# Electronic Supplementary Material (ESI) for Dalton Transactions.
# 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_cyclo
_database_code_depnum_ccdc_archive 'CCDC 2344977'
loop_
_audit_author_name
_audit_author_address
'Raju Mondal'
;Indian Association for the Cultivation of Science
India
;
_audit_update_record             
;
2024-04-01 deposited with the CCDC.	2024-05-31 downloaded from the CCDC.
;
_audit_creation_date             2019-06-17
_audit_creation_method           
;
Olex2 1.2-beta
(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         'C17 H20 Cu3 N6 O5'
_chemical_formula_sum            'C17 H20 Cu3 N6 O5'
_chemical_formula_weight         579.01
_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 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Cu Cu 0.3201 1.2651 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_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                   9.001(3)
_cell_length_b                   9.519(4)
_cell_length_c                   11.394(4)
_cell_angle_alpha                88.919(12)
_cell_angle_beta                 85.325(12)
_cell_angle_gamma                86.622(12)
_cell_volume                     971.3(6)
_cell_formula_units_Z            2
_cell_measurement_reflns_used    3164
_cell_measurement_temperature    100
_cell_measurement_theta_max      24.98
_cell_measurement_theta_min      2.27
_shelx_estimated_absorpt_T_max   0.7454
_shelx_estimated_absorpt_T_min   0.5890
_exptl_absorpt_coefficient_mu    3.300
_exptl_absorpt_correction_T_max  1.0000
_exptl_absorpt_correction_T_min  0.7217
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
;
 TWINABS-2012/1 (Bruker,2012) was used for absorption correction.
 Final HKLF 4 output contains 7200 reflections, Rint = 0.0600
 (3388 reflections with I > 3sig(I), Rint = 0.0435)
;
_exptl_absorpt_special_details   ?
_exptl_crystal_colour            Blue
_exptl_crystal_density_diffrn    1.980
_exptl_crystal_density_meas      'not measured'
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       Block
_exptl_crystal_F_000             582
_exptl_crystal_size_max          0.20
_exptl_crystal_size_mid          0.20
_exptl_crystal_size_min          0.12
_exptl_special_details           
; Full sphere of reciprocal space was nominally covered by 4 runs of 108 
  narrow-frame ω-scans (scan width 1°, 10s exposure), every run at a 
  different φ angle. Crystal to detector distance 3.98 cm. 
  Non-merohedral twinning by 180° rotation about the reciprocal axis z* 
  or the real axis [-0.1 0 1], deconvoluted using CELL_NOW 2008/4 program. 
  Twin law: 
     -1    0    0 
      0   -1    0 
     -0.2  0    1

  897 data ( 388 unique) involve domain  1 only, mean I/sigma  14.5
  875 data ( 376 unique) involve domain  2 only, mean I/sigma  14.2
 5895 data (2839 unique) involve both domains,   mean I/sigma  10.2

;
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0600
_diffrn_reflns_av_unetI/netI     0.0776
_diffrn_reflns_Laue_measured_fraction_full 0.984
_diffrn_reflns_Laue_measured_fraction_max 0.984
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_l_max       13
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_number            7200
_diffrn_reflns_point_group_measured_fraction_full 0.984
_diffrn_reflns_point_group_measured_fraction_max 0.984
_diffrn_reflns_theta_full        25.128
_diffrn_reflns_theta_max         25.128
_diffrn_reflns_theta_min         2.274
_diffrn_ambient_temperature      100
_diffrn_detector                 'Bruker PHOTON 100 CMOS'
_diffrn_detector_area_resol_mean 10.4
_diffrn_detector_type            'CMOS sensor'
_diffrn_measured_fraction_theta_full 0.984
_diffrn_measured_fraction_theta_max 0.984
_diffrn_measurement_device       '3-circle area detector diffractometer'
_diffrn_measurement_device_type  'Bruker D8 Venture'
_diffrn_measurement_method       ω-scan
_diffrn_measurement_specimen_support 'MiTeGen loop'
_diffrn_radiation_monochromator  'focusing mirrors'
_diffrn_radiation_probe          X-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_source                   'microfocus sealed X-ray tube'
_diffrn_source_type              'Incoatec I\mS microsource'
_diffrn_standards_number         0
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                2756
_reflns_number_total             3580
_reflns_special_details          
;
 _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. Completness statistics refer to single and
 composite reflections containing twin component 1 only.
;
_reflns_threshold_expression     'I > 2σ(I)'
_computing_cell_refinement       'SAINT v8.38A (Bruker, 2017)'
_computing_data_collection       'APEX3 v.2016.1-0 (Bruker, 2016)'
_computing_data_reduction        'SAINT v8.38A (Bruker, 2017)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL 2018/3 (Sheldrick, 2015)'
_computing_structure_solution    'ShelXS 2013/1 (Sheldrick, 2008)'
_refine_diff_density_max         0.879
_refine_diff_density_min         -0.726
_refine_diff_density_rms         0.183
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.077
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     264
_refine_ls_number_reflns         3580
_refine_ls_number_restraints     246
_refine_ls_R_factor_all          0.0915
_refine_ls_R_factor_gt           0.0597
_refine_ls_restrained_S_all      1.058
_refine_ls_shift/su_max          0.005
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0409P)²+7.2143P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1229
_refine_ls_wR_factor_ref         0.1398
_refine_special_details          
;
 Refined as a 2-component twin. 
 The 1,3-dicarboxylate-cyclohexane ligand, except C(2), is disordered 
 between positions A and B with occupancies 0.527(11) and 0.473(11). 
;
_olex2_refinement_description    
;
1. Twinned data refinement
 Scales: 0.5015(19)
 0.4985(19)
2. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups, All C(H,H,H,H) groups
 At 1.5 times of:
  All O(H) groups
3. Restrained distances
 C8B-C3A \\sim C8B-C3B \\sim C7B-C1A \\sim C7B-C1B
 with sigma of 0.02
 C4A-C3A \\sim C5A-C4A \\sim C5A-C6A \\sim C6A-C1A \\sim C2-C1A \\sim C1B-C2
\\sim C1B-C6B \\sim C5B-C6B ~
 C5B-C4B \\sim C4B-C3B \\sim C3A-C2 \\sim C3B-C2
 with sigma of 0.02
 C8B-C3B \\sim C8A-C3A
 with sigma of 0.02
 Cu2_$1-O5A \\sim Cu2_$1-O5B
 with sigma of 0.005
 O3A-C7A \\sim O3B-C7B
 with sigma of 0.02
 C7B-C1B \\sim C7A-C1A
 with sigma of 0.02
 O2A-C7A \\sim O2B-C7B
 with sigma of 0.02
 Cu3-O4B_$2 \\sim Cu3-O4A_$2
 with sigma of 0.02
 O4B_$2-C8B_$2 \\sim O5A_$2-C8A_$2
 with sigma of 0.02
 O4A_$2-C8A_$2 \\sim O5B_$2-C8B_$2
 with sigma of 0.02
4. Uiso/Uaniso restraints and constraints
Uiso(C1A) = Uiso(C1B)
Uiso(C6B) = Uiso(C6A)
Uiso(C3A) = Uiso(C3B)
Uiso(C7A) = Uiso(C7B)
Uiso(O2A) = Uiso(O2B)
Uiso(O3B) = Uiso(O3A)
Uiso(O4A) = Uiso(O4B)
5. Rigid body (RIGU) restrains
 C9, C10, C11
 with sigma for 1-2 distances of 0.001 and sigma for 1-3 distances of 0.001
 All non-hydrogen atoms
 with sigma for 1-2 distances of 0.005 and sigma for 1-3 distances of 0.005
6. Others
 Sof(H2BC)=Sof(H2BD)=Sof(O2B)=Sof(O3B)=Sof(O4B)=Sof(O5B)=Sof(C1B)=Sof(H1B)=
 Sof(C3B)=Sof(H3B)=Sof(C4B)=Sof(H4BA)=Sof(H4BB)=Sof(C5B)=Sof(H5BA)=Sof(H5BB)=
 Sof(C6B)=Sof(H6BA)=Sof(H6BB)=Sof(C7B)=Sof(C8B)=1-FVAR(1)
 Sof(H2AA)=Sof(H2AB)=Sof(O2A)=Sof(O3A)=Sof(O4A)=Sof(O5A)=Sof(C1A)=Sof(H1A)=
 Sof(C3A)=Sof(H3A)=Sof(C4A)=Sof(H4AA)=Sof(H4AB)=Sof(C5A)=Sof(H5AA)=Sof(H5AB)=
 Sof(C6A)=Sof(H6AA)=Sof(H6AB)=Sof(C7A)=Sof(C8A)=FVAR(1)
7.a Riding coordinates:
 O1(H1)
7.b Ternary CH refined with riding coordinates:
 C1A(H1A), C3A(H3A), C1B(H1B), C3B(H3B)
7.c Secondary CH2 refined with riding coordinates:
 C2(H2AA,H2AB), C2(H2BC,H2BD), C4A(H4AA,H4AB), C5A(H5AA,H5AB), C6A(H6AA,H6AB),
 C4B(H4BA,H4BB), C5B(H5BA,H5BB), C6B(H6BA,H6BB)
7.d Aromatic/amide H refined with riding coordinates:
 C9(H9), C10(H10), C11(H11), C12(H12), C13(H13), C14(H14), C15(H15), C16(H16),
 C17(H17)
;
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap

loop_
_twin_individual_id
_twin_individual_mass_fraction_refined
_twin_individual_twin_lattice_type
_twin_individual_twin_matrix_11
_twin_individual_twin_matrix_12
_twin_individual_twin_matrix_13
_twin_individual_twin_matrix_21
_twin_individual_twin_matrix_22
_twin_individual_twin_matrix_23
_twin_individual_twin_matrix_31
_twin_individual_twin_matrix_32
_twin_individual_twin_matrix_33
1 0.5015(19) ref 1 0 0 0 1 0 0 0 1
2 0.4985(19) mt2 -1 0 0 0 -1 0 -0.2 0 1

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 0.14004(14) 0.62699(15) 0.36003(13) 0.0228(4) Uani 1 1 d . U . . .
Cu2 Cu -0.13974(15) 0.87906(15) 0.37369(14) 0.0262(4) Uani 1 1 d D U . . .
Cu3 Cu 0.01668(17) 0.76802(17) 0.62418(13) 0.0340(4) Uani 1 1 d D U . . .
O1 O -0.0248(8) 0.7298(8) 0.4586(6) 0.0269(18) Uani 1 1 d . U . . .
H1 H -0.089846 0.668350 0.463975 0.040 Uiso 1 1 d R . . . .
N1 N 0.2192(10) 0.5594(10) 0.5057(9) 0.023(2) Uani 1 1 d . U . . .
N2 N 0.1564(9) 0.6032(10) 0.6120(8) 0.025(2) Uani 1 1 d . U . . .
N3 N 0.0465(10) 0.6917(10) 0.2205(8) 0.026(2) Uani 1 1 d . U . . .
N4 N -0.0708(11) 0.7897(10) 0.2256(9) 0.030(2) Uani 1 1 d . U . . .
N5 N -0.1960(10) 0.9678(10) 0.5245(8) 0.027(2) Uani 1 1 d . U . . .
N6 N -0.1232(10) 0.9337(9) 0.6214(9) 0.028(2) Uani 1 1 d . U . . .
C2 C 0.5105(12) 0.2489(13) 0.2377(9) 0.030(3) Uani 1 1 d D U . . .
H2AA H 0.451038 0.166120 0.257197 0.036 Uiso 0.527(11) 1 calc R . P A 1
H2AB H 0.533810 0.292132 0.311840 0.036 Uiso 0.527(11) 1 calc R . P A 1
H2BC H 0.565560 0.333570 0.250418 0.036 Uiso 0.473(11) 1 calc R . P A 2
H2BD H 0.478196 0.208645 0.315715 0.036 Uiso 0.473(11) 1 calc R . P A 2
C9 C 0.3191(12) 0.4539(12) 0.5276(10) 0.025(2) Uani 1 1 d . U . . .
H9 H 0.378906 0.403302 0.468193 0.030 Uiso 1 1 calc R . . . .
C10 C 0.3245(11) 0.4276(11) 0.6461(10) 0.025(2) Uani 1 1 d . U . . .
H10 H 0.387782 0.360870 0.684048 0.030 Uiso 1 1 calc R . . . .
C11 C 0.2147(12) 0.5225(11) 0.6976(11) 0.026(2) Uani 1 1 d . U . . .
H11 H 0.185867 0.529030 0.779480 0.031 Uiso 1 1 calc R . . . .
C12 C 0.0678(14) 0.6502(12) 0.1089(11) 0.034(3) Uani 1 1 d . U . . .
H12 H 0.142839 0.581899 0.080725 0.041 Uiso 1 1 calc R . . . .
C13 C -0.0336(14) 0.7195(15) 0.0393(11) 0.046(4) Uani 1 1 d . U . . .
H13 H -0.043251 0.709332 -0.042466 0.055 Uiso 1 1 calc R . . . .
C14 C -0.1173(13) 0.8070(12) 0.1184(11) 0.032(3) Uani 1 1 d . U . . .
H14 H -0.196949 0.870667 0.098653 0.038 Uiso 1 1 calc R . . . .
C15 C -0.3058(13) 1.0694(13) 0.5555(11) 0.031(3) Uani 1 1 d . U . . .
H15 H -0.374633 1.111994 0.504835 0.038 Uiso 1 1 calc R . . . .
C16 C -0.2993(13) 1.0992(12) 0.6732(10) 0.029(3) Uani 1 1 d . U . . .
H16 H -0.360394 1.166452 0.718431 0.034 Uiso 1 1 calc R . . . .
C17 C -0.1841(13) 1.0099(12) 0.7115(11) 0.030(3) Uani 1 1 d . U . . .
H17 H -0.153870 1.004308 0.789549 0.036 Uiso 1 1 calc R . . . .
O2A O 0.310(3) 0.5414(19) 0.271(2) 0.024(2) Uiso 0.527(11) 1 d D U P A 1
O3A O 0.178(2) 0.356(3) 0.277(2) 0.041(3) Uiso 0.527(11) 1 d D U P A 1
O4A O 0.890(2) 0.169(3) 0.2330(14) 0.038(3) Uiso 0.527(11) 1 d D U P A 1
O5A O 0.7293(18) 0.0160(18) 0.2967(17) 0.029(6) Uiso 0.527(11) 1 d D U P A 1
C1A C 0.4249(19) 0.3556(18) 0.1622(13) 0.015(4) Uiso 0.527(11) 1 d D U P A 1
H1A H 0.489743 0.433755 0.135626 0.019 Uiso 0.527(11) 1 calc R . P A 1
C3A C 0.6583(17) 0.204(2) 0.1603(14) 0.021(4) Uiso 0.527(11) 1 d D U P A 1
H3A H 0.704179 0.293112 0.131242 0.025 Uiso 0.527(11) 1 calc R . P A 1
C4A C 0.619(2) 0.126(2) 0.0521(15) 0.022(5) Uiso 0.527(11) 1 d D U P A 1
H4AA H 0.567530 0.040147 0.077397 0.026 Uiso 0.527(11) 1 calc R . P A 1
H4AB H 0.711001 0.097646 0.003146 0.026 Uiso 0.527(11) 1 calc R . P A 1
C5A C 0.516(2) 0.221(3) -0.021(2) 0.028(7) Uiso 0.527(11) 1 d D U P A 1
H5AA H 0.571990 0.301081 -0.054769 0.034 Uiso 0.527(11) 1 calc R . P A 1
H5AB H 0.483979 0.167180 -0.086671 0.034 Uiso 0.527(11) 1 calc R . P A 1
C6A C 0.379(2) 0.278(2) 0.0554(16) 0.026(4) Uiso 0.527(11) 1 d D U P A 1
H6AA H 0.317714 0.198790 0.082696 0.032 Uiso 0.527(11) 1 calc R . P A 1
H6AB H 0.317454 0.342973 0.007821 0.032 Uiso 0.527(11) 1 calc R . P A 1
C7A C 0.291(2) 0.413(2) 0.245(2) 0.016(3) Uiso 0.527(11) 1 d D U P A 1
C8A C 0.770(2) 0.126(2) 0.2334(18) 0.018(6) Uiso 0.527(11) 1 d D U P A 1
O2B O 0.301(3) 0.516(2) 0.258(2) 0.024(2) Uiso 0.473(11) 1 d D U P A 2
O3B O 0.139(2) 0.350(3) 0.266(2) 0.041(3) Uiso 0.473(11) 1 d D U P A 2
O4B O 0.858(3) 0.159(3) 0.2502(17) 0.038(3) Uiso 0.473(11) 1 d D U P A 2
O5B O 0.7026(18) -0.015(2) 0.2969(18) 0.030(7) Uiso 0.473(11) 1 d D U P A 2
C1B C 0.3697(18) 0.292(2) 0.1695(14) 0.015(4) Uiso 0.473(11) 1 d D U P A 2
H1B H 0.319597 0.205067 0.149904 0.019 Uiso 0.473(11) 1 calc R . P A 2
C3B C 0.614(2) 0.141(2) 0.1685(14) 0.021(4) Uiso 0.473(11) 1 d D U P A 2
H3B H 0.555165 0.059191 0.149513 0.025 Uiso 0.473(11) 1 calc R . P A 2
C4B C 0.667(2) 0.214(3) 0.0548(17) 0.023(6) Uiso 0.473(11) 1 d D U P A 2
H4BA H 0.735655 0.148092 0.007439 0.028 Uiso 0.473(11) 1 calc R . P A 2
H4BB H 0.723825 0.295317 0.073841 0.028 Uiso 0.473(11) 1 calc R . P A 2
C5B C 0.539(3) 0.266(3) -0.019(2) 0.023(7) Uiso 0.473(11) 1 d D U P A 2
H5BA H 0.487274 0.184530 -0.045014 0.028 Uiso 0.473(11) 1 calc R . P A 2
H5BB H 0.579904 0.316916 -0.089901 0.028 Uiso 0.473(11) 1 calc R . P A 2
C6B C 0.429(3) 0.364(2) 0.0555(17) 0.026(4) Uiso 0.473(11) 1 d D U P A 2
H6BA H 0.480308 0.448794 0.075106 0.032 Uiso 0.473(11) 1 calc R . P A 2
H6BB H 0.344849 0.394318 0.008918 0.032 Uiso 0.473(11) 1 calc R . P A 2
C7B C 0.256(2) 0.394(2) 0.233(2) 0.016(3) Uiso 0.473(11) 1 d D U P A 2
C8B C 0.737(2) 0.089(3) 0.245(2) 0.016(6) Uiso 0.473(11) 1 d D U P A 2


