Coordination polymers and supramolecular cages based on [(MS4)Cux]x−2 cluster units and N-containing ligands
Xu, Meng-Yuan; Wu, Qian; Wang, Chen; Sun, Yao; Teng, Yu-Kang; Zhang, Rui; Lu, Zhen-Zhong; CrystEngComm 26 (2024) 5585–5590; doi:10.1039/D4CE00493K

data_7249260
_publ_section_title
;
 Coordination polymers and supramolecular cages based on
 [(MS4)Cux]x&#x2212;2 cluster units and N-containing ligands
;
_journal_issue                   39
_journal_name_full               CrystEngComm
_journal_page_first              5585
_journal_page_last               5590
_journal_paper_doi               10.1039/D4CE00493K
_journal_volume                  26
_journal_year                    2024
_chemical_formula_moiety         'C54 H90 Cu10 I12 Mo2 N12 S8, 6[C3H7NO]'
_chemical_formula_sum            'C72 H132 Cu10 I12 Mo2 N18 O6 S8'
_chemical_formula_weight         3952.51
_space_group_crystal_system      triclinic
_space_group_IT_number           1
_space_group_name_Hall           'P 1'
_space_group_name_H-M_alt        'P 1'
_atom_sites_solution_hydrogens   geom
_audit_creation_date             2024-08-23
_audit_creation_method
;
Olex2 1.5
(compiled 2023.08.24 svn.re1ec1418 for OlexSys, GUI svn.r6817)
;
_audit_update_record
;
2024-08-23 deposited with the CCDC.	2024-08-28 downloaded from the CCDC.
;
_cell_angle_alpha                82.885(4)
_cell_angle_beta                 77.181(4)
_cell_angle_gamma                89.955(3)
_cell_formula_units_Z            1
_cell_length_a                   11.8390(7)
_cell_length_b                   13.8931(8)
_cell_length_c                   21.9722(14)
_cell_measurement_reflns_used    9984
_cell_measurement_temperature    223.00
_cell_measurement_theta_max      72.31
_cell_measurement_theta_min      3.21
_cell_volume                     3495.5(4)
_computing_cell_refinement       'SAINT V8.40B (?, 2016)'
_computing_data_reduction        'SAINT V8.40B (?, 2016)'
_computing_molecular_graphics    'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_structure_refinement  'XL  (Sheldrick, 2008)'
_computing_structure_solution    'olex2.solve 1.5 (Bourhis et al., 2015)'
_diffrn_ambient_temperature      223.00
_diffrn_measured_fraction_theta_full 0.987
_diffrn_measured_fraction_theta_max 0.975
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54178
_diffrn_reflns_av_unetI/netI     0.0726
_diffrn_reflns_Laue_measured_fraction_full 0.987
_diffrn_reflns_Laue_measured_fraction_max 0.975
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       27
_diffrn_reflns_limit_l_min       -27
_diffrn_reflns_number            23472
_diffrn_reflns_point_group_measured_fraction_full 0.860
_diffrn_reflns_point_group_measured_fraction_max 0.833
_diffrn_reflns_theta_full        67.679
_diffrn_reflns_theta_max         73.418
_diffrn_reflns_theta_min         2.079
_diffrn_source_current           1.1
_diffrn_source_power             0.05500000000000001
_diffrn_source_voltage           50.0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    25.277
_exptl_absorpt_correction_T_max  0.1143
_exptl_absorpt_correction_T_min  0.0115
_exptl_absorpt_correction_type   none
_exptl_absorpt_process_details
;
SADABS-2016/2 (Bruker,2016/2) was used for absorption correction.
wR2(int) was 0.1580 before and 0.1012 after correction.
The Ratio of minimum to maximum transmission is 0.1006.
The \l/2 correction factor is Not present.
;
_exptl_crystal_density_diffrn    1.878
_exptl_crystal_description       block
_exptl_crystal_F_000             1876
_exptl_crystal_size_max          0.15
_exptl_crystal_size_mid          0.13
_exptl_crystal_size_min          0.12
_refine_diff_density_max         2.085
_refine_diff_density_min         -1.540
_refine_diff_density_rms         0.230
_refine_ls_abs_structure_details
;
 Flack x determined using 4747 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   0.287(6)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.993
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     872
_refine_ls_number_reflns         23472
_refine_ls_number_restraints     1218
_refine_ls_restrained_S_all      0.974
_refine_ls_R_factor_all          0.1066
_refine_ls_R_factor_gt           0.0902
_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/[\s^2^(Fo^2^)+(0.1844P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2435
_refine_ls_wR_factor_ref         0.2661
_reflns_Friedel_coverage         0.708
_reflns_Friedel_fraction_full    0.734
_reflns_Friedel_fraction_max     0.691
_reflns_number_gt                16404
_reflns_number_total             23472
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d4ce00493k2.cif
_cod_data_source_block           cu_20240308_zm_ngd_lzz_28_0m
_cod_depositor_comments
'Adding full bibliography for 7249257--7249263.cif.'
