H31), C35(H35), C36(H36), C37(H37)
2.c Idealised Me refined as rotating group:
 C41(H41A,H41B,H41C)
2.d Idealised tetrahedral OH refined as rotating group:
 O5(H5B)
;
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     dual
_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
Zn1 Zn 0.74398(2) 0.31006(2) 0.75161(2) 0.02612(11) Uani 1 1 d . . . . .
Cl1 Cl 0.41780(5) 0.06936(5) 0.74785(4) 0.04635(18) Uani 1 1 d . . . . .
Cl2 Cl 0.29422(5) 0.22065(5) 0.49590(4) 0.04994(19) Uani 1 1 d . . . . .
Cl3 Cl 0.72425(4) 0.30079(4) 0.53697(3) 0.03849(16) Uani 1 1 d . . . . .
Cl4 Cl 1.05593(5) 0.21592(5) 0.46408(4) 0.04315(17) Uani 1 1 d . . . . .
O1 O 0.85090(12) 0.30251(12) 0.69626(9) 0.0330(4) Uani 1 1 d . . . . .
O2 O 0.92830(14) 0.29156(13) 0.80226(9) 0.0409(4) Uani 1 1 d . . . . .
O3 O 0.64620(11) 0.34488(11) 0.67644(8) 0.0311(3) Uani 1 1 d . . . . .
O4 O 0.53732(12) 0.31363(13) 0.74328(9) 0.0366(4) Uani 1 1 d . . . . .
N1 N 0.72730(14) 0.19109(13) 0.79965(10) 0.0289(4) Uani 1 1 d . . . . .
N2 N 0.66356(15) 0.08193(14) 0.85459(10) 0.0328(4) Uani 1 1 d . . . . .
N3 N 0.75735(13) 0.42518(13) 0.80858(10) 0.0290(4) Uani 1 1 d . . . . .
N4 N 0.82064(14) 0.55298(13) 0.85100(10) 0.0287(4) Uani 1 1 d . . . . .
N5 N 0.91836(15) 0.24609(14) 0.56752(11) 0.0327(4) Uani 1 1 d . . . . .
N6 N 0.39125(14) 0.22354(14) 0.64429(12) 0.0331(4) Uani 1 1 d . . . . .
C1 C 0.92504(17) 0.29352(16) 0.73775(13) 0.0323(5) Uani 1 1 d . . . . .
C2 C 1.01174(17) 0.28356(18) 0.70373(14) 0.0355(5) Uani 1 1 d . . . . .
H2A H 1.013440 0.332013 0.667912 0.043 Uiso 1 1 calc R . . . .
H2B H 1.065681 0.291693 0.739713 0.043 Uiso 1 1 calc R . . . .
C3 C 1.06548(19) 0.1196(2) 0.70566(14) 0.0414(6) Uani 1 1 d . . . . .
H3 H 1.096427 0.130376 0.751457 0.050 Uiso 1 1 calc R . . . .
C4 C 1.0699(2) 0.0338(2) 0.67609(16) 0.0473(7) Uani 1 1 d . . . . .
H4 H 1.104260 -0.013621 0.701096 0.057 Uiso 1 1 calc R . . . .
C5 C 1.0242(2) 0.01744(18) 0.60994(15) 0.0422(6) Uani 1 1 d . . . . .
H5A H 1.027079 -0.041476 0.589367 0.051 Uiso 1 1 calc R . . . .
C6 C 0.97391(18) 0.08663(18) 0.57331(14) 0.0363(5) Uani 1 1 d . . . . .
H6A H 0.941645 0.074423 0.528184 0.044 Uiso 1 1 calc R . . . .
C7 C 0.97046(16) 0.17389(17) 0.60231(13) 0.0313(5) Uani 1 1 d . . . . .
C8 C 1.01648(17) 0.19097(17) 0.66975(13) 0.0329(5) Uani 1 1 d . . . . .
C9 C 0.88411(17) 0.24571(16) 0.49645(12) 0.0319(5) Uani 1 1 d . . . . .
C10 C 0.79282(18) 0.27018(16) 0.47358(13) 0.0331(5) Uani 1 1 d . . . . .
C11 C 0.7555(2) 0.27240(18) 0.40335(14) 0.0395(6) Uani 1 1 d . . . . .