_geom_special_details            
;
 All esds (except the esd in the dihedral angle between two l.s. planes)
 are estimated using the full covariance matrix.  The cell esds are taken
 into account individually in the estimation of esds in distances, angles
 and torsion angles; correlations between esds in cell parameters are only
 used when they are defined by crystal symmetry.  An approximate (isotropic)
 treatment of cell esds is used for estimating esds involving l.s. planes.
;
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Cu1 O1 2.005(7) . ?
Cu1 N1 1.943(10) . ?
Cu1 N3 1.933(10) . ?
Cu1 O2A 1.92(2) . ?
Cu1 O2B 2.04(3) . ?
Cu2 O1 1.991(8) . ?
Cu2 N4 1.943(10) . ?
Cu2 N5 1.945(10) . ?
Cu2 O5A 1.951(9) 1_465 ?
Cu2 O5B 1.949(9) 1_465 ?
Cu3 O1 1.996(7) . ?
Cu3 N2 1.952(9) . ?
Cu3 N6 1.960(9) . ?
Cu3 O3A 2.372(17) 2_566 ?
Cu3 O4A 2.011(13) 2_666 ?
Cu3 O3B 2.16(2) 2_566 ?
Cu3 O4B 2.050(14) 2_666 ?
N1 N2 1.357(13) . ?
N1 C9 1.342(14) . ?
N2 C11 1.351(14) . ?
N3 N4 1.365(11) . ?
N3 C12 1.334(14) . ?
N4 C14 1.328(14) . ?
N5 N6 1.354(12) . ?
N5 C15 1.371(14) . ?
N6 C17 1.331(14) . ?
C2 C1A 1.533(13) . ?
C2 C3A 1.575(14) . ?
C2 C1B 1.570(14) . ?
C2 C3B 1.533(14) . ?
C9 C10 1.372(16) . ?
C10 C11 1.399(14) . ?
C12 C13 1.387(16) . ?
C13 C14 1.385(16) . ?
C15 C16 1.382(15) . ?
C16 C17 1.395(16) . ?
O2A C7A 1.290(18) . ?
O3A C7A 1.204(17) . ?
O4A C8A 1.18(2) . ?
O5A C8A 1.31(2) . ?
C1A C6A 1.533(14) . ?
C1A C7A 1.545(16) . ?
C3A C4A 1.530(14) . ?
C3A C8A 1.512(16) . ?
C4A C5A 1.536(15) . ?
C5A C6A 1.527(15) . ?
O2B C7B 1.298(18) . ?
O3B C7B 1.184(18) . ?
O4B C8B 1.31(2) . ?
O5B C8B 1.18(2) . ?
C1B C6B 1.531(15) . ?
C1B C7B 1.520(17) . ?
C3B C4B 1.516(15) . ?
C3B C8B 1.521(17) . ?
C4B C5B 1.531(15) . ?
C5B C6B 1.535(15) . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
O1 Cu1 O2B 177.5(6) . . ?
N1 Cu1 O1 87.7(3) . . ?
N1 Cu1 O2B 93.0(8) . . ?
N3 Cu1 O1 89.1(4) . . ?
N3 Cu1 N1 175.7(4) . . ?
N3 Cu1 O2B 90.1(8) . . ?
O2A Cu1 O1 174.5(6) . . ?
O2A Cu1 N1 90.5(8) . . ?
O2A Cu1 N3 93.0(8) . . ?
N4 Cu2 O1 89.3(3) . . ?
N4 Cu2 N5 176.4(4) . . ?
N4 Cu2 O5A 92.5(7) . 1_465 ?
N4 Cu2 O5B 90.4(7) . 1_465 ?
N5 Cu2 O1 88.4(4) . . ?
N5 Cu2 O5A 90.1(7) . 1_465 ?
N5 Cu2 O5B 92.7(7) . 1_465 ?
O5A Cu2 O1 174.2(6) 1_465 . ?
O5B Cu2 O1 163.1(7) 1_465 . ?
O1 Cu3 O3A 98.6(6) . 2_566 ?
O1 Cu3 O4A 163.3(6) . 2_666 ?
O1 Cu3 O3B 105.8(7) . 2_566 ?
O1 Cu3 O4B 153.6(7) . 2_666 ?
N2 Cu3 O1 86.5(4) . . ?
N2 Cu3 N6 175.0(4) . . ?
N2 Cu3 O3A 94.1(7) . 2_566 ?
N2 Cu3 O4A 90.5(8) . 2_666 ?
N2 Cu3 O3B 90.4(8) . 2_566 ?
N2 Cu3 O4B 87.6(9) . 2_666 ?
N6 Cu3 O1 88.7(4) . . ?
N6 Cu3 O3A 88.1(7) . 2_566 ?
N6 Cu3 O4A 93.7(8) . 2_666 ?
N6 Cu3 O3B 92.3(8) . 2_566 ?
N6 Cu3 O4B 96.0(9) . 2_666 ?
O4A Cu3 O3A 98.0(8) 2_666 2_566 ?
O4A Cu3 O3B 90.6(8) 2_666 2_566 ?
O4A Cu3 O4B 9.8(10) 2_666 2_666 ?
Cu2 O1 Cu1 115.0(4) . . ?
Cu2 O1 Cu3 117.4(4) . . ?
Cu3 O1 Cu1 116.1(4) . . ?
N2 N1 Cu1 121.3(7) . . ?
C9 N1 Cu1 131.5(8) . . ?
C9 N1 N2 106.3(9) . . ?
N1 N2 Cu3 120.8(7) . . ?
C11 N2 Cu3 129.9(8) . . ?
C11 N2 N1 109.1(9) . . ?
N4 N3 Cu1 121.8(8) . . ?
C12 N3 Cu1 131.3(8) . . ?
C12 N3 N4 106.7(9) . . ?
N3 N4 Cu2 120.4(7) . . ?
C14 N4 Cu2 131.2(8) . . ?
C14 N4 N3 108.4(10) . . ?
N6 N5 Cu2 121.8(7) . . ?
N6 N5 C15 107.8(9) . . ?
C15 N5 Cu2 130.5(8) . . ?
N5 N6 Cu3 121.1(7) . . ?
C17 N6 Cu3 128.4(8) . . ?
C17 N6 N5 109.2(9) . . ?
C1A C2 C3A 105.5(12) . . ?
C3B C2 C1B 110.9(12) . . ?
N1 C9 C10 112.0(11) . . ?
C9 C10 C11 103.5(10) . . ?
N2 C11 C10 108.9(11) . . ?
N3 C12 C13 111.3(10) . . ?
C14 C13 C12 102.9(11) . . ?
N4 C14 C13 110.7(11) . . ?
N5 C15 C16 108.4(11) . . ?
C15 C16 C17 105.5(10) . . ?
N6 C17 C16 109.1(11) . . ?
C7A O2A Cu1 112.3(16) . . ?
C7A O3A Cu3 168(2) . 2_566 ?
C8A O4A Cu3 125.3(16) . 2_666 ?
C8A O5A Cu2 126.8(14) . 1_645 ?
C2 C1A C6A 107.8(14) . . ?
C2 C1A C7A 104.8(14) . . ?
C6A C1A C7A 113.7(15) . . ?
C4A C3A C2 109.2(13) . . ?
C8A C3A C2 111.1(14) . . ?
C8A C3A C4A 114.9(16) . . ?
C3A C4A C5A 110.1(17) . . ?
C6A C5A C4A 110.8(18) . . ?
C5A C6A C1A 110.9(17) . . ?
O2A C7A C1A 109.6(17) . . ?
O3A C7A O2A 122(2) . . ?
O3A C7A C1A 129(2) . . ?
O4A C8A O5A 122.6(19) . . ?
O4A C8A C3A 117.6(19) . . ?
O5A C8A C3A 119.8(18) . . ?
C7B O2B Cu1 110.5(18) . . ?
C6B C1B C2 105.6(14) . . ?
C7B C1B C2 115.1(15) . . ?
C7B C1B C6B 107.7(16) . . ?
C4B C3B C2 106.0(14) . . ?
C4B C3B C8B 114.9(17) . . ?
C8B C3B C2 108.8(16) . . ?
C3B C4B C5B 113.3(18) . . ?
C4B C5B C6B 109.2(19) . . ?
C1B C6B C5B 111.8(18) . . ?
O2B C7B C1B 117(2) . . ?
O3B C7B O2B 126(2) . . ?
O3B C7B C1B 116(2) . . ?
O4B C8B C3B 121(2) . . ?
O5B C8B O4B 129(2) . . ?
O5B C8B C3B 109.8(17) . . ?


#===END
####################################################################### 
# 
# 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_oba
_database_code_depnum_ccdc_archive 'CCDC 2344979'
loop_
_audit_author_name
_audit_author_address
'Raju Mondal'
;Indian Association for the Cultivation of Science
India
;
_audit_update_record             
;
2024-04-01 deposited with the CCDC.	2024-05-31 downloaded from the CCDC.
;
_audit_creation_method           
;
Olex2 1.2-beta
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_shelx_SHELXL_version_number     2016/6
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C92 H92 Cu12 N24 O34'
_chemical_formula_weight         2840.37

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Cu Cu 0.3201 1.2651 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_space_group_crystal_system      monoclinic
_space_group_IT_number           13
_space_group_name_H-M_alt        'P 2/c'
_space_group_name_Hall           '-P 2yc'

_shelx_space_group_comment       
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;

loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, y, -z+1/2'
'-x, -y, -z'
'x, -y, z-1/2'

_cell_length_a                   17.760(12)
_cell_length_b                   9.823(7)
_cell_length_c                   17.162(12)
_cell_angle_alpha                90
_cell_angle_beta                 116.558(12)
_cell_angle_gamma                90
_cell_volume                     2678(3)
_cell_formula_units_Z            1
_cell_measurement_temperature    100(2)
_cell_measurement_reflns_used    2389
_cell_measurement_theta_min      2.38
_cell_measurement_theta_max      16.66

_exptl_crystal_description       Block
_exptl_crystal_colour            Blue
_exptl_crystal_density_meas      'not measured'
_exptl_crystal_density_method    'not measured'
_exptl_crystal_density_diffrn    1.761
_exptl_crystal_F_000             1432
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.30
_exptl_crystal_size_mid          0.24
_exptl_crystal_size_min          0.20
_exptl_special_details           
; Data were collected in shutterless mode. Full sphere of reciprocal 
  space was nominally covered by 8 runs of 112 narrow-frame ω-scans 
  (scan width 1°, 20s exposure), every run at a different φ angle. 
  Crystal to detector distance 5.98 cm. 
  Pseudo-merohedral twinning was deconvoluted using CELL_NOW 2008/4 
  program. Twin law:
     -1  0  0 
      0 -1  0 
      1  0  1
  (180° rotation about the reciprocal axis z* or the direct axis 
   [1/2 0 1]).
   7108 data (1459 unique) involve domain 1 only, mean I/sigma 3.2
   6975 data (1436 unique) involve domain 2 only, mean I/sigma 2.6
  47383 data (5615 unique) involve  both domains, mean I/sigma 2.6

;
_exptl_absorpt_coefficient_mu    2.422
_shelx_estimated_absorpt_T_min   ?
_shelx_estimated_absorpt_T_max   ?
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.5271
_exptl_absorpt_correction_T_max  1.0000
_exptl_absorpt_process_details   
;
 TWINABS-2012/1 (Bruker,2012) was used for absorption correction.
 Final HKLF 4 output contains 60217 reflections, Rint = 0.2063
 (8874 with I > 3sig(I), Rint = 0.1281)
;
_exptl_absorpt_special_details   ?
_diffrn_ambient_temperature      100(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_source                   '3-circle area detector diffractometer'
_diffrn_measurement_device_type  'Bruker D8 Venture'
_diffrn_measurement_method       ω-scan
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            7494
_diffrn_reflns_av_unetI/netI     0.1476
_diffrn_reflns_av_R_equivalents  ?
_diffrn_reflns_limit_h_min       0
_diffrn_reflns_limit_h_max       21
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_k_max       0
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_theta_min         2.073
_diffrn_reflns_theta_max         24.996
_diffrn_reflns_theta_full        24.996
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measured_fraction_theta_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_point_group_measured_fraction_full 0.999
_reflns_number_total             7494
_reflns_number_gt                4868
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_max     .
_reflns_Friedel_fraction_full    .

_reflns_special_details          
;
 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.
;

_computing_data_collection       'APEX3 v.2016.1-0 (Bruker, 2016)'
_computing_cell_refinement       'SAINT v8.38A (Bruker, 2017)'
_computing_data_reduction        'SAINT v8.38A (Bruker, 2017)'
_computing_structure_solution    'ShelXS 2013/1 (Sheldrick, 2008)'
_computing_structure_refinement  'SHELXL-2016/6 (Sheldrick, 2016)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_refine_special_details          
;
 Refined as a 2-component twin.
;
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0988P)²+15.6042P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
_atom_sites_solution_hydrogens   mixed
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_number_reflns         7494
_refine_ls_number_parameters     371
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.1406
_refine_ls_R_factor_gt           0.0834
_refine_ls_wR_factor_ref         0.2364
_refine_ls_wR_factor_gt          0.1927
_refine_ls_goodness_of_fit_ref   1.037
_refine_ls_restrained_S_all      1.037
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
Cu1 Cu 0.09662(11) 0.35559(15) 0.59095(10) 0.0372(4) Uani 1 1 d . . . . .
Cu2 Cu -0.08698(10) 0.20388(16) 0.45475(10) 0.0372(4) Uani 1 1 d . . . . .
Cu3 Cu 0.09792(11) 0.10989(16) 0.45604(10) 0.0371(4) Uani 1 1 d . . . . .
O1 O 0.0315(5) 0.2518(8) 0.4804(5) 0.033(2) Uani 1 1 d . . . . .
H1 H 0.022682 0.309620 0.440400 0.040 Uiso 1 1 d R U . . .
O2 O 0.1663(6) 0.4490(10) 0.6996(6) 0.044(2) Uani 1 1 d . . . . .
O3 O 0.1318(7) 0.6667(11) 0.6690(7) 0.069(3) Uani 1 1 d . . . . .
O4 O 0.4792(6) 0.7361(13) 1.0003(7) 0.066(3) Uani 1 1 d . . . . .
O5 O 0.8312(6) 0.9665(10) 1.0597(6) 0.046(2) Uani 1 1 d . . . . .
O6 O 0.7979(5) 0.8474(10) 0.9369(6) 0.044(2) Uani 1 1 d . . . . .
N1 N -0.0103(6) 0.4052(10) 0.5901(7) 0.035(3) Uani 1 1 d . . . . .
N2 N -0.0837(7) 0.3534(10) 0.5307(7) 0.037(3) Uani 1 1 d . . . . .
N3 N -0.0794(6) 0.0447(11) 0.3910(6) 0.034(2) Uani 1 1 d . . . . .
N4 N -0.0057(7) 0.0066(13) 0.3931(6) 0.037(3) Uani 1 1 d . . . . .
N5 N 0.1968(7) 0.2136(13) 0.5227(8) 0.047(3) Uani 1 1 d . . . . .
N6 N 0.1994(7) 0.3077(11) 0.5835(7) 0.042(3) Uani 1 1 d . . . . .
C0AA C -0.0275(9) 0.4918(16) 0.6398(9) 0.048(4) Uani 1 1 d . . . . .
H0AA H 0.013418 0.541160 0.687611 0.057 Uiso 1 1 calc R U . . .
C2 C -0.1118(9) 0.4993(19) 0.6122(10) 0.057(4) Uani 1 1 d . . . . .
H2 H -0.141299 0.554039 0.635047 0.068 Uiso 1 1 calc R U . . .
C3 C -0.1449(9) 0.4093(14) 0.5433(9) 0.046(4) Uani 1 1 d . . . . .
H3 H -0.203136 0.390384 0.509993 0.055 Uiso 1 1 calc R U . . .
C4 C -0.1394(8) -0.0382(14) 0.3374(9) 0.040(3) Uani 1 1 d . . . . .
H4 H -0.196822 -0.036010 0.326322 0.049 Uiso 1 1 calc R U . . .
C5 C -0.1048(9) -0.1277(13) 0.3005(9) 0.045(4) Uani 1 1 d . . . . .
H5 H -0.133400 -0.195397 0.257957 0.054 Uiso 1 1 calc R U . . .
C6 C -0.0207(9) -0.0985(13) 0.3381(8) 0.037(3) Uani 1 1 d . . . . .
H6 H 0.020434 -0.145048 0.327050 0.044 Uiso 1 1 calc R U . . .
C7 C 0.2739(10) 0.2143(17) 0.5250(10) 0.057(4) Uani 1 1 d . . . . .
H7 H 0.290011 0.159659 0.489303 0.068 Uiso 1 1 calc R U . . .
C8 C 0.3259(11) 0.306(2) 0.5869(11) 0.072(5) Uani 1 1 d . . . . .
H8 H 0.382934 0.326639 0.601616 0.087 Uiso 1 1 calc R U . . .
C9 C 0.2774(9) 0.3607(16) 0.6222(11) 0.060(5) Uani 1 1 d . . . . .
H9 H 0.296090 0.426536 0.667567 0.072 Uiso 1 1 calc R U . . .
C10 C 0.1801(9) 0.5739(15) 0.7123(9) 0.039(3) Uani 1 1 d . . . . .
C11 C 0.2612(8) 0.6140(12) 0.7872(8) 0.034(3) Uani 1 1 d . . . . .
C12 C 0.3088(9) 0.5247(15) 0.8534(9) 0.048(4) Uani 1 1 d . . . . .
H12 H 0.290252 0.433251 0.850167 0.058 Uiso 1 1 calc R U . . .
C13 C 0.3815(11) 0.5638(18) 0.9231(11) 0.063(5) Uani 1 1 d . . . . .
H13 H 0.412398 0.501489 0.968613 0.075 Uiso 1 1 calc R U . . .
C14 C 0.4088(9) 0.6937(18) 0.9259(9) 0.049(4) Uani 1 1 d . . . . .
C15 C 0.3659(10) 0.7853(16) 0.8622(11) 0.054(4) Uani 1 1 d . . . . .
H15 H 0.385787 0.876002 0.865725 0.065 Uiso 1 1 calc R U . . .
C16 C 0.2915(10) 0.7428(15) 0.7911(10) 0.053(4) Uani 1 1 d . . . . .
H16 H 0.261807 0.804631 0.744900 0.063 Uiso 1 1 calc R U . . .
C17 C 0.7822(8) 0.8928(14) 0.9968(9) 0.036(3) Uani 1 1 d . . . . .
C18 C 0.7016(9) 0.8517(14) 0.9964(9) 0.038(3) Uani 1 1 d . . . . .
C19 C 0.6417(9) 0.7832(16) 0.9271(9) 0.048(4) Uani 1 1 d . . . . .
H19 H 0.652555 0.761783 0.879081 0.058 Uiso 1 1 calc R U . . .
C20 C 0.5673(10) 0.7446(18) 0.9246(10) 0.058(4) Uani 1 1 d . . . . .
H20 H 0.526604 0.698264 0.875154 0.069 Uiso 1 1 calc R U . . .
C21 C 0.5510(9) 0.7735(15) 0.9949(10) 0.042(4) Uani 1 1 d . . . . .
C22 C 0.6101(10) 0.8415(16) 1.0661(10) 0.049(4) Uani 1 1 d . . . . .
H22 H 0.599678 0.862327 1.114482 0.059 Uiso 1 1 calc R U . . .
C23 C 0.6845(10) 0.8785(16) 1.0657(10) 0.052(4) Uani 1 1 d . . . . .
H23 H 0.725682 0.924410 1.115023 0.062 Uiso 1 1 calc R U . . .
O2W O 0.468(7) 1.062(11) 0.753(9) 0.18(4) Uani 0.25 1 d . . P A 1
O3W O 0.387(6) 1.053(5) 0.735(4) 0.12(3) Uani 0.25 1 d . . P B 2
O1W O 0.0863(9) 0.1825(12) 0.3029(7) 0.082(4) Uani 1 1 d . . . . .


_geom_special_details            
;
 All esds (except the esd in the dihedral angle between two l.s. planes)
 are estimated using the full covariance matrix.  The cell esds are taken
 into account individually in the estimation of esds in distances, angles
 and torsion angles; correlations between esds in cell parameters are only
 used when they are defined by crystal symmetry.  An approximate (isotropic)
 treatment of cell esds is used for estimating esds involving l.s. planes.
;

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Cu1 N6 1.944(11) . ?
Cu1 O2 1.946(9) . ?
Cu1 N1 1.953(11) . ?
Cu1 O1 2.003(8) . ?
Cu2 N3 1.947(10) . ?
Cu2 N2 1.947(11) . ?
Cu2 O6 1.992(9) 4_465 ?
Cu2 O1 2.004(8) . ?
Cu2 O3 2.291(10) 3_566 ?
Cu3 N5 1.906(12) . ?
Cu3 N4 1.950(12) . ?
Cu3 O5 1.986(9) 2_646 ?
Cu3 O1 1.987(8) . ?
O2 C10 1.251(16) . ?
O3 C10 1.244(16) . ?
O4 C21 1.370(16) . ?
O4 C14 1.393(16) . ?
O5 C17 1.268(16) . ?
O6 C17 1.261(15) . ?
N1 C0AA 1.334(17) . ?
N1 N2 1.345(15) . ?
N2 C3 1.320(17) . ?
N3 C4 1.329(16) . ?
N3 N4 1.347(14) . ?
N4 C6 1.343(16) . ?
N5 C7 1.352(18) . ?
N5 N6 1.379(15) . ?
N6 C9 1.345(17) . ?
C0AA C2 1.36(2) . ?
C2 C3 1.38(2) . ?
C4 C5 1.378(19) . ?
C5 C6 1.37(2) . ?
C7 C8 1.39(2) . ?
C8 C9 1.36(2) . ?
C10 C11 1.492(18) . ?
C11 C16 1.365(18) . ?
C11 C12 1.383(18) . ?
C12 C13 1.37(2) . ?
C13 C14 1.36(2) . ?
C14 C15 1.36(2) . ?
C15 C16 1.40(2) . ?
C17 C18 1.484(18) . ?
C18 C19 1.37(2) . ?
C18 C23 1.379(19) . ?
C19 C20 1.36(2) . ?
C20 C21 1.389(19) . ?
C21 C22 1.38(2) . ?
C22 C23 1.37(2) . ?
O2W O2W 1.18(17) 2_656 ?

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
N6 Cu1 O2 87.9(4) . . ?
N6 Cu1 N1 176.2(5) . . ?
O2 Cu1 N1 95.1(4) . . ?
N6 Cu1 O1 88.6(4) . . ?
O2 Cu1 O1 176.2(4) . . ?
N1 Cu1 O1 88.4(4) . . ?
N3 Cu2 N2 173.2(4) . . ?
N3 Cu2 O6 92.0(4) . 4_465 ?
N2 Cu2 O6 90.9(4) . 4_465 ?
N3 Cu2 O1 89.0(4) . . ?
N2 Cu2 O1 87.8(4) . . ?
O6 Cu2 O1 176.5(4) 4_465 . ?
N3 Cu2 O3 90.5(4) . 3_566 ?
N2 Cu2 O3 95.5(4) . 3_566 ?
O6 Cu2 O3 95.2(4) 4_465 3_566 ?
O1 Cu2 O3 88.2(4) . 3_566 ?
N5 Cu3 N4 176.5(5) . . ?
N5 Cu3 O5 89.5(5) . 2_646 ?
N4 Cu3 O5 93.1(4) . 2_646 ?
N5 Cu3 O1 88.4(4) . . ?
N4 Cu3 O1 88.8(4) . . ?
O5 Cu3 O1 176.2(4) 2_646 . ?
Cu3 O1 Cu1 114.2(4) . . ?
Cu3 O1 Cu2 116.9(4) . . ?
Cu1 O1 Cu2 115.6(4) . . ?
C10 O2 Cu1 128.4(9) . . ?
C10 O3 Cu2 145.2(11) . 3_566 ?
C21 O4 C14 120.0(11) . . ?
C17 O5 Cu3 121.6(9) . 2_666 ?
C17 O6 Cu2 123.3(8) . 4_666 ?
C0AA N1 N2 107.7(11) . . ?
C0AA N1 Cu1 130.9(9) . . ?
N2 N1 Cu1 121.4(8) . . ?
C3 N2 N1 108.0(11) . . ?
C3 N2 Cu2 130.0(10) . . ?
N1 N2 Cu2 121.5(8) . . ?
C4 N3 N4 108.5(11) . . ?
C4 N3 Cu2 130.2(9) . . ?
N4 N3 Cu2 121.2(9) . . ?
C6 N4 N3 108.0(11) . . ?
C6 N4 Cu3 129.1(9) . . ?
N3 N4 Cu3 122.4(9) . . ?
C7 N5 N6 106.5(12) . . ?
C7 N5 Cu3 132.0(11) . . ?
N6 N5 Cu3 121.6(9) . . ?
C9 N6 N5 108.2(11) . . ?
C9 N6 Cu1 131.6(10) . . ?
N5 N6 Cu1 119.8(8) . . ?
N1 C0AA C2 110.1(14) . . ?
C0AA C2 C3 104.3(14) . . ?
N2 C3 C2 109.9(13) . . ?
N3 C4 C5 108.9(11) . . ?
C6 C5 C4 105.5(12) . . ?
N4 C6 C5 108.9(12) . . ?
N5 C7 C8 110.2(14) . . ?
C9 C8 C7 105.1(14) . . ?
N6 C9 C8 110.1(14) . . ?
O3 C10 O2 125.8(13) . . ?
O3 C10 C11 117.6(12) . . ?
O2 C10 C11 116.6(12) . . ?
C16 C11 C12 117.7(13) . . ?
C16 C11 C10 119.6(12) . . ?
C12 C11 C10 122.7(12) . . ?
C13 C12 C11 122.2(14) . . ?
C14 C13 C12 118.5(16) . . ?
C15 C14 C13 122.2(15) . . ?
C15 C14 O4 119.4(15) . . ?
C13 C14 O4 118.2(15) . . ?
C14 C15 C16 118.3(14) . . ?
C11 C16 C15 121.1(14) . . ?
O6 C17 O5 125.4(12) . . ?
O6 C17 C18 117.6(13) . . ?
O5 C17 C18 116.9(13) . . ?
C19 C18 C23 117.3(13) . . ?
C19 C18 C17 120.8(13) . . ?
C23 C18 C17 121.9(13) . . ?
C20 C19 C18 122.2(14) . . ?
C19 C20 C21 119.6(14) . . ?
O4 C21 C22 115.7(13) . . ?
O4 C21 C20 124.4(13) . . ?
C22 C21 C20 119.9(13) . . ?
C23 C22 C21 118.5(14) . . ?
C22 C23 C18 122.6(14) . . ?

_refine_diff_density_max         0.705
_refine_diff_density_min         -0.661
_refine_diff_density_rms         0.149




# start Validation Reply Form
_vrf_PLAT341_oba                 
;
PROBLEM: Low Bond Precision on  C-C Bonds ...............    0.02195 Ang.  
RESPONSE: This alert is generated due to poor crystal quality.
;
# 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_19rmd001
_database_code_depnum_ccdc_archive 'CCDC 2344978'
loop_
_audit_author_name
_audit_author_address
'Raju Mondal'
;Indian Association for the Cultivation of Science
India
;
_audit_update_record             
;
2024-04-01 deposited with the CCDC.	2024-05-31 downloaded from the CCDC.
;
_audit_creation_date             2019-06-17
_audit_creation_method           
;
Olex2 1.2-beta
(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         'C28 H21 Cu3 F6 N7 O5.5, 0.45(C2 H4 O2)'
_chemical_formula_sum            'C28.90 H22.80 Cu3 F6 N7 O6.40'
_chemical_formula_weight         875.16
_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'
Cu Cu 0.3201 1.2651 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
F F 0.0171 0.0103 '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      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                   9.4907(10)
_cell_length_b                   13.7197(14)
_cell_length_c                   16.1356(17)
_cell_angle_alpha                114.378(4)
_cell_angle_beta                 92.674(4)
_cell_angle_gamma                107.127(4)
_cell_volume                     1794.4(3)
_cell_formula_units_Z            2
_cell_measurement_reflns_used    9942
_cell_measurement_temperature    120
_cell_measurement_theta_max      25.36
_cell_measurement_theta_min      2.29
_shelx_estimated_absorpt_T_max   0.806
_shelx_estimated_absorpt_T_min   0.631
_exptl_absorpt_coefficient_mu    1.844
_exptl_absorpt_correction_T_max  0.8486
_exptl_absorpt_correction_T_min  0.6913
_exptl_absorpt_correction_type   integration
_exptl_absorpt_process_details   
; SADABS-2016/2 (Bruker, 2016) was used for absorption correction. wR2(int) 
  was 0.0892 before and 0.0701 after correction. The Ratio of minimum to maximum 
  transmission is 0.8146. The λ/2 correction factor is Not present.
;

loop_
_exptl_crystal_face_index_h
_exptl_crystal_face_index_k
_exptl_crystal_face_index_l
_exptl_crystal_face_perp_dist
0.00 -1.00 1.00 0.0520
0.00 1.00 -1.00 0.0610
1.00 -1.00 1.00 0.1110
1.00 2.00 2.00 0.0720
0.00 0.00 1.00 0.0670
0.00 0.00 -1.00 0.1440
1.00 -1.00 0.00 0.0920
-2.00 1.00 0.00 0.1070
1.00 -2.00 0.00 0.0710
2.00 -1.00 -2.00 0.0930
-2.00 1.00 -1.00 0.1090
-2.00 -2.00 1.00 0.1180

_exptl_absorpt_special_details   ?
_exptl_crystal_colour            blue
_exptl_crystal_density_diffrn    1.620
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       wedge
_exptl_crystal_F_000             875
_exptl_crystal_size_max          0.275
_exptl_crystal_size_mid          0.242
_exptl_crystal_size_min          0.122
_exptl_special_details           
; Data were collected in shutterless mode. Full sphere of reciprocal space was 
  nominally covered by 4 runs of 170 narrow-frame ω-scans (scan width 1°, 10s 
  exposure), every run at a different φ angle. Two runs of 358 φ-scans (scan 
  width 1°, 1.5s exposure) were used for scaling overflowing intensities. 
  Crystal to detector distance 3.49 cm.
;
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0581
_diffrn_reflns_av_unetI/netI     0.0682
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -11
_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            26677
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_theta_full        25.0
_diffrn_reflns_theta_max         25.0
_diffrn_reflns_theta_min         2.289
_diffrn_ambient_temperature      120
_diffrn_detector                 'Bruker PHOTON 100 CMOS'
_diffrn_detector_area_resol_mean 10.4
_diffrn_detector_type            'CMOS sensor'
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device       '3-circle area detector diffractometer'
_diffrn_measurement_device_type  'Bruker D8 Venture'
_diffrn_measurement_method       'φ and ω scans'
_diffrn_measurement_specimen_support 'MiTeGen loop'
_diffrn_radiation_monochromator  'focusing mirrors'
_diffrn_radiation_probe          X-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_source                   'microfocus sealed X-ray tube'
_diffrn_source_type              'Incoatec I\mS microsource'
_diffrn_standards_number         0
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                4811
_reflns_number_total             6317
_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 (Bruker, 2017)'
_computing_data_collection       'APEX3 v.2016.1-0 (Bruker, 2016)'
_computing_data_reduction        'SAINT v8.38A (Bruker, 2017)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL 2018/3 (Sheldrick, 2015a)'
_computing_structure_solution    'ShelXT 2018/2 (Sheldrick, 2015)'
_refine_diff_density_max         0.599
_refine_diff_density_min         -0.655
_refine_diff_density_rms         0.092
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.135
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     512
_refine_ls_number_reflns         6317
_refine_ls_number_restraints     31
_refine_ls_R_factor_all          0.0734
_refine_ls_R_factor_gt           0.0486
_refine_ls_restrained_S_all      1.133
_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)+6.5259P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1132
_refine_ls_wR_factor_ref         0.1252
_refine_special_details          
; The apical coordination site at Cu(3) is shared by neutral pyrazole (50%) 
 and acetic acid (25%) ligands, the coordinated N and O atoms coinciding. 
 The void is occupied by an acetic acid molecule (45%), forming an H-bonded 
 dimer with ints inversion equivalent. The μ-hydroxyl hydrogen - refall, 
 other H atoms - riding.  
;
_olex2_refinement_description    
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All N(H) groups
 At 1.5 times of:
  All C(H,H,H) groups, All O(H) groups
2. Shared sites
{N7, O8}
3. Restrained distances
 O1-H1
 0.85 with sigma of 0.02
4. Uiso/Uaniso restraints and constraints
Uanis(N7) = Uanis(O8)
5. Rigid body (RIGU) restrains
 N7, N8, C30, C31, C32
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
6. Others
 Fixed Sof: N7(0.5) N8(0.5) H8A(0.5) C30(0.5) H30(0.5) C31(0.5) H31(0.5)
 C32(0.5) H32(0.5) O8(0.25) O9(0.25) H9A(0.25) C33(0.25) C34(0.25) H34A(0.25)
 H34B(0.25) H34C(0.25) O6(0.45) O7(0.45) H7A(0.45) C27(0.45) C29(0.45)
 H29A(0.45) H29B(0.45) H29C(0.45)
7.a Riding coordinates:
 O9(H9A), O7(H7A)
7.b Me refined with riding coordinates:
 C34(H34A,H34B,H34C), C29(H29A,H29B,H29C)
7.c Aromatic/amide H refined with riding coordinates:
 C1(H1A), C2(H2), C3(H3), C4(H4), C5(H5), C6(H6), C7(H7), C8(H8), C9(H9),
 C12(H12), C13(H13), C15(H15), C16(H16), C22(H22), C23(H23), C25(H25), C26(H26),
  N8(H8A), C30(H30), C31(H31), C32(H32)
;
_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 0.25049(7) 0.59808(5) 1.07421(4) 0.02176(16) Uani 1 1 d . . . . .
Cu2 Cu 0.31965(7) 0.41875(5) 0.87601(4) 0.02801(18) Uani 1 1 d . . . . .
Cu3 Cu 0.03990(7) 0.31666(5) 0.97218(5) 0.03030(19) Uani 1 1 d . . . . .
F1 F 0.4643(5) 0.3784(3) 0.3529(3) 0.0620(11) Uani 1 1 d . . . . .
F2 F 0.6886(5) 0.4925(3) 0.4264(3) 0.0681(13) Uani 1 1 d . . . . .
F3 F 0.6481(5) 0.3875(3) 0.2795(3) 0.0796(15) Uani 1 1 d . . . . .
F4 F 0.9031(4) 0.4045(3) 0.4086(3) 0.0671(12) Uani 1 1 d . . . . .
F5 F 0.8110(5) 0.2591(4) 0.2763(3) 0.0772(14) Uani 1 1 d . . . . .
F6 F 0.8449(4) 0.2360(3) 0.3984(3) 0.0600(11) Uani 1 1 d . . . . .
O1 O 0.2352(4) 0.4386(3) 0.9905(2) 0.0227(8) Uani 1 1 d D . . . .
H1 H 0.293(5) 0.429(5) 1.026(3) 0.039(18) Uiso 1 1 d D . . . .
O2 O 0.3843(4) 0.3922(3) 0.7581(3) 0.0423(10) Uani 1 1 d . . . . .
O3 O 0.6217(5) 0.4258(4) 0.8141(3) 0.0553(13) Uani 1 1 d . . . . .
O4 O 0.1587(4) -0.1916(3) 0.0626(2) 0.0335(9) Uani 1 1 d . . . . .
O5 O 0.2657(4) -0.2442(3) 0.1556(2) 0.0309(9) Uani 1 1 d . . . . .
N1 N 0.4217(5) 0.6520(3) 1.0222(3) 0.0293(10) Uani 1 1 d . . . . .
N2 N 0.4378(5) 0.5808(4) 0.9369(3) 0.0271(10) Uani 1 1 d . . . . .
N3 N 0.2109(5) 0.2569(4) 0.8269(3) 0.0351(11) Uani 1 1 d . . . . .
N4 N 0.1016(5) 0.2158(4) 0.8676(3) 0.0372(12) Uani 1 1 d . . . . .
N5 N -0.0156(5) 0.4264(3) 1.0744(3) 0.0243(9) Uani 1 1 d . . . . .
N6 N 0.0668(5) 0.5401(3) 1.1133(3) 0.0211(9) Uani 1 1 d . . . . .
C1 C 0.5156(6) 0.7570(5) 1.0458(4) 0.0318(13) Uani 1 1 d . . . . .
H1A H 0.526663 0.821870 1.102427 0.038 Uiso 1 1 calc R . . . .
C2 C 0.5945(7) 0.7581(5) 0.9764(4) 0.0402(15) Uani 1 1 d . . . . .
H2 H 0.668604 0.821297 0.975173 0.048 Uiso 1 1 calc R . . . .
C3 C 0.5405(6) 0.6456(5) 0.9085(4) 0.0348(13) Uani 1 1 d . . . . .
H3 H 0.571577 0.618280 0.850561 0.042 Uiso 1 1 calc R . . . .
C4 C 0.2300(7) 0.1672(5) 0.7583(4) 0.0487(17) Uani 1 1 d . . . . .
H4 H 0.298637 0.172058 0.717942 0.058 Uiso 1 1 calc R . . . .
C5 C 0.1362(8) 0.0673(5) 0.7548(5) 0.060(2) Uani 1 1 d . . . . .
H5 H 0.128115 -0.008338 0.713876 0.072 Uiso 1 1 calc R . . . .
C6 C 0.0568(7) 0.1016(5) 0.8235(5) 0.0524(18) Uani 1 1 d . . . . .
H6 H -0.019220 0.051534 0.838007 0.063 Uiso 1 1 calc R . . . .
C7 C -0.1165(6) 0.4105(4) 1.1269(4) 0.0318(13) Uani 1 1 d . . . . .
H7 H -0.187667 0.338866 1.115388 0.038 Uiso 1 1 calc R . . . .
C8 C -0.1019(6) 0.5137(4) 1.2003(3) 0.0275(12) Uani 1 1 d . . . . .
H8 H -0.159053 0.527304 1.248056 0.033 Uiso 1 1 calc R . . . .
C9 C 0.0147(6) 0.5926(4) 1.1885(3) 0.0241(11) Uani 1 1 d . . . . .
H9 H 0.052037 0.672305 1.228094 0.029 Uiso 1 1 calc R . . . .
C10 C 0.5187(6) 0.3971(5) 0.7500(4) 0.0320(13) Uani 1 1 d . . . . .
C11 C 0.5514(6) 0.3686(4) 0.6544(3) 0.0267(12) Uani 1 1 d . . . . .
C12 C 0.4359(6) 0.3147(4) 0.5774(4) 0.0304(12) Uani 1 1 d . . . . .
H12 H 0.334256 0.294730 0.584863 0.036 Uiso 1 1 calc R . . . .
C13 C 0.4680(6) 0.2902(4) 0.4906(4) 0.0298(12) Uani 1 1 d . . . . .
H13 H 0.387867 0.252166 0.438476 0.036 Uiso 1 1 calc R . . . .
C14 C 0.6146(6) 0.3199(4) 0.4773(3) 0.0259(11) Uani 1 1 d . . . . .
C15 C 0.7306(6) 0.3753(5) 0.5543(4) 0.0326(13) Uani 1 1 d . . . . .
H15 H 0.832084 0.398280 0.547065 0.039 Uiso 1 1 calc R . . . .
C16 C 0.6977(6) 0.3969(5) 0.6412(4) 0.0324(13) Uani 1 1 d . . . . .
H16 H 0.777683 0.432105 0.693084 0.039 Uiso 1 1 calc R . . . .
C17 C 0.6385(6) 0.2951(4) 0.3779(4) 0.0337(13) Uani 1 1 d . . . . .
C18 C 0.6076(10) 0.3886(5) 0.3586(4) 0.055(2) Uani 1 1 d . . . . .
C19 C 0.8007(8) 0.2996(6) 0.3659(4) 0.0514(18) Uani 1 1 d . . . . .
C20 C 0.2508(6) -0.1707(4) 0.1318(4) 0.0290(12) Uani 1 1 d . . . . .
C21 C 0.3513(6) -0.0502(4) 0.1918(3) 0.0280(12) Uani 1 1 d . . . . .
C22 C 0.4369(6) -0.0239(4) 0.2747(4) 0.0332(13) Uani 1 1 d . . . . .
H22 H 0.434682 -0.082898 0.291570 0.040 Uiso 1 1 calc R . . . .
C23 C 0.5254(6) 0.0868(4) 0.3331(4) 0.0328(13) Uani 1 1 d . . . . .
H23 H 0.581457 0.103527 0.390629 0.039 Uiso 1 1 calc R . . . .
C24 C 0.5339(6) 0.1743(4) 0.3092(4) 0.0290(12) Uani 1 1 d . . . . .
C25 C 0.4528(7) 0.1468(5) 0.2244(4) 0.0395(15) Uani 1 1 d . . . . .
H25 H 0.460860 0.204694 0.205121 0.047 Uiso 1 1 calc R . . . .
C26 C 0.3601(7) 0.0361(5) 0.1673(4) 0.0351(13) Uani 1 1 d . . . . .
H26 H 0.301693 0.019417 0.110593 0.042 Uiso 1 1 calc R . . . .
N7 N 0.0993(8) 0.2606(6) 1.0891(5) 0.0574(18) Uani 0.5 1 d . U P A 1
N8 N 0.1546(13) 0.3410(10) 1.1716(8) 0.057(3) Uani 0.5 1 d . U P A 1
H8A H 0.192987 0.413817 1.185587 0.069 Uiso 0.5 1 calc R . P A 1
C30 C 0.036(2) 0.1611(17) 1.0958(15) 0.066(4) Uani 0.5 1 d . U P A 1
H30 H -0.021659 0.088663 1.046834 0.080 Uiso 0.5 1 calc R . P A 1
C31 C 0.074(3) 0.1878(19) 1.1890(18) 0.074(5) Uani 0.5 1 d . U P A 1
H31 H 0.052323 0.136304 1.215685 0.089 Uiso 0.5 1 calc R . P A 1
C32 C 0.1459(19) 0.2994(16) 1.2329(13) 0.067(4) Uani 0.5 1 d . U P A 1
H32 H 0.184821 0.342451 1.297649 0.081 Uiso 0.5 1 calc R . P A 1
O8 O 0.0993(8) 0.2606(6) 1.0891(5) 0.0574(18) Uani 0.25 1 d . . P A 2
O9 O -0.092(3) 0.126(2) 1.0949(17) 0.085(7) Uiso 0.25 1 d . . P A 2
H9A H -0.147325 0.141347 1.131996 0.127 Uiso 0.25 1 d R . P A 2
C33 C 0.049(3) 0.208(3) 1.133(2) 0.038(8) Uiso 0.25 1 d . . P A 2
C34 C 0.122(6) 0.225(4) 1.224(3) 0.076(17) Uiso 0.25 1 d . . P A 2
H34A H 0.056204 0.171244 1.242462 0.115 Uiso 0.25 1 calc R . P A 2
H34B H 0.218148 0.213059 1.218456 0.115 Uiso 0.25 1 calc R . P A 2
H34C H 0.138637 0.303430 1.270372 0.115 Uiso 0.25 1 calc R . P A 2
O6 O 0.679(3) -0.0262(15) 0.4746(12) 0.140(8) Uani 0.45 1 d . . P B 1
O7 O 0.655(3) 0.1321(18) 0.5720(11) 0.187(11) Uani 0.45 1 d . . P B 1
H7A H 0.566907 0.090948 0.551635 0.280 Uiso 0.45 1 d R . P B 1
C27 C 0.744(5) 0.069(3) 0.5316(19) 0.123(12) Uani 0.45 1 d . . P B 1
C29 C 0.911(4) 0.127(3) 0.5634(19) 0.154(14) Uani 0.45 1 d . . P B 1
H29A H 0.933179 0.205215 0.610930 0.232 Uiso 0.45 1 calc R . P B 1
H29B H 0.950819 0.085057 0.589351 0.232 Uiso 0.45 1 calc R . P B 1
H29C H 0.956980 0.127597 0.510533 0.232 Uiso 0.45 1 calc R . P B 1