H11 H 0.693386 0.289401 0.390151 0.047 Uiso 1 1 calc R . . . .
C12 C 0.8108(2) 0.24922(19) 0.35273(14) 0.0440(6) Uani 1 1 d . . . . .
H12 H 0.785825 0.247682 0.304619 0.053 Uiso 1 1 calc R . . . .
C13 C 0.9021(2) 0.22843(19) 0.37236(14) 0.0414(6) Uani 1 1 d . . . . .
H13 H 0.940040 0.213596 0.337692 0.050 Uiso 1 1 calc R . . . .
C14 C 0.93848(18) 0.22923(17) 0.44290(14) 0.0357(5) Uani 1 1 d . . . . .
C15 C 0.56285(16) 0.34490(15) 0.68912(11) 0.0274(4) Uani 1 1 d . . . . .
C16 C 0.49618(16) 0.38413(18) 0.63036(13) 0.0332(5) Uani 1 1 d . . . . .
H16A H 0.516587 0.447005 0.620918 0.040 Uiso 1 1 calc R . . . .
H16B H 0.500789 0.347365 0.587725 0.040 Uiso 1 1 calc R . . . .
C17 C 0.39668(16) 0.38890(16) 0.64035(12) 0.0290(5) Uani 1 1 d . . . . .
C18 C 0.35282(17) 0.47305(17) 0.64186(13) 0.0347(5) Uani 1 1 d . . . . .
H18 H 0.387288 0.527803 0.640144 0.042 Uiso 1 1 calc R . . . .
C19 C 0.26011(19) 0.47867(19) 0.64582(15) 0.0422(6) Uani 1 1 d . . . . .
H19 H 0.231308 0.536817 0.646527 0.051 Uiso 1 1 calc R . . . .
C20 C 0.20952(19) 0.3997(2) 0.64874(16) 0.0441(6) Uani 1 1 d . . . . .
H20 H 0.145762 0.403540 0.651398 0.053 Uiso 1 1 calc R . . . .
C21 C 0.25132(18) 0.31461(18) 0.64781(15) 0.0375(6) Uani 1 1 d . . . . .
H21 H 0.216268 0.260262 0.649639 0.045 Uiso 1 1 calc R . . . .
C22 C 0.34484(16) 0.30922(16) 0.64417(13) 0.0297(5) Uani 1 1 d . . . . .
C23 C 0.34530(16) 0.14270(16) 0.62343(13) 0.0321(5) Uani 1 1 d . . . . .
C24 C 0.35102(18) 0.06435(17) 0.66568(14) 0.0354(5) Uani 1 1 d . . . . .
C25 C 0.3084(2) -0.01768(19) 0.64506(16) 0.0428(6) Uani 1 1 d . . . . .
H25 H 0.314377 -0.069344 0.675355 0.051 Uiso 1 1 calc R . . . .
C26 C 0.2569(2) -0.0231(2) 0.57972(17) 0.0475(7) Uani 1 1 d . . . . .
H26 H 0.225801 -0.078307 0.565375 0.057 Uiso 1 1 calc R . . . .
C27 C 0.2506(2) 0.0517(2) 0.53513(16) 0.0446(6) Uani 1 1 d . . . . .
H27 H 0.215397 0.047744 0.490160 0.054 Uiso 1 1 calc R . . . .
C28 C 0.29576(18) 0.13243(18) 0.55612(14) 0.0373(5) Uani 1 1 d . . . . .
C29 C 0.78968(18) 0.12064(17) 0.81412(13) 0.0349(5) Uani 1 1 d . . . . .
H29 H 0.850117 0.119920 0.802086 0.042 Uiso 1 1 calc R . . . .
C30 C 0.75085(19) 0.05279(18) 0.84820(14) 0.0372(6) Uani 1 1 d . . . . .
H30 H 0.778322 -0.003491 0.864389 0.045 Uiso 1 1 calc R . . . .
C31 C 0.65233(17) 0.16433(17) 0.82484(12) 0.0316(5) Uani 1 1 d . . . . .
H31 H 0.597629 0.199299 0.822080 0.038 Uiso 1 1 calc R . . . .
C32 C 0.59471(19) 0.0319(2) 0.88830(13) 0.0406(6) Uani 1 1 d . . . . .