_geom_special_details            
;
 All esds (except the esd in the dihedral angle between two l.s. planes)
 are estimated using the full covariance matrix.  The cell esds are taken
 into account individually in the estimation of esds in distances, angles
 and torsion angles; correlations between esds in cell parameters are only
 used when they are defined by crystal symmetry.  An approximate (isotropic)
 treatment of cell esds is used for estimating esds involving l.s. planes.
;
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Cu1 O1 1.997(3) . ?
Cu1 O3 2.312(4) 2_667 ?
Cu1 O5 1.970(3) 1_566 ?
Cu1 N1 1.955(4) . ?
Cu1 N6 1.942(4) . ?
Cu2 O1 1.995(3) . ?
Cu2 O2 1.949(4) . ?
Cu2 N2 1.947(4) . ?
Cu2 N3 1.935(5) . ?
Cu3 O1 2.009(3) . ?
Cu3 O4 2.003(4) 2_556 ?
Cu3 N4 1.936(4) . ?
Cu3 N5 1.940(4) . ?
Cu3 N7 2.413(7) . ?
Cu3 O8 2.413(7) . ?
F1 C18 1.320(9) . ?
F2 C18 1.345(7) . ?
F3 C18 1.346(7) . ?
F4 C19 1.336(7) . ?
F5 C19 1.338(7) . ?
F6 C19 1.336(8) . ?
O2 C10 1.273(6) . ?
O3 C10 1.233(7) . ?
O4 C20 1.261(7) . ?
O5 C20 1.257(6) . ?
N1 N2 1.367(6) . ?
N1 C1 1.332(6) . ?
N2 C3 1.348(7) . ?
N3 N4 1.360(6) . ?
N3 C4 1.341(7) . ?
N4 C6 1.343(7) . ?
N5 N6 1.366(5) . ?
N5 C7 1.337(6) . ?
N6 C9 1.334(6) . ?
C1 C2 1.379(7) . ?
C2 C3 1.390(8) . ?
C4 C5 1.373(9) . ?
C5 C6 1.369(9) . ?
C7 C8 1.383(7) . ?
C8 C9 1.385(7) . ?
C10 C11 1.499(7) . ?
C11 C12 1.390(7) . ?
C11 C16 1.380(7) . ?
C12 C13 1.370(7) . ?
C13 C14 1.384(7) . ?
C14 C15 1.389(7) . ?
C14 C17 1.540(7) . ?
C15 C16 1.380(7) . ?
C17 C18 1.539(9) . ?
C17 C19 1.547(9) . ?
C17 C24 1.540(7) . ?
C20 C21 1.498(7) . ?
C21 C22 1.380(8) . ?
C21 C26 1.378(7) . ?
C22 C23 1.376(7) . ?
C23 C24 1.387(7) . ?
C24 C25 1.383(8) . ?
C25 C26 1.383(7) . ?
N7 N8 1.283(13) . ?
N7 C30 1.371(18) . ?
N8 C32 1.325(19) . ?
C30 C31 1.39(3) . ?
C31 C32 1.32(3) . ?
O8 C33 1.22(3) . ?
O9 C33 1.38(4) . ?
C33 C34 1.48(5) . ?
O6 C27 1.19(3) . ?
O7 C27 1.37(3) . ?
C27 C29 1.50(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 Cu1 O3 84.93(15) . 2_667 ?
O5 Cu1 O1 179.35(15) 1_566 . ?
O5 Cu1 O3 95.63(16) 1_566 2_667 ?
N1 Cu1 O1 88.40(15) . . ?
N1 Cu1 O3 98.21(18) . 2_667 ?
N1 Cu1 O5 91.18(16) . 1_566 ?
N6 Cu1 O1 89.94(15) . . ?
N6 Cu1 O3 87.60(17) . 2_667 ?
N6 Cu1 O5 90.43(15) . 1_566 ?
N6 Cu1 N1 173.79(18) . . ?
O2 Cu2 O1 175.02(16) . . ?
N2 Cu2 O1 88.69(15) . . ?
N2 Cu2 O2 94.63(17) . . ?
N3 Cu2 O1 87.64(16) . . ?
N3 Cu2 O2 89.35(18) . . ?
N3 Cu2 N2 174.0(2) . . ?
O1 Cu3 N7 101.0(2) . . ?
O1 Cu3 O8 101.0(2) . . ?
O4 Cu3 O1 172.88(15) 2_556 . ?
O4 Cu3 N7 85.3(2) 2_556 . ?
O4 Cu3 O8 85.3(2) 2_556 . ?
N4 Cu3 O1 86.89(16) . . ?
N4 Cu3 O4 88.59(17) . 2_556 ?
N4 Cu3 N5 175.85(19) . . ?
N4 Cu3 N7 101.0(2) . . ?
N4 Cu3 O8 101.0(2) . . ?
N5 Cu3 O1 89.86(15) . . ?
N5 Cu3 O4 94.40(16) . 2_556 ?
N5 Cu3 N7 82.1(2) . . ?
N5 Cu3 O8 82.1(2) . . ?
Cu1 O1 Cu3 115.77(16) . . ?
Cu2 O1 Cu1 115.19(17) . . ?
Cu2 O1 Cu3 115.03(16) . . ?
C10 O2 Cu2 121.1(4) . . ?
C10 O3 Cu1 154.7(5) . 2_667 ?
C20 O4 Cu3 118.0(3) . 2_556 ?
C20 O5 Cu1 127.6(3) . 1_544 ?
N2 N1 Cu1 119.3(3) . . ?
C1 N1 Cu1 130.7(4) . . ?
C1 N1 N2 108.5(4) . . ?
N1 N2 Cu2 121.8(3) . . ?
C3 N2 Cu2 131.1(3) . . ?
C3 N2 N1 107.0(4) . . ?
N4 N3 Cu2 121.2(3) . . ?
C4 N3 Cu2 131.0(4) . . ?
C4 N3 N4 107.5(5) . . ?
N3 N4 Cu3 121.6(3) . . ?
C6 N4 Cu3 131.0(4) . . ?
C6 N4 N3 107.5(5) . . ?
N6 N5 Cu3 121.2(3) . . ?
C7 N5 Cu3 130.3(3) . . ?
C7 N5 N6 107.9(4) . . ?
N5 N6 Cu1 121.7(3) . . ?
C9 N6 Cu1 129.1(3) . . ?
C9 N6 N5 108.0(4) . . ?
N1 C1 C2 110.3(5) . . ?
C1 C2 C3 104.1(5) . . ?
N2 C3 C2 110.1(5) . . ?
N3 C4 C5 110.3(6) . . ?
C6 C5 C4 104.4(5) . . ?
N4 C6 C5 110.4(6) . . ?
N5 C7 C8 109.9(4) . . ?
C7 C8 C9 104.4(4) . . ?
N6 C9 C8 109.8(4) . . ?
O2 C10 C11 115.7(5) . . ?
O3 C10 O2 125.4(5) . . ?
O3 C10 C11 119.0(5) . . ?
C12 C11 C10 121.1(5) . . ?
C16 C11 C10 120.5(5) . . ?
C16 C11 C12 118.4(5) . . ?
C13 C12 C11 120.3(5) . . ?
C12 C13 C14 121.4(5) . . ?
C13 C14 C15 118.6(5) . . ?
C13 C14 C17 117.3(5) . . ?
C15 C14 C17 123.9(5) . . ?
C16 C15 C14 119.7(5) . . ?
C15 C16 C11 121.6(5) . . ?
C14 C17 C19 112.7(5) . . ?
C14 C17 C24 110.0(4) . . ?
C18 C17 C14 106.5(4) . . ?
C18 C17 C19 108.6(5) . . ?
C18 C17 C24 112.7(5) . . ?
C24 C17 C19 106.6(4) . . ?
F1 C18 F2 108.1(6) . . ?
F1 C18 F3 107.9(6) . . ?
F1 C18 C17 112.0(5) . . ?
F2 C18 F3 105.9(5) . . ?
F2 C18 C17 110.5(6) . . ?
F3 C18 C17 112.1(6) . . ?
F4 C19 F5 106.4(5) . . ?
F4 C19 C17 113.9(6) . . ?
F5 C19 C17 111.0(6) . . ?
F6 C19 F4 106.8(6) . . ?
F6 C19 F5 106.7(6) . . ?
F6 C19 C17 111.7(5) . . ?
O4 C20 C21 119.1(5) . . ?
O5 C20 O4 124.9(5) . . ?
O5 C20 C21 116.0(5) . . ?
C22 C21 C20 119.5(5) . . ?
C26 C21 C20 121.9(5) . . ?
C26 C21 C22 118.6(5) . . ?
C23 C22 C21 120.8(5) . . ?
C22 C23 C24 120.9(5) . . ?
C23 C24 C17 117.3(5) . . ?
C25 C24 C17 124.5(5) . . ?
C25 C24 C23 118.1(5) . . ?
C26 C25 C24 120.7(5) . . ?
C21 C26 C25 120.8(5) . . ?
N8 N7 Cu3 116.4(7) . . ?
N8 N7 C30 107.7(13) . . ?
C30 N7 Cu3 130.6(11) . . ?
N7 N8 C32 110.8(13) . . ?
N7 C30 C31 106.0(18) . . ?
C32 C31 C30 106.4(18) . . ?
C31 C32 N8 108.7(17) . . ?
C33 O8 Cu3 145.9(15) . . ?
O8 C33 O9 116(3) . . ?
O8 C33 C34 127(3) . . ?
O9 C33 C34 117(3) . . ?
O6 C27 O7 116(4) . . ?
O6 C27 C29 127(3) . . ?
O7 C27 C29 117(3) . . ?

_olex2_diffrn_ambient_temperature_device 'Oxford Cryosystems'
_olex2_submission_special_instructions 'No special instructions were received'
####################################################################### 
# 
# 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_rm200223_0m_b
_database_code_depnum_ccdc_archive 'CCDC 2344980'
loop_
_audit_author_name
_audit_author_address
'Raju Mondal'
;Indian Association for the Cultivation of Science
India
;
_audit_update_record             
;
2024-04-01 deposited with the CCDC.	2024-05-31 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2016/6
_shelx_SHELXL_version_number     2016/6
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C31 H38 Cu3 N9 O11 S'
_chemical_formula_weight         935.38

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Cu Cu 0.3201 1.2651 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_H-M_alt        'P -1'
_space_group_name_Hall           '-P 1'

_shelx_space_group_comment       
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;

loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, -y, -z'

_cell_length_a                   9.221(2)
_cell_length_b                   12.471(4)
_cell_length_c                   17.304(5)
_cell_angle_alpha                77.215(8)
_cell_angle_beta                 88.784(7)
_cell_angle_gamma                78.935(8)
_cell_volume                     1904.0(9)
_cell_formula_units_Z            2
_cell_measurement_temperature    120(2)
_cell_measurement_reflns_used    3942
_cell_measurement_theta_min      2.500
_cell_measurement_theta_max      30.160

_exptl_crystal_description       Needle
_exptl_crystal_colour            Blue
_exptl_crystal_density_meas      'not measured'
_exptl_crystal_density_method    'not measured'
_exptl_crystal_density_diffrn    1.632
_exptl_crystal_F_000             956
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.30
_exptl_crystal_size_mid          0.20
_exptl_crystal_size_min          0.16
_exptl_absorpt_coefficient_mu    1.784
_shelx_estimated_absorpt_T_min   0.6016
_shelx_estimated_absorpt_T_max   0.7468
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.80557043
_exptl_absorpt_correction_T_max  1.00000000
_exptl_absorpt_process_details   
'SADABS v.2.03 (Bruker, 2001), R(int)= 0.1198 before correction'

_exptl_absorpt_special_details   ?
_diffrn_ambient_temperature      120(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_source                   'fine-focus sealed tube'
_diffrn_measurement_device_type  'Bruker APEX-2 CCD area detector'
_diffrn_measurement_method       '/w scans'
_diffrn_detector_area_resol_mean 8
_diffrn_reflns_number            17302
_diffrn_reflns_av_unetI/netI     0.1362
_diffrn_reflns_av_R_equivalents  0.0892
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_theta_min         2.298
_diffrn_reflns_theta_max         25.393
_diffrn_reflns_theta_full        25.242
_diffrn_measured_fraction_theta_max 0.984
_diffrn_measured_fraction_theta_full 0.988
_diffrn_reflns_Laue_measured_fraction_max 0.984
_diffrn_reflns_Laue_measured_fraction_full 0.988
_diffrn_reflns_point_group_measured_fraction_max 0.984
_diffrn_reflns_point_group_measured_fraction_full 0.988
_reflns_number_total             6881
_reflns_number_gt                3865
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_max     .
_reflns_Friedel_fraction_full    .

_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
;

_computing_data_collection       'Bruker APEX-3'
_computing_cell_refinement       'Bruker APEX-3'
_computing_data_reduction        'Bruker SHELXTL'
_computing_structure_solution    'SHELXT 2014/5 (Sheldrick, 2014)'
_computing_structure_refinement  'SHELXL-2016/6 (Sheldrick, 2016)'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_refine_special_details          ?
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0511P)²+16.4309P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
_atom_sites_solution_hydrogens   mixed
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_number_reflns         6881
_refine_ls_number_parameters     502
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.1674
_refine_ls_R_factor_gt           0.0880
_refine_ls_wR_factor_ref         0.1998
_refine_ls_wR_factor_gt          0.1754
_refine_ls_goodness_of_fit_ref   1.030
_refine_ls_restrained_S_all      1.030
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
Cu01 Cu 0.24625(12) 0.35537(10) 0.31881(6) 0.0287(3) Uani 1 1 d . . . . .
Cu02 Cu 0.23706(13) 0.30024(10) 1.13612(7) 0.0321(3) Uani 1 1 d . . . . .
Cu03 Cu -0.00149(13) 0.22545(11) 0.27959(7) 0.0385(4) Uani 1 1 d . . . . .
S004 S 0.7879(3) 0.2873(2) 0.73081(14) 0.0328(6) Uani 1 1 d . . . . .
O005 O 0.1270(7) 0.3337(5) 1.2314(4) 0.0327(16) Uani 1 1 d . . . . .
H005 H 0.058201 0.406999 1.212230 0.049 Uiso 1 1 calc R U . . .
O006 O 0.3632(7) 0.3571(5) 0.4111(3) 0.0324(16) Uani 1 1 d . . . . .
O007 O 0.8101(7) 0.4016(6) 0.7159(4) 0.0378(17) Uani 1 1 d . . . . .
O008 O 0.2199(7) 0.1053(6) 0.3390(4) 0.0409(18) Uani 1 1 d . . . . .
H00A H 0.280518 0.088984 0.301945 0.061 Uiso 1 1 d R U . . .
H00B H 0.266615 0.142165 0.364461 0.061 Uiso 1 1 d R U . . .
O009 O 0.3986(7) 0.1713(6) 0.4428(4) 0.0385(17) Uani 1 1 d . . . . .
O00A O 0.3361(8) 0.2867(6) 1.0370(4) 0.0433(18) Uani 1 1 d . . . . .
N00B N 0.4160(8) 0.3550(6) 0.2528(4) 0.0281(18) Uani 1 1 d . . . . .
O00C O 0.9126(7) 0.1968(6) 0.7349(4) 0.0428(18) Uani 1 1 d . . . . .
N00D N 0.4123(8) 0.3422(7) 0.1765(4) 0.0311(19) Uani 1 1 d . . . . .
N00E N -0.0368(9) 0.3030(7) 0.3670(5) 0.039(2) Uani 1 1 d . . . . .
N00F N 0.0728(9) 0.3550(7) 0.3835(5) 0.039(2) Uani 1 1 d . . . . .
O00G O 0.1206(9) 0.4813(7) 1.0648(5) 0.063(2) Uani 1 1 d . . . . .
N00H N 0.0927(9) 0.2110(7) 0.1221(4) 0.035(2) Uani 1 1 d . . . . .
O10 O 0.3964(10) 0.0490(7) 1.2234(4) 0.065(2) Uani 1 1 d . . . . .
H10 H 0.389210 0.061300 1.173806 0.098 Uiso 1 1 calc R U . . .
O00J O -0.0739(9) 0.5239(8) 1.1853(6) 0.070(3) Uani 1 1 d . . . . .
C00K C 0.5778(10) 0.3735(8) 0.6144(5) 0.030(2) Uani 1 1 d . . . . .
H00K H 0.575586 0.443236 0.628476 0.036 Uiso 1 1 calc R U . . .
C00L C 0.6661(9) 0.2773(8) 0.6556(5) 0.024(2) Uani 1 1 d . . . . .
N00M N -0.0015(9) 0.1763(8) 0.1809(5) 0.045(2) Uani 1 1 d . . . . .
N00N N -0.1131(10) 0.1117(9) 0.3356(6) 0.056(3) Uani 1 1 d . . . . .
C00O C 0.4958(10) 0.2673(8) 0.5284(5) 0.026(2) Uani 1 1 d . . . . .
O00P O 0.4537(11) 0.1102(7) 1.0714(5) 0.075(3) Uani 1 1 d . . . . .
C00Q C 0.6374(10) 0.3731(9) 0.1976(6) 0.039(3) Uani 1 1 d . . . . .
H00Q H 0.736424 0.383798 0.190061 0.047 Uiso 1 1 calc R U . . .
C00R C 0.4908(10) 0.3660(8) 0.5509(5) 0.029(2) Uani 1 1 d . . . . .
H00R H 0.426820 0.431486 0.522895 0.035 Uiso 1 1 calc R U . . .
C00S C 0.5524(10) 0.3749(8) 0.2653(6) 0.035(2) Uani 1 1 d . . . . .
H00S H 0.585364 0.388281 0.313298 0.042 Uiso 1 1 calc R U . . .
C00T C 0.5431(11) 0.3519(8) 0.1443(5) 0.033(2) Uani 1 1 d . . . . .
H00T H 0.567985 0.345189 0.091823 0.039 Uiso 1 1 calc R U . . .
C00U C 0.6855(10) 0.2618(9) 0.8183(5) 0.033(2) Uani 1 1 d . . . . .
C00V C 0.4118(10) 0.2609(9) 0.4555(5) 0.033(2) Uani 1 1 d . . . . .
N00W N -0.1854(12) 0.6783(11) 1.2276(8) 0.069(3) Uani 1 1 d . . . . .
C00X C 0.5826(11) 0.1704(9) 0.5724(5) 0.038(3) Uani 1 1 d . . . . .
H00X H 0.583398 0.100217 0.559285 0.046 Uiso 1 1 calc R U . . .
C00Y C 0.5889(11) 0.3505(8) 0.8379(6) 0.038(3) Uani 1 1 d . . . . .
H00Y H 0.578479 0.423658 0.805126 0.045 Uiso 1 1 calc R U . . .
C00Z C 0.7012(11) 0.1522(9) 0.8648(5) 0.039(3) Uani 1 1 d . . . . .
H00Z H 0.768806 0.092064 0.850943 0.047 Uiso 1 1 calc R U . . .
C010 C 0.6156(12) 0.1343(9) 0.9313(6) 0.044(3) Uani 1 1 d . . . . .
H010 H 0.621815 0.060753 0.962869 0.053 Uiso 1 1 calc R U . . .
C011 C 0.0677(12) 0.1639(10) 0.0619(6) 0.047(3) Uani 1 1 d . . . . .
H011 H 0.120383 0.171564 0.013832 0.057 Uiso 1 1 calc R U . . .
C012 C 0.4317(12) 0.2021(11) 1.0268(6) 0.044(3) Uani 1 1 d . . . . .
C013 C 0.6691(11) 0.1769(9) 0.6361(6) 0.040(3) Uani 1 1 d . . . . .
H013 H 0.730095 0.111122 0.665854 0.048 Uiso 1 1 calc R U . . .
C014 C -0.0801(11) 0.1112(10) 0.1537(7) 0.055(3) Uani 1 1 d . . . . .
H014 H -0.152094 0.075424 0.183502 0.066 Uiso 1 1 calc R U . . .
C015 C -0.1383(12) 0.3122(10) 0.4209(7) 0.051(3) Uani 1 1 d . . . . .
H015 H -0.226441 0.282883 0.422566 0.061 Uiso 1 1 calc R U . . .
C016 C 0.0335(12) 0.3959(10) 0.4476(6) 0.052(3) Uani 1 1 d . . . . .
H016 H 0.089495 0.437048 0.471347 0.062 Uiso 1 1 calc R U . . .
C017 C 0.5203(11) 0.2240(9) 0.9518(5) 0.034(2) Uani 1 1 d . . . . .
C018 C -0.1009(12) 0.3696(10) 0.4746(7) 0.054(3) Uani 1 1 d . . . . .
H018 H -0.154166 0.387036 0.519216 0.064 Uiso 1 1 calc R U . . .
C019 C 0.5077(12) 0.3313(9) 0.9060(6) 0.042(3) Uani 1 1 d . . . . .
H019 H 0.443232 0.391906 0.921236 0.051 Uiso 1 1 calc R U . . .
N01A N -0.0317(17) 0.0101(11) 0.3834(9) 0.116(6) Uani 1 1 d . . . . .
H01A H 0.065505 -0.006360 0.383791 0.139 Uiso 1 1 calc R U . . .
C01B C -0.0440(13) 0.1031(10) 0.0787(7) 0.056(3) Uani 1 1 d . . . . .
H01B H -0.085404 0.064785 0.045594 0.067 Uiso 1 1 calc R U . . .
C01C C -0.1112(17) -0.0574(15) 0.4269(8) 0.083(5) Uani 1 1 d . . . . .
H01C H -0.074807 -0.131805 0.455451 0.099 Uiso 1 1 calc R U . . .
C01D C 0.1990(14) 0.5537(11) 1.0126(7) 0.065(4) Uani 1 1 d . . . . .
H01D H 0.133673 0.597909 0.968270 0.097 Uiso 1 1 calc R U . . .
H01E H 0.284355 0.509019 0.992231 0.097 Uiso 1 1 calc R U . . .
H01F H 0.233142 0.604084 1.041244 0.097 Uiso 1 1 calc R U . . .
C01E C -0.245(2) -0.0055(13) 0.4241(10) 0.107(6) Uani 1 1 d . . . . .
H01G H -0.326321 -0.025251 0.455050 0.129 Uiso 1 1 calc R U . . .
C01F C -0.1258(19) 0.581(2) 1.233(2) 0.212(17) Uani 1 1 d . . . . .
H01I H -0.117457 0.538444 1.286374 0.255 Uiso 1 1 calc R U . . .
C01G C -0.188(2) 0.758(2) 1.1594(11) 0.145(9) Uani 1 1 d . . . . .
H01J H -0.102660 0.794086 1.159167 0.218 Uiso 1 1 calc R U . . .
H01K H -0.279334 0.813891 1.156108 0.218 Uiso 1 1 calc R U . . .
H01L H -0.183909 0.722556 1.113908 0.218 Uiso 1 1 calc R U . . .
C01H C -0.240(2) 0.0904(15) 0.3616(10) 0.110(6) Uani 1 1 d . . . . .
H01H H -0.329549 0.138253 0.339326 0.132 Uiso 1 1 calc R U . . .
C01I C -0.235(2) 0.720(2) 1.2987(12) 0.187(12) Uani 1 1 d . . . . .
H01M H -0.224196 0.656761 1.344800 0.280 Uiso 1 1 calc R U . . .
H01N H -0.339369 0.756912 1.291501 0.280 Uiso 1 1 calc R U . . .
H01O H -0.175448 0.773382 1.307138 0.280 Uiso 1 1 calc R U . . .
C01J C 0.5375(18) 0.0334(17) 1.2451(11) 0.140(9) Uani 1 1 d . . . . .
H01P H 0.581934 0.094353 1.214322 0.211 Uiso 1 1 calc R U . . .
H01Q H 0.590231 -0.038295 1.235391 0.211 Uiso 1 1 calc R U . . .
H01R H 0.544612 0.032625 1.301686 0.211 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
Cu01 N00B 1.918(7) . ?
Cu01 N00F 1.933(8) . ?
Cu01 O006 1.952(6) . ?
Cu01 O005 1.984(6) 1_554 ?
Cu02 N00H 1.942(8) 1_556 ?
Cu02 O00A 1.951(7) . ?
Cu02 N00D 1.977(8) 1_556 ?
Cu02 O005 1.998(6) . ?
Cu02 O00G 2.380(8) . ?
Cu03 N00M 1.938(8) . ?
Cu03 N00E 1.958(8) . ?
Cu03 N00N 1.980(9) . ?
Cu03 O005 1.999(6) 1_554 ?
Cu03 O008 2.388(7) . ?
S004 O00C 1.439(7) . ?
S004 O007 1.445(7) . ?
S004 C00U 1.769(9) . ?
S004 C00L 1.777(9) . ?
O005 H005 1.0000 . ?
O006 C00V 1.278(11) . ?
O008 H00A 0.8743 . ?
O008 H00B 0.8742 . ?
O009 C00V 1.214(11) . ?
O00A C012 1.281(13) . ?
N00B C00S 1.359(11) . ?
N00B N00D 1.366(9) . ?
N00D C00T 1.333(11) . ?
N00E C015 1.315(12) . ?
N00E N00F 1.367(11) . ?
N00F C016 1.337(12) . ?
O00G C01D 1.420(13) . ?
N00H C011 1.348(11) . ?
N00H N00M 1.374(11) . ?
O10 C01J 1.328(17) . ?
O10 H10 0.8400 . ?
O00J C01F 1.23(3) . ?
C00K C00L 1.372(12) . ?
C00K C00R 1.404(12) . ?
C00K H00K 0.9500 . ?
C00L C013 1.362(13) . ?
N00M C014 1.347(12) . ?
N00N C01H 1.303(18) . ?
N00N N01A 1.432(17) . ?
C00O C00R 1.364(12) . ?
C00O C00X 1.388(13) . ?
C00O C00V 1.519(13) . ?
O00P C012 1.215(13) . ?
C00Q C00T 1.381(13) . ?
C00Q C00S 1.397(13) . ?
C00Q H00Q 0.9500 . ?
C00R H00R 0.9500 . ?
C00S H00S 0.9500 . ?
C00T H00T 0.9500 . ?
C00U C00Y 1.381(13) . ?
C00U C00Z 1.407(14) . ?
N00W C01F 1.22(2) . ?
N00W C01G 1.36(2) . ?
N00W C01I 1.47(2) . ?
C00X C013 1.401(13) . ?
C00X H00X 0.9500 . ?
C00Y C019 1.383(13) . ?
C00Y H00Y 0.9500 . ?
C00Z C010 1.382(13) . ?
C00Z H00Z 0.9500 . ?
C010 C017 1.391(14) . ?
C010 H010 0.9500 . ?
C011 C01B 1.382(15) . ?
C011 H011 0.9500 . ?
C012 C017 1.520(13) . ?
C013 H013 0.9500 . ?
C014 C01B 1.354(15) . ?
C014 H014 0.9500 . ?
C015 C018 1.379(15) . ?
C015 H015 0.9500 . ?
C016 C018 1.387(14) . ?
C016 H016 0.9500 . ?
C017 C019 1.382(14) . ?
C018 H018 0.9500 . ?
C019 H019 0.9500 . ?
N01A C01C 1.321(16) . ?
N01A H01A 0.8800 . ?
C01B H01B 0.9500 . ?
C01C C01E 1.28(2) . ?
C01C H01C 0.9500 . ?
C01D H01D 0.9800 . ?
C01D H01E 0.9800 . ?
C01D H01F 0.9800 . ?
C01E C01H 1.43(2) . ?
C01E H01G 0.9500 . ?
C01F H01I 0.9500 . ?
C01G H01J 0.9800 . ?
C01G H01K 0.9800 . ?
C01G H01L 0.9800 . ?
C01H H01H 0.9500 . ?
C01I H01M 0.9800 . ?
C01I H01N 0.9800 . ?
C01I H01O 0.9800 . ?
C01J H01P 0.9800 . ?
C01J H01Q 0.9800 . ?
C01J H01R 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
N00B Cu01 N00F 178.7(3) . . ?
N00B Cu01 O006 91.7(3) . . ?
N00F Cu01 O006 89.6(3) . . ?
N00B Cu01 O005 90.4(3) . 1_554 ?
N00F Cu01 O005 88.3(3) . 1_554 ?
O006 Cu01 O005 172.8(3) . 1_554 ?
N00H Cu02 O00A 94.4(3) 1_556 . ?
N00H Cu02 N00D 160.1(3) 1_556 1_556 ?
O00A Cu02 N00D 90.6(3) . 1_556 ?
N00H Cu02 O005 88.1(3) 1_556 . ?
O00A Cu02 O005 173.0(3) . . ?
N00D Cu02 O005 89.2(3) 1_556 . ?
N00H Cu02 O00G 101.4(3) 1_556 . ?
O00A Cu02 O00G 85.2(3) . . ?
N00D Cu02 O00G 98.3(3) 1_556 . ?
O005 Cu02 O00G 88.0(3) . . ?
N00M Cu03 N00E 166.9(4) . . ?
N00M Cu03 N00N 93.3(4) . . ?
N00E Cu03 N00N 89.7(4) . . ?
N00M Cu03 O005 89.8(3) . 1_554 ?
N00E Cu03 O005 88.4(3) . 1_554 ?
N00N Cu03 O005 174.3(4) . 1_554 ?
N00M Cu03 O008 99.0(3) . . ?
N00E Cu03 O008 93.8(3) . . ?
N00N Cu03 O008 88.4(4) . . ?
O005 Cu03 O008 86.4(2) 1_554 . ?
O00C S004 O007 120.1(4) . . ?
O00C S004 C00U 109.1(4) . . ?
O007 S004 C00U 108.2(4) . . ?
O00C S004 C00L 106.8(4) . . ?
O007 S004 C00L 107.8(4) . . ?
C00U S004 C00L 103.6(4) . . ?
Cu01 O005 Cu02 116.5(3) 1_556 . ?
Cu01 O005 Cu03 107.2(3) 1_556 1_556 ?
Cu02 O005 Cu03 115.3(3) . 1_556 ?
Cu01 O005 H005 105.6 1_556 . ?
Cu02 O005 H005 105.6 . . ?
Cu03 O005 H005 105.6 1_556 . ?
C00V O006 Cu01 114.9(6) . . ?
Cu03 O008 H00A 109.5 . . ?
Cu03 O008 H00B 109.2 . . ?
H00A O008 H00B 104.3 . . ?
C012 O00A Cu02 125.3(7) . . ?
C00S N00B N00D 106.4(7) . . ?
C00S N00B Cu01 130.9(6) . . ?
N00D N00B Cu01 122.5(6) . . ?
C00T N00D N00B 108.9(7) . . ?
C00T N00D Cu02 131.1(6) . 1_554 ?
N00B N00D Cu02 119.7(6) . 1_554 ?
C015 N00E N00F 107.7(9) . . ?
C015 N00E Cu03 135.8(8) . . ?
N00F N00E Cu03 116.3(6) . . ?
C016 N00F N00E 107.5(8) . . ?
C016 N00F Cu01 132.4(7) . . ?
N00E N00F Cu01 120.1(6) . . ?
C01D O00G Cu02 122.4(7) . . ?
C011 N00H N00M 105.9(8) . . ?
C011 N00H Cu02 131.4(7) . 1_554 ?
N00M N00H Cu02 122.6(6) . 1_554 ?
C01J O10 H10 109.5 . . ?
C00L C00K C00R 118.2(9) . . ?
C00L C00K H00K 120.9 . . ?
C00R C00K H00K 120.9 . . ?
C013 C00L C00K 121.2(9) . . ?
C013 C00L S004 120.0(7) . . ?
C00K C00L S004 118.6(7) . . ?
C014 N00M N00H 107.4(8) . . ?
C014 N00M Cu03 133.1(7) . . ?
N00H N00M Cu03 119.5(6) . . ?
C01H N00N N01A 93.5(12) . . ?
C01H N00N Cu03 146.9(12) . . ?
N01A N00N Cu03 118.2(8) . . ?
C00R C00O C00X 119.0(8) . . ?
C00R C00O C00V 121.8(8) . . ?
C00X C00O C00V 119.1(9) . . ?
C00T C00Q C00S 103.4(9) . . ?
C00T C00Q H00Q 128.3 . . ?
C00S C00Q H00Q 128.3 . . ?
C00O C00R C00K 121.8(9) . . ?
C00O C00R H00R 119.1 . . ?
C00K C00R H00R 119.1 . . ?
N00B C00S C00Q 110.5(9) . . ?
N00B C00S H00S 124.7 . . ?
C00Q C00S H00S 124.7 . . ?
N00D C00T C00Q 110.8(8) . . ?
N00D C00T H00T 124.6 . . ?
C00Q C00T H00T 124.6 . . ?
C00Y C00U C00Z 121.8(9) . . ?
C00Y C00U S004 118.6(8) . . ?
C00Z C00U S004 119.6(8) . . ?
O009 C00V O006 126.1(9) . . ?
O009 C00V C00O 121.1(9) . . ?
O006 C00V C00O 112.8(9) . . ?
C01F N00W C01G 123(2) . . ?
C01F N00W C01I 121(2) . . ?
C01G N00W C01I 115.9(17) . . ?
C00O C00X C013 119.5(9) . . ?
C00O C00X H00X 120.3 . . ?
C013 C00X H00X 120.3 . . ?
C00U C00Y C019 119.0(9) . . ?
C00U C00Y H00Y 120.5 . . ?
C019 C00Y H00Y 120.5 . . ?
C010 C00Z C00U 118.2(10) . . ?
C010 C00Z H00Z 120.9 . . ?
C00U C00Z H00Z 120.9 . . ?
C00Z C010 C017 120.0(10) . . ?
C00Z C010 H010 120.0 . . ?
C017 C010 H010 120.0 . . ?
N00H C011 C01B 111.7(10) . . ?
N00H C011 H011 124.2 . . ?
C01B C011 H011 124.2 . . ?
O00P C012 O00A 125.2(10) . . ?
O00P C012 C017 120.3(11) . . ?
O00A C012 C017 114.5(10) . . ?
C00L C013 C00X 120.2(9) . . ?
C00L C013 H013 119.9 . . ?
C00X C013 H013 119.9 . . ?
N00M C014 C01B 111.7(10) . . ?
N00M C014 H014 124.2 . . ?
C01B C014 H014 124.2 . . ?
N00E C015 C018 111.5(10) . . ?
N00E C015 H015 124.3 . . ?
C018 C015 H015 124.3 . . ?
N00F C016 C018 110.2(10) . . ?
N00F C016 H016 124.9 . . ?
C018 C016 H016 124.9 . . ?
C019 C017 C010 121.0(9) . . ?
C019 C017 C012 120.3(10) . . ?
C010 C017 C012 118.7(10) . . ?
C015 C018 C016 103.2(9) . . ?
C015 C018 H018 128.4 . . ?
C016 C018 H018 128.4 . . ?
C017 C019 C00Y 119.9(10) . . ?
C017 C019 H019 120.0 . . ?
C00Y C019 H019 120.0 . . ?
C01C N01A N00N 116.0(14) . . ?
C01C N01A H01A 122.0 . . ?
N00N N01A H01A 122.0 . . ?
C014 C01B C011 103.3(9) . . ?
C014 C01B H01B 128.4 . . ?
C011 C01B H01B 128.4 . . ?
C01E C01C N01A 108.3(17) . . ?
C01E C01C H01C 125.8 . . ?
N01A C01C H01C 125.8 . . ?
O00G C01D H01D 109.5 . . ?
O00G C01D H01E 109.5 . . ?
H01D C01D H01E 109.5 . . ?
O00G C01D H01F 109.5 . . ?
H01D C01D H01F 109.5 . . ?
H01E C01D H01F 109.5 . . ?
C01C C01E C01H 101.2(15) . . ?
C01C C01E H01G 129.4 . . ?
C01H C01E H01G 129.4 . . ?
N00W C01F O00J 135(3) . . ?
N00W C01F H01I 112.7 . . ?
O00J C01F H01I 112.7 . . ?
N00W C01G H01J 109.5 . . ?
N00W C01G H01K 109.5 . . ?
H01J C01G H01K 109.5 . . ?
N00W C01G H01L 109.5 . . ?
H01J C01G H01L 109.5 . . ?
H01K C01G H01L 109.5 . . ?
N00N C01H C01E 119.5(18) . . ?
N00N C01H H01H 120.3 . . ?
C01E C01H H01H 120.3 . . ?
N00W C01I H01M 109.5 . . ?
N00W C01I H01N 109.5 . . ?
H01M C01I H01N 109.5 . . ?
N00W C01I H01O 109.5 . . ?
H01M C01I H01O 109.5 . . ?
H01N C01I H01O 109.5 . . ?
O10 C01J H01P 109.5 . . ?
O10 C01J H01Q 109.5 . . ?
H01P C01J H01Q 109.5 . . ?
O10 C01J H01R 109.5 . . ?
H01P C01J H01R 109.5 . . ?
H01Q C01J H01R 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
C00S N00B N00D C00T 1.2(10) . . . . ?
Cu01 N00B N00D C00T 176.4(6) . . . . ?
C00S N00B N00D Cu02 175.4(6) . . . 1_554 ?
Cu01 N00B N00D Cu02 -9.3(9) . . . 1_554 ?
C015 N00E N00F C016 -0.6(12) . . . . ?
Cu03 N00E N00F C016 -175.7(8) . . . . ?
C015 N00E N00F Cu01 178.1(7) . . . . ?
Cu03 N00E N00F Cu01 2.9(10) . . . . ?
C00R C00K C00L C013 -0.4(13) . . . . ?
C00R C00K C00L S004 174.9(6) . . . . ?
O00C S004 C00L C013 24.6(9) . . . . ?
O007 S004 C00L C013 154.9(7) . . . . ?
C00U S004 C00L C013 -90.6(8) . . . . ?
O00C S004 C00L C00K -150.8(7) . . . . ?
O007 S004 C00L C00K -20.5(8) . . . . ?
C00U S004 C00L C00K 94.0(8) . . . . ?
C011 N00H N00M C014 -0.7(12) . . . . ?
Cu02 N00H N00M C014 -176.4(8) 1_554 . . . ?
C011 N00H N00M Cu03 180.0(7) . . . . ?
Cu02 N00H N00M Cu03 4.2(11) 1_554 . . . ?
C00X C00O C00R C00K 3.8(13) . . . . ?
C00V C00O C00R C00K -174.7(8) . . . . ?
C00L C00K C00R C00O -1.9(13) . . . . ?
N00D N00B C00S C00Q -1.0(10) . . . . ?
Cu01 N00B C00S C00Q -175.7(7) . . . . ?
C00T C00Q C00S N00B 0.5(11) . . . . ?
N00B N00D C00T C00Q -0.9(11) . . . . ?
Cu02 N00D C00T C00Q -174.2(7) 1_554 . . . ?
C00S C00Q C00T N00D 0.2(11) . . . . ?
O00C S004 C00U C00Y 161.2(8) . . . . ?
O007 S004 C00U C00Y 28.9(9) . . . . ?
C00L S004 C00U C00Y -85.4(8) . . . . ?
O00C S004 C00U C00Z -20.5(9) . . . . ?
O007 S004 C00U C00Z -152.7(7) . . . . ?
C00L S004 C00U C00Z 93.0(8) . . . . ?
Cu01 O006 C00V O009 4.4(12) . . . . ?
Cu01 O006 C00V C00O -177.3(5) . . . . ?
C00R C00O C00V O009 -168.6(9) . . . . ?
C00X C00O C00V O009 12.8(13) . . . . ?
C00R C00O C00V O006 12.9(12) . . . . ?
C00X C00O C00V O006 -165.6(8) . . . . ?
C00R C00O C00X C013 -3.4(14) . . . . ?
C00V C00O C00X C013 175.2(9) . . . . ?
C00Z C00U C00Y C019 1.3(15) . . . . ?
S004 C00U C00Y C019 179.6(8) . . . . ?
C00Y C00U C00Z C010 0.7(14) . . . . ?
S004 C00U C00Z C010 -177.6(7) . . . . ?
C00U C00Z C010 C017 -1.8(15) . . . . ?
N00M N00H C011 C01B 2.3(13) . . . . ?
Cu02 N00H C011 C01B 177.5(8) 1_554 . . . ?
Cu02 O00A C012 O00P 15.4(16) . . . . ?
Cu02 O00A C012 C017 -165.0(6) . . . . ?
C00K C00L C013 C00X 0.8(14) . . . . ?
S004 C00L C013 C00X -174.5(8) . . . . ?
C00O C00X C013 C00L 1.1(15) . . . . ?
N00H N00M C014 C01B -1.2(14) . . . . ?
Cu03 N00M C014 C01B 178.0(9) . . . . ?
N00F N00E C015 C018 0.0(13) . . . . ?
Cu03 N00E C015 C018 173.7(8) . . . . ?
N00E N00F C016 C018 1.0(14) . . . . ?
Cu01 N00F C016 C018 -177.4(8) . . . . ?
C00Z C010 C017 C019 1.1(15) . . . . ?
C00Z C010 C017 C012 -177.9(9) . . . . ?
O00P C012 C017 C019 -172.5(11) . . . . ?
O00A C012 C017 C019 7.9(14) . . . . ?
O00P C012 C017 C010 6.5(15) . . . . ?
O00A C012 C017 C010 -173.2(9) . . . . ?
N00E C015 C018 C016 0.6(14) . . . . ?
N00F C016 C018 C015 -1.0(14) . . . . ?
C010 C017 C019 C00Y 1.0(16) . . . . ?
C012 C017 C019 C00Y 179.9(9) . . . . ?
C00U C00Y C019 C017 -2.1(16) . . . . ?
C01H N00N N01A C01C 2.2(16) . . . . ?
Cu03 N00N N01A C01C 172.3(10) . . . . ?
N00M C014 C01B C011 2.5(14) . . . . ?
N00H C011 C01B C014 -2.9(14) . . . . ?
N00N N01A C01C C01E -10(2) . . . . ?
N01A C01C C01E C01H 11.3(19) . . . . ?
C01G N00W C01F O00J -11(3) . . . . ?
C01I N00W C01F O00J -179.8(18) . . . . ?
N01A N00N C01H C01E 5.7(18) . . . . ?
Cu03 N00N C01H C01E -158.2(14) . . . . ?
C01C C01E C01H N00N -12(2) . . . . ?