H32A H 0.587206 -0.030155 0.867529 0.049 Uiso 1 1 calc R . . . .
H32B H 0.535278 0.063957 0.878175 0.049 Uiso 1 1 calc R . . . .
C33 C 0.61887(18) 0.02297(19) 0.96663(13) 0.0378(6) Uani 1 1 d . . . . .
H33A H 0.628013 0.084802 0.987535 0.045 Uiso 1 1 calc R . . . .
H33B H 0.677175 -0.011043 0.977000 0.045 Uiso 1 1 calc R . . . .
C34 C 0.54437(18) -0.02694(18) 1.00030(14) 0.0381(6) Uani 1 1 d . . . . .
H34A H 0.530463 -0.085578 0.975271 0.046 Uiso 1 1 calc R . . . .
H34B H 0.568573 -0.041695 1.049499 0.046 Uiso 1 1 calc R . . . .
C35 C 0.83435(16) 0.47283(16) 0.82078(12) 0.0301(5) Uani 1 1 d . . . . .
H35 H 0.891834 0.452520 0.809475 0.036 Uiso 1 1 calc R . . . .
C36 C 0.69120(17) 0.47854(18) 0.83256(12) 0.0338(5) Uani 1 1 d . . . . .
H36 H 0.628508 0.462525 0.830884 0.041 Uiso 1 1 calc R . . . .
C37 C 0.72968(18) 0.55756(18) 0.85896(13) 0.0350(5) Uani 1 1 d . . . . .
H37 H 0.699583 0.606537 0.879040 0.042 Uiso 1 1 calc R . . . .
C38 C 0.89244(17) 0.61933(16) 0.87563(13) 0.0320(5) Uani 1 1 d . . . . .
H38A H 0.866205 0.681855 0.872252 0.038 Uiso 1 1 calc R . . . .
H38B H 0.941082 0.616494 0.844812 0.038 Uiso 1 1 calc R . . . .
C39 C 0.93447(17) 0.60118(16) 0.95126(13) 0.0330(5) Uani 1 1 d . . . . .
H39A H 0.982347 0.647664 0.965115 0.040 Uiso 1 1 calc R . . . .
H39B H 0.886480 0.608600 0.982274 0.040 Uiso 1 1 calc R . . . .
C40 C 0.97644(17) 0.50640(16) 0.96263(12) 0.0325(5) Uani 1 1 d . . . . .
H40A H 1.021550 0.496982 0.929484 0.039 Uiso 1 1 calc R . . . .
H40B H 0.927870 0.459622 0.952487 0.039 Uiso 1 1 calc R . . . .
O5 O 0.53225(18) 0.3354(2) 0.37837(12) 0.0661(7) Uani 1 1 d . . . . .
H5B H 0.509191 0.286974 0.360144 0.099 Uiso 1 1 calc GR . . . .
C41 C 0.4998(2) 0.3504(3) 0.44233(16) 0.0571(8) Uani 1 1 d . . . . .
H41A H 0.434658 0.366227 0.433859 0.086 Uiso 1 1 calc GR . . . .
H41B H 0.533938 0.400896 0.467127 0.086 Uiso 1 1 calc GR . . . .
H41C H 0.507924 0.294732 0.470935 0.086 Uiso 1 1 calc GR . . . .
H5 H 0.8792(18) 0.2719(18) 0.5954(14) 0.024(6) Uiso 1 1 d . . . . .
H6 H 0.435(3) 0.221(2) 0.6826(19) 0.052(9) Uiso 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
Zn1 O1 2.0187(17) . ?
Zn1 O3 1.9689(17) . ?
Zn1 N1 1.9976(19) . ?
Zn1 N3 2.0015(19) . ?
Cl1 C24 1.750(3) . ?
Cl2 C28 1.730(3) . ?
Cl3 C10 1.742(3) . ?
Cl4 C14 1.737(3) . ?
O1 C1 1.272(3) . ?
O2 C1 1.236(3) . ?
O3 C15 1.284(3) . ?
O4 C15 1.241(3) . ?
N1 C29 1.383(3) . ?
N1 C31 1.323(3) . ?
N2 C30 1.376(3) . ?
N2 C31 1.333(3) . ?
N2 C32 1.469(3) . ?
N3 C35 1.326(3) . ?
N3 C36 1.375(3) . ?
N4 C35 1.334(3) . ?
N4 C37 1.372(3) . ?
N4 C38 1.467(3) . ?
N5 C7 1.419(3) . ?
N5 C9 1.393(3) . ?
N5 H5 0.92(3) . ?
N6 C22 1.425(3) . ?
N6 C23 1.393(3) . ?
N6 H6 0.91(4) . ?
C1 C2 1.518(3) . ?
C2 H2A 0.9900 . ?
C2 H2B 0.9900 . ?
C2 C8 1.507(4) . ?
C3 H3 0.9500 . ?
C3 C4 1.381(4) . ?
C3 C8 1.397(4) . ?
C4 H4 0.9500 . ?
C4 C5 1.380(4) . ?
C5 H5A 0.9500 . ?
C5 C6 1.388(4) . ?
C6 H6A 0.9500 . ?
C6 C7 1.394(4) . ?
C7 C8 1.405(4) . ?
C9 C10 1.406(4) . ?
C9 C14 1.407(3) . ?
C10 C11 1.390(4) . ?
C11 H11 0.9500 . ?
C11 C12 1.393(4) . ?
C12 H12 0.9500 . ?
C12 C13 1.383(4) . ?
C13 H13 0.9500 . ?
C13 C14 1.391(4) . ?
C15 C16 1.509(3) . ?
C16 H16A 0.9900 . ?
C16 H16B 0.9900 . ?
C16 C17 1.506(3) . ?
C17 C18 1.390(3) . ?
C17 C22 1.399(3) . ?
C18 H18 0.9500 . ?
C18 C19 1.382(4) . ?
C19 H19 0.9500 . ?
C19 C20 1.378(4) . ?
C20 H20 0.9500 . ?
C20 C21 1.388(4) . ?
C21 H21 0.9500 . ?
C21 C22 1.392(4) . ?
C23 C24 1.399(4) . ?
C23 C28 1.408(4) . ?
C24 C25 1.386(4) . ?
C25 H25 0.9500 . ?
C25 C26 1.382(4) . ?
C26 H26 0.9500 . ?
C26 C27 1.384(4) . ?
C27 H27 0.9500 . ?
C27 C28 1.387(4) . ?
C29 H29 0.9500 . ?
C29 C30 1.356(4) . ?
C30 H30 0.9500 . ?
C31 H31 0.9500 . ?
C32 H32A 0.9900 . ?
C32 H32B 0.9900 . ?
C32 C33 1.507(3) . ?
C33 H33A 0.9900 . ?
C33 H33B 0.9900 . ?
C33 C34 1.531(3) . ?
C34 C34 1.526(5) 3_657 ?
C34 H34A 0.9900 . ?
C34 H34B 0.9900 . ?
C35 H35 0.9500 . ?
C36 H36 0.9500 . ?
C36 C37 1.354(4) . ?
C37 H37 0.9500 . ?
C38 H38A 0.9900 . ?
C38 H38B 0.9900 . ?
C38 C39 1.527(3) . ?
C39 H39A 0.9900 . ?
C39 H39B 0.9900 . ?
C39 C40 1.520(3) . ?
C40 C40 1.523(5) 3_767 ?
C40 H40A 0.9900 . ?
C40 H40B 0.9900 . ?
O5 H5B 0.8400 . ?
O5 C41 1.396(4) . ?
C41 H41A 0.9800 . ?
C41 H41B 0.9800 . ?
C41 H41C 0.9800 . ?

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
O3 Zn1 O1 100.02(7) . . ?
O3 Zn1 N1 116.18(8) . . ?
O3 Zn1 N3 101.24(8) . . ?
N1 Zn1 O1 110.43(8) . . ?
N1 Zn1 N3 119.06(8) . . ?
N3 Zn1 O1 107.90(8) . . ?
C1 O1 Zn1 109.95(15) . . ?
C15 O3 Zn1 119.14(14) . . ?
C29 N1 Zn1 128.31(17) . . ?
C31 N1 Zn1 125.87(17) . . ?
C31 N1 C29 105.8(2) . . ?
C30 N2 C32 126.5(2) . . ?
C31 N2 C30 107.8(2) . . ?