_refine_diff_density_max         1.081
_refine_diff_density_min         -0.931
_refine_diff_density_rms         0.142



# start Validation Reply Form
_vrf_PLAT213_mo_rm200223_0m_b    
;
PROBLEM: Atom C01E            has ADP max/min Ratio .....        4.6 oblate
RESPONSE: The alert is resulted because of the presence of several lattice
 solvent molecules for which  seeral of the atoms are still not ideally shaped. 
;
_vrf_PLAT234_mo_rm200223_0m_b    
;
PROBLEM: Large Hirshfeld Difference C01E     --C01H     .       0.28 Ang.  
RESPONSE: The alert is resulted because of the presence of several lattice
 solvent molecules for which  seeral of the atoms are still not ideally shaped. 
;
_vrf_PLAT341_mo_rm200223_0m_b    
;
PROBLEM: Low Bond Precision on  C-C Bonds ...............    0.01523 Ang.  
RESPONSE: The alert is resulted because of the presence of several lattice
 solvent molecules for which  seeral of the atoms are still not ideally shaped.  
;
_vrf_PLAT430_mo_rm200223_0m_b    
;
PROBLEM: Short Inter D...A Contact  O00G     ..O00J     .       2.80 Ang.  
RESPONSE: The structure contains several short O...O distances which are
thought to result from possible hydrogen bonding interactions.
;
# 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_SO3H
_database_code_depnum_ccdc_archive 'CCDC 2344981'
loop_
_audit_author_name
_audit_author_address
'Raju Mondal'
;Indian Association for the Cultivation of Science
India
;
_audit_update_record             
;
2024-04-01 deposited with the CCDC.	2024-05-31 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2013
_chemical_name_systematic        
;
 ?
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C42 H45 Cu6 N20 O12 S'
_chemical_formula_weight         1435.28

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Cu Cu 0.3201 1.2651 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_H-M_alt        'P -1'
_space_group_name_Hall           '-P 1'

_shelx_space_group_comment       
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;

loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, -y, -z'

_cell_length_a                   11.5378(11)
_cell_length_b                   15.7422(13)
_cell_length_c                   16.9487(16)
_cell_angle_alpha                107.464(3)
_cell_angle_beta                 102.375(3)
_cell_angle_gamma                96.080(3)
_cell_volume                     2820.0(4)
_cell_formula_units_Z            2
_cell_measurement_temperature    120(2)
_cell_measurement_reflns_used    8282
_cell_measurement_theta_min      2.451
_cell_measurement_theta_max      25.569

_exptl_crystal_description       Cube
_exptl_crystal_colour            Blue
_exptl_crystal_density_meas      'not measured'
_exptl_crystal_density_method    'not measured'
_exptl_crystal_density_diffrn    1.690
_exptl_crystal_F_000             1446
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.28
_exptl_crystal_size_mid          0.26
_exptl_crystal_size_min          0.26
_exptl_absorpt_coefficient_mu    2.334
_shelx_estimated_absorpt_T_min   0.6321
_shelx_estimated_absorpt_T_max   0.7453
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.84811485
_exptl_absorpt_correction_T_max  1.00000000
_exptl_absorpt_process_details   
'SADABS v.2.03 (Bruker, 2001), R(int)=0.1082 before correction'

_exptl_special_details           
;
 ?
;

_diffrn_ambient_temperature      120(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_source                   'fine-focus sealed tube'
_diffrn_measurement_device_type  'Bruker APEX-2 CCD area detector'
_diffrn_measurement_method       '/w scans'
_diffrn_detector_area_resol_mean 8
_diffrn_reflns_number            30557
_diffrn_reflns_av_unetI/netI     0.0845
_diffrn_reflns_av_R_equivalents  0.0636
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_theta_min         2.451
_diffrn_reflns_theta_max         26.043
_diffrn_reflns_theta_full        25.242
_diffrn_measured_fraction_theta_max 0.992
_diffrn_measured_fraction_theta_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.992
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_point_group_measured_fraction_max 0.992
_diffrn_reflns_point_group_measured_fraction_full 0.997
_reflns_number_total             11058
_reflns_number_gt                6799
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_max     .
_reflns_Friedel_fraction_full    .