C31 N2 C32 125.7(2) . . ?
C35 N3 Zn1 123.88(16) . . ?
C35 N3 C36 105.8(2) . . ?
C36 N3 Zn1 129.52(17) . . ?
C35 N4 C37 107.4(2) . . ?
C35 N4 C38 125.1(2) . . ?
C37 N4 C38 127.4(2) . . ?
C7 N5 H5 111.8(16) . . ?
C9 N5 C7 124.3(2) . . ?
C9 N5 H5 113.6(16) . . ?
C22 N6 H6 109(2) . . ?
C23 N6 C22 121.8(2) . . ?
C23 N6 H6 117(2) . . ?
O1 C1 C2 116.3(2) . . ?
O2 C1 O1 123.3(2) . . ?
O2 C1 C2 120.5(2) . . ?
C1 C2 H2A 109.4 . . ?
C1 C2 H2B 109.4 . . ?
H2A C2 H2B 108.0 . . ?
C8 C2 C1 111.3(2) . . ?
C8 C2 H2A 109.4 . . ?
C8 C2 H2B 109.4 . . ?
C4 C3 H3 119.3 . . ?
C4 C3 C8 121.5(3) . . ?
C8 C3 H3 119.3 . . ?
C3 C4 H4 120.2 . . ?
C5 C4 C3 119.5(3) . . ?
C5 C4 H4 120.2 . . ?
C4 C5 H5A 119.8 . . ?
C4 C5 C6 120.3(3) . . ?
C6 C5 H5A 119.8 . . ?
C5 C6 H6A 119.8 . . ?
C5 C6 C7 120.5(3) . . ?
C7 C6 H6A 119.8 . . ?
C6 C7 N5 122.4(2) . . ?
C6 C7 C8 119.5(2) . . ?
C8 C7 N5 118.0(2) . . ?
C3 C8 C2 120.3(2) . . ?
C3 C8 C7 118.7(2) . . ?
C7 C8 C2 121.0(2) . . ?
N5 C9 C10 120.9(2) . . ?
N5 C9 C14 123.4(2) . . ?
C10 C9 C14 115.4(2) . . ?
C9 C10 Cl3 117.80(19) . . ?
C11 C10 Cl3 118.8(2) . . ?
C11 C10 C9 123.4(2) . . ?
C10 C11 H11 120.6 . . ?
C10 C11 C12 118.7(3) . . ?
C12 C11 H11 120.6 . . ?
C11 C12 H12 119.9 . . ?
C13 C12 C11 120.1(3) . . ?
C13 C12 H12 119.9 . . ?
C12 C13 H13 120.0 . . ?
C12 C13 C14 120.0(3) . . ?
C14 C13 H13 120.0 . . ?
C9 C14 Cl4 119.6(2) . . ?
C13 C14 Cl4 118.1(2) . . ?
C13 C14 C9 122.1(3) . . ?
O3 C15 C16 113.75(19) . . ?
O4 C15 O3 124.3(2) . . ?
O4 C15 C16 121.9(2) . . ?
C15 C16 H16A 107.8 . . ?
C15 C16 H16B 107.8 . . ?
H16A C16 H16B 107.1 . . ?
C17 C16 C15 118.1(2) . . ?
C17 C16 H16A 107.8 . . ?
C17 C16 H16B 107.8 . . ?
C18 C17 C16 120.5(2) . . ?
C18 C17 C22 118.3(2) . . ?
C22 C17 C16 121.1(2) . . ?
C17 C18 H18 119.3 . . ?
C19 C18 C17 121.3(2) . . ?
C19 C18 H18 119.3 . . ?
C18 C19 H19 120.1 . . ?
C20 C19 C18 119.8(2) . . ?
C20 C19 H19 120.1 . . ?
C19 C20 H20 119.9 . . ?
C19 C20 C21 120.3(2) . . ?
C21 C20 H20 119.9 . . ?
C20 C21 H21 120.1 . . ?
C20 C21 C22 119.7(2) . . ?
C22 C21 H21 120.1 . . ?
C17 C22 N6 117.6(2) . . ?
C21 C22 N6 121.9(2) . . ?
C21 C22 C17 120.5(2) . . ?
N6 C23 C24 122.4(2) . . ?
N6 C23 C28 121.9(2) . . ?