_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
;

_computing_data_collection       'Bruker APEX-3'
_computing_cell_refinement       'Bruker APEX-3'
_computing_data_reduction        'Bruker SHELXTL'
_computing_structure_solution    'SHELXT 2014/5 (Sheldrick, 2014)'
_computing_structure_refinement  'SHELXL-2016/6 (Sheldrick, 2016)'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'

_refine_special_details          
;
 ?
;
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.1000P)²] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_number_reflns         11058
_refine_ls_number_parameters     705
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.1384
_refine_ls_R_factor_gt           0.0838
_refine_ls_wR_factor_ref         0.2631
_refine_ls_wR_factor_gt          0.2332
_refine_ls_goodness_of_fit_ref   1.497
_refine_ls_restrained_S_all      1.497
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
Cu1 Cu 0.67661(9) 0.22658(6) 0.45674(6) 0.0282(3) Uani 1 1 d . . . . .
Cu2 Cu 0.81425(9) 0.07742(7) 0.33839(7) 0.0323(3) Uani 1 1 d . . . . .
Cu3 Cu 0.83185(9) 0.28390(7) 0.32720(7) 0.0311(3) Uani 1 1 d . . . . .
Cu4 Cu 0.25452(11) 0.67155(8) 1.04867(8) 0.0453(3) Uani 1 1 d . . . . .
Cu5 Cu 0.32113(11) 0.49560(8) 0.92760(7) 0.0454(3) Uani 1 1 d . . . . .
Cu6 Cu 0.32389(12) 0.50578(8) 1.13054(8) 0.0479(4) Uani 1 1 d . . . . .
S1 S 0.0146(2) 0.24447(14) 0.49080(14) 0.0325(5) Uani 1 1 d . . . . .
O1S O 0.7364(5) 0.1859(3) 0.3526(4) 0.0312(13) Uani 1 1 d . . . . .
O2S O 0.3515(6) 0.5716(4) 1.0502(4) 0.0429(16) Uani 1 1 d . . . . .
O1 O 0.5764(5) 0.2584(4) 0.5393(4) 0.0304(13) Uani 1 1 d . . . . .
O2 O 0.4321(5) 0.2013(4) 0.4177(4) 0.0361(14) Uani 1 1 d . . . . .
O3 O 0.2754(6) 0.4204(5) 0.8056(4) 0.0480(18) Uani 1 1 d . . . . .
O4 O 0.4698(6) 0.4264(5) 0.8066(4) 0.061(2) Uani 1 1 d . . . . .
O5 O -0.0031(5) 0.1497(4) 0.4411(4) 0.0345(14) Uani 1 1 d . . . . .
O6 O -0.0579(5) 0.2640(4) 0.5517(4) 0.0414(15) Uani 1 1 d . . . . .
O7 O 0.0016(5) 0.2998(4) 0.4379(4) 0.0442(16) Uani 1 1 d . . . . .
N1 N 0.6868(6) 0.1101(4) 0.4719(5) 0.0330(17) Uani 1 1 d . . . . .
N2 N 0.7412(6) 0.0485(4) 0.4238(5) 0.0315(16) Uani 1 1 d . . . . .
C1 C 0.6500(8) 0.0747(6) 0.5260(6) 0.036(2) Uani 1 1 d . . . . .
H1A H 0.6088 0.1037 0.5665 0.043 Uiso 1 1 calc R U . . .
C2 C 0.6797(8) -0.0100(6) 0.5154(6) 0.041(2) Uani 1 1 d . . . . .
H2A H 0.6644 -0.0495 0.5462 0.049 Uiso 1 1 calc R U . . .
C3 C 0.7359(8) -0.0241(6) 0.4506(7) 0.045(2) Uani 1 1 d . . . . .
H3A H 0.7667 -0.0771 0.4277 0.054 Uiso 1 1 calc R U . . .
N1A N 0.8613(7) 0.1022(5) 0.2428(5) 0.0409(19) Uani 1 1 d . . . . .
N2A N 0.8740(7) 0.1872(5) 0.2393(5) 0.0380(18) Uani 1 1 d . . . . .
C1A C 0.8909(12) 0.0489(8) 0.1741(7) 0.071(4) Uani 1 1 d . . . . .
H1AA H 0.8890 -0.0144 0.1599 0.086 Uiso 1 1 calc R U . . .
C2A C 0.9243(13) 0.1018(8) 0.1278(7) 0.076(4) Uani 1 1 d . . . . .
H2AA H 0.9484 0.0819 0.0760 0.092 Uiso 1 1 calc R U . . .
C3A C 0.9158(10) 0.1881(8) 0.1712(6) 0.052(3) Uani 1 1 d . . . . .
H3AA H 0.9359 0.2401 0.1560 0.062 Uiso 1 1 calc R U . . .
N1B N 0.7535(6) 0.3712(4) 0.3962(5) 0.0325(16) Uani 1 1 d . . . . .
N2B N 0.6911(6) 0.3479(4) 0.4498(5) 0.0304(16) Uani 1 1 d . . . . .
C1B C 0.7486(8) 0.4591(5) 0.4059(6) 0.037(2) Uani 1 1 d . . . . .
H1BA H 0.7852 0.4929 0.3768 0.045 Uiso 1 1 calc R U . . .
C2B C 0.6836(8) 0.4927(6) 0.4633(6) 0.040(2) Uani 1 1 d . . . . .
H2BA H 0.6667 0.5523 0.4811 0.048 Uiso 1 1 calc R U . . .
C3B C 0.6476(8) 0.4209(6) 0.4899(6) 0.035(2) Uani 1 1 d . . . . .
H3BA H 0.6004 0.4228 0.5298 0.042 Uiso 1 1 calc R U . . .
N1C N 0.9347(6) 0.3865(5) 0.3103(5) 0.0340(17) Uani 1 1 d . . . . .
N2C N 1.0186(7) 0.4423(5) 0.3796(5) 0.0391(18) Uani 1 1 d . . . . .
H2CA H 1.0469 0.4291 0.4262 0.047 Uiso 1 1 calc R U . . .
C1C C 0.9173(8) 0.4297(6) 0.2556(6) 0.040(2) Uani 1 1 d . . . . .
H1CA H 0.8623 0.4058 0.2004 0.048 Uiso 1 1 calc R U . . .
C2C C 0.9897(9) 0.5160(6) 0.2881(7) 0.047(2) Uani 1 1 d . . . . .
H2CB H 0.9940 0.5607 0.2612 0.056 Uiso 1 1 calc R U . . .
C3C C 1.0532(9) 0.5208(6) 0.3684(7) 0.047(3) Uani 1 1 d . . . . .
H3CA H 1.1112 0.5708 0.4087 0.056 Uiso 1 1 calc R U . . .
N1D N 0.8876(7) -0.0339(5) 0.3207(5) 0.0385(18) Uani 1 1 d . . . . .
N2D N 0.9920(7) -0.0345(5) 0.3719(5) 0.0414(19) Uani 1 1 d . . . . .
H2DA H 1.0379 0.0136 0.4127 0.050 Uiso 1 1 calc R U . . .
C1D C 0.8482(9) -0.1219(6) 0.2643(6) 0.046(3) Uani 1 1 d . . . . .
H1DA H 0.7760 -0.1433 0.2193 0.056 Uiso 1 1 calc R U . . .
C2D C 0.9306(10) -0.1719(6) 0.2846(7) 0.053(3) Uani 1 1 d . . . . .
H2DB H 0.9275 -0.2342 0.2556 0.064 Uiso 1 1 calc R U . . .
C3D C 1.0180(10) -0.1178(7) 0.3531(8) 0.055(3) Uani 1 1 d . . . . .
H3DA H 1.0857 -0.1356 0.3827 0.066 Uiso 1 1 calc R U . . .
N1E N 0.3468(8) 0.6073(6) 0.9023(5) 0.049(2) Uani 1 1 d . . . . .
N2E N 0.3136(8) 0.6824(6) 0.9534(5) 0.052(2) Uani 1 1 d . . . . .
C1E C 0.3818(10) 0.6275(9) 0.8406(7) 0.065(3) Uani 1 1 d . . . . .
H1EA H 0.4078 0.5869 0.7968 0.078 Uiso 1 1 calc R U . . .
C2E C 0.3751(11) 0.7187(10) 0.8492(8) 0.070(4) Uani 1 1 d . . . . .
H2EA H 0.3942 0.7511 0.8132 0.084 Uiso 1 1 calc R U . . .
C3E C 0.3347(11) 0.7498(8) 0.9214(7) 0.059(3) Uani 1 1 d . . . . .
H3EA H 0.3231 0.8101 0.9454 0.071 Uiso 1 1 calc R U . . .
N1F N 0.3320(8) 0.3899(6) 0.9631(5) 0.053(2) Uani 1 1 d . . . . .
N2F N 0.3336(8) 0.3941(6) 1.0461(5) 0.051(2) Uani 1 1 d . . . . .
C1F C 0.3374(11) 0.3039(7) 0.9186(8) 0.067(3) Uani 1 1 d . . . . .
H1FA H 0.3375 0.2821 0.8599 0.080 Uiso 1 1 calc R U . . .
C2F C 0.3427(11) 0.2536(8) 0.9722(8) 0.068(3) Uani 1 1 d . . . . .
H2FA H 0.3477 0.1912 0.9581 0.082 Uiso 1 1 calc R U . . .
C3F C 0.3395(9) 0.3114(7) 1.0509(7) 0.051(3) Uani 1 1 d . . . . .
H3FA H 0.3412 0.2950 1.1006 0.061 Uiso 1 1 calc R U . . .
N1G N 0.2636(7) 0.6082(5) 1.1933(5) 0.0391(18) Uani 1 1 d . . . . .
N2G N 0.2186(8) 0.6665(5) 1.1538(5) 0.048(2) Uani 1 1 d . . . . .
C1G C 0.1701(10) 0.7243(7) 1.2099(6) 0.053(3) Uani 1 1 d . . . . .
H1GA H 0.1297 0.7707 1.1987 0.063 Uiso 1 1 calc R U . . .
C2G C 0.1891(9) 0.7047(6) 1.2868(7) 0.051(3) Uani 1 1 d . . . . .
H2GA H 0.1667 0.7351 1.3373 0.062 Uiso 1 1 calc R U . . .
C3G C 0.2463(8) 0.6328(7) 1.2732(6) 0.043(2) Uani 1 1 d . . . . .
H3GA H 0.2710 0.6037 1.3140 0.052 Uiso 1 1 calc R U . . .
N1H N 0.1405(11) 0.7582(7) 1.0394(6) 0.063(3) Uani 1 1 d . . . . .
N2H N 0.0302(12) 0.7356(11) 1.0083(11) 0.119(6) Uani 1 1 d . . . . .
H2HA H -0.0096 0.6817 0.9741 0.143 Uiso 1 1 calc R U . . .
C1H C 0.180(2) 0.8576(13) 1.0816(14) 0.136(7) Uani 1 1 d . . . . .
H1HA H 0.2630 0.8860 1.1001 0.163 Uiso 1 1 calc R U . . .
C2H C 0.090(3) 0.9044(18) 1.0917(17) 0.164(10) Uani 1 1 d . . . . .
H2HB H 0.0901 0.9667 1.1191 0.196 Uiso 1 1 calc R U . . .
C3H C -0.021(2) 0.816(2) 1.0397(16) 0.159(10) Uani 1 1 d . . . . .
H3HA H -0.1043 0.8172 1.0317 0.191 Uiso 1 1 calc R U . . .
N1I N 0.3132(7) 0.4446(6) 1.2185(5) 0.048(2) Uani 1 1 d . . . . .
N2I N 0.2098(8) 0.3932(6) 1.2136(6) 0.059(2) Uani 1 1 d . . . . .
H2IA H 0.1407 0.3880 1.1768 0.070 Uiso 1 1 calc R U . . .
C1I C 0.3962(9) 0.4323(8) 1.2825(6) 0.050(3) Uani 1 1 d . . . . .
H1IA H 0.4789 0.4602 1.3021 0.060 Uiso 1 1 calc R U . . .
C2I C 0.3417(12) 0.3741(9) 1.3136(7) 0.066(3) Uani 1 1 d . . . . .
H2IB H 0.3802 0.3532 1.3578 0.079 Uiso 1 1 calc R U . . .
C3I C 0.2244(12) 0.3504(8) 1.2718(8) 0.065(3) Uani 1 1 d . . . . .
H3IA H 0.1641 0.3115 1.2814 0.078 Uiso 1 1 calc R U . . .
C4 C 0.4670(8) 0.2387(5) 0.4953(6) 0.031(2) Uani 1 1 d . . . . .
C5 C 0.3748(7) 0.2680(5) 0.5448(5) 0.0266(18) Uani 1 1 d . . . . .
C6 C 0.2540(7) 0.2449(5) 0.5024(5) 0.0273(18) Uani 1 1 d . . . . .
H6B H 0.2296 0.2108 0.4430 0.033 Uiso 1 1 calc R U . . .
C7 C 0.1694(7) 0.2708(5) 0.5454(5) 0.0269(18) Uani 1 1 d . . . . .
C8 C 0.2032(8) 0.3226(5) 0.6313(6) 0.034(2) Uani 1 1 d . . . . .
H8A H 0.1434 0.3417 0.6600 0.041 Uiso 1 1 calc R U . . .
C9 C 0.3247(7) 0.3468(5) 0.6758(5) 0.0285(18) Uani 1 1 d . . . . .
C10 C 0.4111(7) 0.3184(5) 0.6319(5) 0.0320(19) Uani 1 1 d . . . . .
H10A H 0.4943 0.3334 0.6615 0.038 Uiso 1 1 calc R U . . .
C11 C 0.3594(6) 0.4031(5) 0.7700(4) 0.0206(16) Uani 1 1 d . . . . .
O1SA O 0.1232(8) 0.5266(10) 0.9447(7) 0.125(5) Uani 1 1 d . . . . .
C1SA C 0.012(2) 0.5240(14) 0.9168(13) 0.130(7) Uiso 1 1 d . . . . .
C2SA C -0.0472(12) 0.5859(11) 0.9243(7) 0.118(8) Uani 1 1 d . . . . .
H2SA H -0.1327 0.5602 0.8964 0.177 Uiso 1 1 calc R U . . .
H2SB H -0.0184 0.6279 0.8971 0.177 Uiso 1 1 calc R U . . .
H2SC H -0.0374 0.6185 0.9851 0.177 Uiso 1 1 calc R U . . .
O1W O 0.5098(14) 0.1411(10) 0.2493(10) 0.172(6) Uiso 1 1 d . . . . .
O1SB O 0.424(2) 0.8028(17) 1.1482(17) 0.283(11) Uiso 1 1 d . . . . .
C1SB C 0.479(2) 0.8217(17) 1.2503(16) 0.178(10) Uiso 1 1 d . . . . .
H1SB H 0.4203 0.8101 1.2822 0.213 Uiso 1 1 calc R U . . .
H1SC H 0.5543 0.7983 1.2657 0.213 Uiso 1 1 calc R U . . .
C2SB C 0.495(2) 0.9072(15) 1.2430(14) 0.158(8) Uiso 1 1 d . . . . .
H2SD H 0.5378 0.9517 1.2988 0.237 Uiso 1 1 calc R U . . .
H2SE H 0.4155 0.9222 1.2237 0.237 Uiso 1 1 calc R U . . .
H2SF H 0.5414 0.9081 1.2013 0.237 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
Cu1 N1 1.938(7) . ?
Cu1 N2B 1.940(7) . ?
Cu1 O1S 1.984(5) . ?
Cu1 O1 1.985(5) . ?
Cu2 N1A 1.945(8) . ?
Cu2 N2 1.962(7) . ?
Cu2 O1S 1.988(5) . ?
Cu2 N1D 1.997(7) . ?
Cu2 O5 2.344(5) 1_655 ?
Cu3 N1B 1.956(7) . ?
Cu3 N2A 1.969(7) . ?
Cu3 O1S 2.005(5) . ?
Cu3 N1C 2.029(7) . ?
Cu3 O7 2.336(6) 1_655 ?
Cu4 N2E 1.927(9) . ?
Cu4 N2G 1.936(8) . ?
Cu4 N1H 2.008(9) . ?
Cu4 O2S 2.029(6) . ?
Cu5 N1E 1.939(9) . ?
Cu5 N1F 1.940(9) . ?
Cu5 O3 1.972(6) . ?
Cu5 O2S 1.995(6) . ?
Cu6 N1G 1.934(7) . ?
Cu6 N2F 1.937(8) . ?
Cu6 O2S 1.998(7) . ?
Cu6 N1I 2.020(9) . ?
Cu6 O4 2.373(8) 2_667 ?
S1 O7 1.423(6) . ?
S1 O5 1.444(6) . ?
S1 O6 1.446(6) . ?
S1 C7 1.768(8) . ?
O1 C4 1.273(10) . ?
O2 C4 1.224(10) . ?
O3 C11 1.260(9) . ?
O4 C11 1.252(9) . ?
O4 Cu6 2.373(7) 2_667 ?
O5 Cu2 2.344(5) 1_455 ?
O7 Cu3 2.336(6) 1_455 ?
N1 C1 1.325(11) . ?
N1 N2 1.368(9) . ?
N2 C3 1.351(11) . ?
C1 C2 1.381(12) . ?
C1 H1A 0.9500 . ?
C2 C3 1.366(13) . ?
C2 H2A 0.9500 . ?
C3 H3A 0.9500 . ?
N1A C1A 1.350(12) . ?
N1A N2A 1.352(10) . ?
N2A C3A 1.346(11) . ?
C1A C2A 1.383(16) . ?
C1A H1AA 0.9500 . ?
C2A C3A 1.363(15) . ?
C2A H2AA 0.9500 . ?
C3A H3AA 0.9500 . ?
N1B C1B 1.354(10) . ?
N1B N2B 1.378(9) . ?
N2B C3B 1.355(10) . ?
C1B C2B 1.370(12) . ?
C1B H1BA 0.9500 . ?
C2B C3B 1.394(12) . ?
C2B H2BA 0.9500 . ?
C3B H3BA 0.9500 . ?
N1C C1C 1.301(11) . ?
N1C N2C 1.343(10) . ?
N2C C3C 1.338(11) . ?
N2C H2CA 0.8800 . ?
C1C C2C 1.400(13) . ?
C1C H1CA 0.9500 . ?
C2C C3C 1.376(14) . ?
C2C H2CB 0.9500 . ?
C3C H3CA 0.9500 . ?
N1D N2D 1.328(10) . ?
N1D C1D 1.388(11) . ?
N2D C3D 1.336(12) . ?
N2D H2DA 0.8800 . ?
C1D C2D 1.349(14) . ?
C1D H1DA 0.9500 . ?
C2D C3D 1.347(15) . ?
C2D H2DB 0.9500 . ?
C3D H3DA 0.9500 . ?
N1E C1E 1.307(13) . ?
N1E N2E 1.384(11) . ?
N2E C3E 1.353(13) . ?
C1E C2E 1.410(17) . ?
C1E H1EA 0.9500 . ?
C2E C3E 1.375(15) . ?
C2E H2EA 0.9500 . ?
C3E H3EA 0.9500 . ?
N1F C1F 1.353(13) . ?
N1F N2F 1.384(11) . ?
N2F C3F 1.336(13) . ?
C1F C2F 1.369(17) . ?
C1F H1FA 0.9500 . ?
C2F C3F 1.382(14) . ?
C2F H2FA 0.9500 . ?
C3F H3FA 0.9500 . ?
N1G C3G 1.357(11) . ?
N1G N2G 1.371(11) . ?
N2G C1G 1.364(11) . ?
C1G C2G 1.406(14) . ?
C1G H1GA 0.9500 . ?
C2G C3G 1.355(13) . ?
C2G H2GA 0.9500 . ?
C3G H3GA 0.9500 . ?
N1H N2H 1.237(15) . ?
N1H C1H 1.49(2) . ?
N2H C3H 1.45(2) . ?
N2H H2HA 0.8800 . ?
C1H C2H 1.35(2) . ?
C1H H1HA 0.9500 . ?
C2H C3H 1.66(3) . ?
C2H H2HB 0.9500 . ?
C3H H3HA 0.9500 . ?
N1I N2I 1.341(12) . ?
N1I C1I 1.360(13) . ?
N2I C3I 1.344(14) . ?
N2I H2IA 0.8800 . ?
C1I C2I 1.351(16) . ?
C1I H1IA 0.9500 . ?
C2I C3I 1.340(16) . ?
C2I H2IB 0.9500 . ?
C3I H3IA 0.9500 . ?
C4 C5 1.517(11) . ?
C5 C6 1.377(11) . ?
C5 C10 1.396(12) . ?
C6 C7 1.364(10) . ?
C6 H6B 0.9500 . ?
C7 C8 1.384(12) . ?
C8 C9 1.393(12) . ?
C8 H8A 0.9500 . ?
C9 C10 1.399(11) . ?
C9 C11 1.516(10) . ?
C10 H10A 0.9500 . ?
O1SA C1SA 1.26(2) . ?
C1SA C2SA 1.24(2) . ?
C2SA H2SA 0.9800 . ?
C2SA H2SB 0.9800 . ?
C2SA H2SC 0.9800 . ?
O1SB C1SB 1.63(3) . ?
O1SB C2SB 1.88(3) . ?
C1SB C2SB 1.38(3) . ?
C1SB H1SB 0.9900 . ?
C1SB H1SC 0.9900 . ?
C2SB H2SD 0.9800 . ?
C2SB H2SE 0.9800 . ?
C2SB H2SF 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
N1 Cu1 N2B 171.7(3) . . ?
N1 Cu1 O1S 89.6(3) . . ?
N2B Cu1 O1S 89.4(3) . . ?
N1 Cu1 O1 92.5(3) . . ?
N2B Cu1 O1 90.6(2) . . ?
O1S Cu1 O1 165.5(2) . . ?
N1A Cu2 N2 171.1(3) . . ?
N1A Cu2 O1S 87.2(3) . . ?
N2 Cu2 O1S 89.2(2) . . ?
N1A Cu2 N1D 92.4(3) . . ?
N2 Cu2 N1D 90.9(3) . . ?
O1S Cu2 N1D 178.0(3) . . ?
N1A Cu2 O5 96.4(3) . 1_655 ?
N2 Cu2 O5 92.1(3) . 1_655 ?
O1S Cu2 O5 96.8(2) . 1_655 ?
N1D Cu2 O5 85.2(3) . 1_655 ?
N1B Cu3 N2A 166.9(3) . . ?
N1B Cu3 O1S 88.3(2) . . ?
N2A Cu3 O1S 87.4(3) . . ?
N1B Cu3 N1C 90.1(3) . . ?
N2A Cu3 N1C 95.0(3) . . ?
O1S Cu3 N1C 176.0(3) . . ?
N1B Cu3 O7 96.1(3) . 1_655 ?
N2A Cu3 O7 96.5(3) . 1_655 ?
O1S Cu3 O7 93.5(2) . 1_655 ?
N1C Cu3 O7 83.0(3) . 1_655 ?
N2E Cu4 N2G 171.9(4) . . ?
N2E Cu4 N1H 93.7(4) . . ?
N2G Cu4 N1H 90.6(3) . . ?
N2E Cu4 O2S 87.6(3) . . ?
N2G Cu4 O2S 89.1(3) . . ?
N1H Cu4 O2S 172.9(4) . . ?
N1E Cu5 N1F 167.9(4) . . ?
N1E Cu5 O3 92.9(3) . . ?
N1F Cu5 O3 91.7(3) . . ?
N1E Cu5 O2S 87.5(3) . . ?
N1F Cu5 O2S 88.9(3) . . ?
O3 Cu5 O2S 174.8(3) . . ?
N1G Cu6 N2F 162.3(3) . . ?
N1G Cu6 O2S 88.9(3) . . ?
N2F Cu6 O2S 89.0(3) . . ?
N1G Cu6 N1I 91.4(3) . . ?
N2F Cu6 N1I 92.4(4) . . ?
O2S Cu6 N1I 174.3(3) . . ?
N1G Cu6 O4 94.6(3) . 2_667 ?
N2F Cu6 O4 102.3(3) . 2_667 ?
O2S Cu6 O4 79.7(3) . 2_667 ?
N1I Cu6 O4 94.5(3) . 2_667 ?
O7 S1 O5 111.9(4) . . ?
O7 S1 O6 111.8(4) . . ?
O5 S1 O6 114.0(4) . . ?
O7 S1 C7 105.0(4) . . ?
O5 S1 C7 103.3(4) . . ?
O6 S1 C7 110.0(4) . . ?
Cu1 O1S Cu2 116.3(3) . . ?
Cu1 O1S Cu3 115.5(2) . . ?
Cu2 O1S Cu3 111.5(3) . . ?
Cu5 O2S Cu6 116.1(3) . . ?
Cu5 O2S Cu4 105.0(3) . . ?
Cu6 O2S Cu4 114.9(3) . . ?
C4 O1 Cu1 106.7(5) . . ?
C11 O3 Cu5 117.4(5) . . ?
C11 O4 Cu6 169.8(7) . 2_667 ?
S1 O5 Cu2 120.4(3) . 1_455 ?
S1 O7 Cu3 125.3(4) . 1_455 ?
C1 N1 N2 107.6(7) . . ?
C1 N1 Cu1 130.8(6) . . ?
N2 N1 Cu1 121.6(5) . . ?
C3 N2 N1 107.3(7) . . ?
C3 N2 Cu2 132.3(6) . . ?
N1 N2 Cu2 120.4(5) . . ?
N1 C1 C2 110.7(8) . . ?
N1 C1 H1A 124.7 . . ?
C2 C1 H1A 124.7 . . ?
C3 C2 C1 104.4(8) . . ?
C3 C2 H2A 127.8 . . ?
C1 C2 H2A 127.8 . . ?
N2 C3 C2 110.0(8) . . ?
N2 C3 H3A 125.0 . . ?
C2 C3 H3A 125.0 . . ?
C1A N1A N2A 107.4(8) . . ?
C1A N1A Cu2 132.2(7) . . ?
N2A N1A Cu2 120.4(5) . . ?
C3A N2A N1A 109.1(8) . . ?
C3A N2A Cu3 131.7(7) . . ?
N1A N2A Cu3 119.2(6) . . ?
N1A C1A C2A 108.8(10) . . ?
N1A C1A H1AA 125.6 . . ?
C2A C1A H1AA 125.6 . . ?
C3A C2A C1A 106.2(10) . . ?
C3A C2A H2AA 126.9 . . ?
C1A C2A H2AA 126.9 . . ?
N2A C3A C2A 108.5(10) . . ?
N2A C3A H3AA 125.8 . . ?
C2A C3A H3AA 125.8 . . ?
C1B N1B N2B 106.8(7) . . ?
C1B N1B Cu3 132.2(6) . . ?
N2B N1B Cu3 121.0(5) . . ?
C3B N2B N1B 108.4(7) . . ?
C3B N2B Cu1 131.0(6) . . ?
N1B N2B Cu1 120.6(5) . . ?
N1B C1B C2B 110.7(8) . . ?
N1B C1B H1BA 124.7 . . ?
C2B C1B H1BA 124.7 . . ?
C1B C2B C3B 105.3(7) . . ?
C1B C2B H2BA 127.3 . . ?
C3B C2B H2BA 127.3 . . ?
N2B C3B C2B 108.8(8) . . ?
N2B C3B H3BA 125.6 . . ?
C2B C3B H3BA 125.6 . . ?
C1C N1C N2C 106.3(7) . . ?
C1C N1C Cu3 133.2(6) . . ?
N2C N1C Cu3 116.6(6) . . ?
C3C N2C N1C 110.8(8) . . ?
C3C N2C H2CA 124.6 . . ?
N1C N2C H2CA 124.6 . . ?
N1C C1C C2C 111.5(9) . . ?
N1C C1C H1CA 124.2 . . ?
C2C C1C H1CA 124.2 . . ?
C3C C2C C1C 103.7(9) . . ?
C3C C2C H2CB 128.1 . . ?
C1C C2C H2CB 128.1 . . ?
N2C C3C C2C 107.6(9) . . ?
N2C C3C H3CA 126.2 . . ?
C2C C3C H3CA 126.2 . . ?
N2D N1D C1D 105.7(7) . . ?
N2D N1D Cu2 121.2(6) . . ?
C1D N1D Cu2 132.9(7) . . ?
N1D N2D C3D 110.9(8) . . ?
N1D N2D H2DA 124.6 . . ?
C3D N2D H2DA 124.6 . . ?
C2D C1D N1D 107.9(9) . . ?
C2D C1D H1DA 126.1 . . ?
N1D C1D H1DA 126.1 . . ?
C3D C2D C1D 108.1(9) . . ?
C3D C2D H2DB 126.0 . . ?
C1D C2D H2DB 126.0 . . ?
N2D C3D C2D 107.4(9) . . ?
N2D C3D H3DA 126.3 . . ?
C2D C3D H3DA 126.3 . . ?
C1E N1E N2E 109.2(9) . . ?
C1E N1E Cu5 133.2(8) . . ?
N2E N1E Cu5 117.3(6) . . ?
C3E N2E N1E 106.5(8) . . ?
C3E N2E Cu4 135.1(7) . . ?
N1E N2E Cu4 118.4(7) . . ?
N1E C1E C2E 109.7(10) . . ?
N1E C1E H1EA 125.2 . . ?
C2E C1E H1EA 125.2 . . ?
C3E C2E C1E 104.3(11) . . ?
C3E C2E H2EA 127.9 . . ?
C1E C2E H2EA 127.9 . . ?
N2E C3E C2E 110.3(11) . . ?
N2E C3E H3EA 124.9 . . ?
C2E C3E H3EA 124.9 . . ?
C1F N1F N2F 108.0(9) . . ?
C1F N1F Cu5 130.8(8) . . ?
N2F N1F Cu5 121.2(6) . . ?
C3F N2F N1F 107.5(8) . . ?
C3F N2F Cu6 131.4(7) . . ?
N1F N2F Cu6 121.0(7) . . ?
N1F C1F C2F 108.6(11) . . ?
N1F C1F H1FA 125.7 . . ?
C2F C1F H1FA 125.7 . . ?
C1F C2F C3F 106.5(10) . . ?
C1F C2F H2FA 126.7 . . ?
C3F C2F H2FA 126.7 . . ?
N2F C3F C2F 109.3(10) . . ?
N2F C3F H3FA 125.3 . . ?
C2F C3F H3FA 125.3 . . ?
C3G N1G N2G 108.1(8) . . ?
C3G N1G Cu6 131.4(7) . . ?
N2G N1G Cu6 120.3(6) . . ?
C1G N2G N1G 106.8(8) . . ?
C1G N2G Cu4 130.7(7) . . ?
N1G N2G Cu4 121.3(6) . . ?
N2G C1G C2G 109.4(9) . . ?
N2G C1G H1GA 125.3 . . ?
C2G C1G H1GA 125.3 . . ?
C3G C2G C1G 104.9(9) . . ?
C3G C2G H2GA 127.6 . . ?
C1G C2G H2GA 127.6 . . ?
C2G C3G N1G 110.7(10) . . ?
C2G C3G H3GA 124.7 . . ?
N1G C3G H3GA 124.7 . . ?
N2H N1H C1H 113.1(13) . . ?
N2H N1H Cu4 124.7(10) . . ?
C1H N1H Cu4 121.6(12) . . ?
N1H N2H C3H 106.2(17) . . ?
N1H N2H H2HA 126.9 . . ?
C3H N2H H2HA 126.9 . . ?
C2H C1H N1H 115(2) . . ?
C2H C1H H1HA 122.6 . . ?
N1H C1H H1HA 122.6 . . ?
C1H C2H C3H 95(2) . . ?
C1H C2H H2HB 132.3 . . ?
C3H C2H H2HB 132.3 . . ?
N2H C3H C2H 109.6(16) . . ?
N2H C3H H3HA 125.2 . . ?
C2H C3H H3HA 125.2 . . ?
N2I N1I C1I 104.8(9) . . ?
N2I N1I Cu6 120.9(7) . . ?
C1I N1I Cu6 133.8(7) . . ?
N1I N2I C3I 111.8(10) . . ?
N1I N2I H2IA 124.1 . . ?
C3I N2I H2IA 124.1 . . ?
C2I C1I N1I 108.8(10) . . ?
C2I C1I H1IA 125.6 . . ?
N1I C1I H1IA 125.6 . . ?
C3I C2I C1I 108.9(11) . . ?
C3I C2I H2IB 125.6 . . ?
C1I C2I H2IB 125.6 . . ?
C2I C3I N2I 105.7(11) . . ?
C2I C3I H3IA 127.2 . . ?
N2I C3I H3IA 127.2 . . ?
O2 C4 O1 125.6(8) . . ?
O2 C4 C5 118.6(8) . . ?
O1 C4 C5 115.7(7) . . ?
C6 C5 C10 120.0(7) . . ?
C6 C5 C4 119.1(8) . . ?
C10 C5 C4 120.9(7) . . ?
C7 C6 C5 120.3(8) . . ?
C7 C6 H6B 119.9 . . ?
C5 C6 H6B 119.9 . . ?
C6 C7 C8 120.8(7) . . ?
C6 C7 S1 120.5(6) . . ?
C8 C7 S1 118.5(6) . . ?
C7 C8 C9 120.1(7) . . ?
C7 C8 H8A 120.0 . . ?
C9 C8 H8A 120.0 . . ?
C8 C9 C10 118.9(7) . . ?
C8 C9 C11 119.1(7) . . ?
C10 C9 C11 122.0(7) . . ?
C5 C10 C9 119.9(8) . . ?
C5 C10 H10A 120.1 . . ?
C9 C10 H10A 120.1 . . ?
O4 C11 O3 125.4(7) . . ?
O4 C11 C9 117.0(6) . . ?
O3 C11 C9 117.6(6) . . ?
C2SA C1SA O1SA 130(2) . . ?
C1SA C2SA H2SA 109.5 . . ?
C1SA C2SA H2SB 109.5 . . ?
H2SA C2SA H2SB 109.5 . . ?
C1SA C2SA H2SC 109.5 . . ?
H2SA C2SA H2SC 109.5 . . ?
H2SB C2SA H2SC 109.5 . . ?
C1SB O1SB C2SB 45.8(12) . . ?
C2SB C1SB O1SB 76.3(18) . . ?
C2SB C1SB H1SB 115.8 . . ?
O1SB C1SB H1SB 115.8 . . ?
C2SB C1SB H1SC 115.8 . . ?
O1SB C1SB H1SC 115.8 . . ?
H1SB C1SB H1SC 112.8 . . ?
C1SB C2SB O1SB 57.8(14) . . ?
C1SB C2SB H2SD 109.5 . . ?
O1SB C2SB H2SD 166.9 . . ?
C1SB C2SB H2SE 109.5 . . ?
O1SB C2SB H2SE 79.9 . . ?
H2SD C2SB H2SE 109.5 . . ?
C1SB C2SB H2SF 109.5 . . ?
O1SB C2SB H2SF 74.6 . . ?
H2SD C2SB H2SF 109.5 . . ?
H2SE C2SB H2SF 109.5 . . ?