C24 C23 C28 115.5(2) . . ?
C23 C24 Cl1 118.30(19) . . ?
C25 C24 Cl1 118.3(2) . . ?
C25 C24 C23 123.3(3) . . ?
C24 C25 H25 120.5 . . ?
C26 C25 C24 118.9(3) . . ?
C26 C25 H25 120.5 . . ?
C25 C26 H26 119.9 . . ?
C25 C26 C27 120.2(3) . . ?
C27 C26 H26 119.9 . . ?
C26 C27 H27 120.0 . . ?
C26 C27 C28 120.0(3) . . ?
C28 C27 H27 120.0 . . ?
C23 C28 Cl2 119.7(2) . . ?
C27 C28 Cl2 118.3(2) . . ?
C27 C28 C23 121.9(3) . . ?
N1 C29 H29 125.4 . . ?
C30 C29 N1 109.2(2) . . ?
C30 C29 H29 125.4 . . ?
N2 C30 H30 127.0 . . ?
C29 C30 N2 106.1(2) . . ?
C29 C30 H30 127.0 . . ?
N1 C31 N2 111.2(2) . . ?
N1 C31 H31 124.4 . . ?
N2 C31 H31 124.4 . . ?
N2 C32 H32A 108.9 . . ?
N2 C32 H32B 108.9 . . ?
N2 C32 C33 113.5(2) . . ?
H32A C32 H32B 107.7 . . ?
C33 C32 H32A 108.9 . . ?
C33 C32 H32B 108.9 . . ?
C32 C33 H33A 109.2 . . ?
C32 C33 H33B 109.2 . . ?
C32 C33 C34 112.1(2) . . ?
H33A C33 H33B 107.9 . . ?
C34 C33 H33A 109.2 . . ?
C34 C33 H33B 109.2 . . ?
C33 C34 H34A 108.6 . . ?
C33 C34 H34B 108.6 . . ?
C34 C34 C33 114.5(3) 3_657 . ?
C34 C34 H34A 108.6 3_657 . ?
C34 C34 H34B 108.6 3_657 . ?
H34A C34 H34B 107.6 . . ?
N3 C35 N4 111.2(2) . . ?
N3 C35 H35 124.4 . . ?
N4 C35 H35 124.4 . . ?
N3 C36 H36 125.4 . . ?
C37 C36 N3 109.1(2) . . ?
C37 C36 H36 125.4 . . ?
N4 C37 H37 126.7 . . ?
C36 C37 N4 106.5(2) . . ?
C36 C37 H37 126.7 . . ?
N4 C38 H38A 109.2 . . ?
N4 C38 H38B 109.2 . . ?
N4 C38 C39 112.20(19) . . ?
H38A C38 H38B 107.9 . . ?
C39 C38 H38A 109.2 . . ?
C39 C38 H38B 109.2 . . ?
C38 C39 H39A 108.8 . . ?
C38 C39 H39B 108.8 . . ?
H39A C39 H39B 107.7 . . ?
C40 C39 C38 113.7(2) . . ?
C40 C39 H39A 108.8 . . ?
C40 C39 H39B 108.8 . . ?
C39 C40 C40 111.9(2) . 3_767 ?
C39 C40 H40A 109.2 . . ?
C39 C40 H40B 109.2 . . ?
C40 C40 H40A 109.2 3_767 . ?
C40 C40 H40B 109.2 3_767 . ?
H40A C40 H40B 107.9 . . ?
C41 O5 H5B 109.5 . . ?
O5 C41 H41A 109.5 . . ?
O5 C41 H41B 109.5 . . ?
O5 C41 H41C 109.5 . . ?
H41A C41 H41B 109.5 . . ?
H41A C41 H41C 109.5 . . ?
H41B C41 H41C 109.5 . . ?

# end Validation Reply Form
_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
- Detector area scaling
;
_oxdiff_exptl_absorpt_empirical_full_max 2.320
_oxdiff_exptl_absorpt_empirical_full_min 0.611
# start Validation Reply Form
_vrf_PLAT978_cu_jnm038           
;
PROBLEM: Number C-C Bonds with Positive Residual Density.          0 Info  
RESPONSE: No problem here! This is where we would like to see the
calculated residual electron density at the "end" of a refinement.
;