_refine_diff_density_max         1.634
_refine_diff_density_min         -1.403
_refine_diff_density_rms         0.192

_shelxl_version_number           2013-4



# start Validation Reply Form
_vrf_PLAT213_SO3H                
;
PROBLEM: Atom C2SA            has ADP max/min Ratio .....        9.5 prolat
RESPONSE:These alerts are generated because the atom was still not 
 ideally shaped.
;
_vrf_PLAT241_SO3H                
;
PROBLEM: High   'MainMol' Ueq as Compared to Neighbors of       O1SB Check 
RESPONSE: These alerts are generated because several of the atoms
 were still not ideally shaped.
;
_vrf_PLAT369_SO3H                
;
PROBLEM: Long   C(sp2)-C(sp2) Bond  C2H      - C3H      .       1.66 Ang.  
RESPONSE: These alerts are generated because several of the atoms
 were still not ideally shaped.
;
_vrf_PLAT414_SO3H                
;
PROBLEM: Short Intra D-H..H-X       H2HA     ..H2SB     .       1.30 Ang.  
RESPONSE: Ligand pyrazole group are in close approximate to the
 neighbouring methyl group
;
_vrf_PLAT601_SO3H                
;
PROBLEM: Unit Cell Contains Solvent Accessible VOIDS of .        296 Ang**3
RESPONSE: The alert arise from the large cage like structure conatining
 accessible solvent voids but cannot be found from the weak residual 
electron peaks.
;
_vrf_PLAT201_SO3H                
;
PROBLEM: Isotropic non-H Atoms in Main Residue(s) .......          4 Report
RESPONSE: The cage structure contains large solvent accesible void inside 
 framework as a resut atoms were still not ideally shaped. Hence refined 
 isotropically.
;
_vrf_PLAT220_SO3H                
;
PROBLEM: NonSolvent   Resd 1  C   Ueq(max)/Ueq(min) Range        8.9 Ratio 
RESPONSE: The cage structure contains large solvent accesible void inside 
 framework0 as a result atoms were still not ideally shaped, however, this does
 not indicate an overall structure of the ligand molecule incorrect
;
_vrf_PLAT242_SO3H                
;
PROBLEM: Low    'MainMol' Ueq as Compared to Neighbors of        Cu4 Check 
RESPONSE: The alert arised due to the presence of heavy metal atom.
;
_vrf_PLAT306_SO3H                
;
PROBLEM: Isolated Oxygen Atom (H-atoms Missing ?) .......        O1W Check 
RESPONSE: The hydrogen atoms of the water molecule could not be
 directly locate from the difference Fourier maps because of the presence of
 many heavy atoms in structures. When we provide the formula in CIF files,
 these hydrogen atoms are d added according to the principle of charge
 balance and the case that one water have two hydrogen atom
;
_vrf_PLAT341_SO3H                
;
PROBLEM: Low Bond Precision on  C-C Bonds ...............     0.0179 Ang.  
RESPONSE: The cage structure contains large solvent accesible void inside 
 framework0 as a result atoms were still not ideally shaped, however, this does
 not indicate an overall structure of the ligand molecule incorrect
;
_vrf_PLAT430_SO3H                
;
PROBLEM: Short Inter D...A Contact  O1S      ..O1W      .       2.70 Ang.  
RESPONSE: The lattrice water molecule and metal coordinated oxygen atom
 are in close approximate to each other
;
_vrf_PLAT919_SO3H                
;
PROBLEM: Reflection # Likely Affected by the Beamstop ...          1 Check 
RESPONSE: This alert may arise during data collection,  SADABS has been 
 used for correction.
;
_vrf_PLAT973_SO3H                
;
PROBLEM: Check Calcd Resid. Dens.  0.71Ang From O1W     .       1.55 eA-3  
RESPONSE: There is no chemically sensible species corresponding to this residual 
density peak. The positive density may arise due to the presence of heavy metal atoms.
;
# end Validation Reply Form