_cod_database_code               7249260
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   0.151
_shelx_estimated_absorpt_t_min   0.116
_olex2_refinement_description
;
1. Twinned data refinement
 Scales: 0.872(6)
 0.128(6)
2. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
3. Restrained distances
 C56-C55
 1.5 with sigma of 0.02
 C40-C39
 1.41 with sigma of 0.02
 C47-C46
 1.5 with sigma of 0.02
 C31-C30
 1.5 with sigma of 0.02
 C29-C28
 1.5 with sigma of 0.02
 C18-C17
 1.5 with sigma of 0.02
 C60-C59
 1.5 with sigma of 0.02
 C4-C3
 1.5 with sigma of 0.02
 C25-C24
 1.5 with sigma of 0.02
 H23B-H25A
 2.1 with sigma of 0.02
 C25-C23
 2.2 with sigma of 0.02
 C20-C16
 2.2 with sigma of 0.02
 C15-C16
 1.5 with sigma of 0.02
 H16B-H20A
 2.1 with sigma of 0.02
 N11-C55 \\sim N11-C57 \\sim N11-C59 \\sim N12-C56 \\sim N12-C58 \\sim N12-C60
 with sigma of 0.02
 N7-C30 \\sim N7-C28 \\sim N7-C32 \\sim N8-C29 \\sim N8-C33 \\sim N8-C31
 with sigma of 0.02
 N6-C25 \\sim N6-C23 \\sim N6-C27
 with sigma of 0.02
 N4-C18 \\sim N4-C20 \\sim N4-C16
 with sigma of 0.02
 C20-C19 \\sim C16-C15 \\sim C18-C17
 with sigma of 0.02
4. Restrained planarity
 C12, C11, C10, C9, C8, C13, C7
 with sigma of 0.1
 C38, C39, C40, C35, C36, C37, C34, C54, C41
 with sigma of 0.1
5. Uiso/Uaniso restraints and constraints
C35 \\sim C23 \\sim C30 \\sim C21 \\sim C22 \\sim C34 \\sim C44 \\sim C38 \\sim
C36 \\sim C33 \\sim C29 \\sim C43 \\sim C46 \\sim C5 \\sim C26 \\sim C6 \\sim
C45 \\sim C3 \\sim C7 \\sim C37 \\sim C14 \\sim C32 \\sim C2 \\sim C42 \\sim
C27 \\sim C54 \\sim C41 \\sim C18 \\sim C24 \\sim C25 \\sim C9 \\sim C8 \\sim
C13 \\sim C12 \\sim C11 \\sim C10 \\sim C17 \\sim C57 \\sim C47 \\sim C15 \\sim
C59 \\sim C4 \\sim C1 \\sim C19 \\sim C58 \\sim C31 \\sim C28 \\sim C55 \\sim
C60 \\sim C56 \\sim C16 \\sim C20 \\sim C40 \\sim C39: within 3.8A with sigma
of 0.03 and sigma for terminal atoms of 0.06 within 3.8A
Uanis(N4) \\sim Ueq: with sigma of 0.02 and sigma for terminal atoms of 0.04
Uanis(N8) \\sim Ueq: with sigma of 0.02 and sigma for terminal atoms of 0.04
6.a Secondary CH2 refined with riding coordinates:
 C23(H23A,H23B), C30(H30A,H30B), C21(H21A,H21B), C22(H22A,H22B), C34(H34A,
 H34B), C44(H44A,H44B), C33(H33A,H33B), C29(H29A,H29B), C43(H43A,H43B),
 C46(H46A,H46B), C5(H5A,H5B), C26(H26A,H26B), C6(H6A,H6B), C45(H45A,H45B),
 C3(H3A,H3B), C7(H7A,H7B), C14(H14A,H14B), C32(H32A,H32B), C2(H2A,H2B),
 C42(H42A,H42B), C27(H27A,H27B), C54(H54A,H54B), C41(H41A,H41B), C18(H18A,H18B),
  C24(H24A,H24B), C25(H25A,H25B), C17(H17A,H17B), C57(H57A,H57B), C47(H47A,
 H47B), C15(H15A,H15B), C59(H59A,H59B), C4(H4A,H4B), C1(H1A,H1B), C19(H19A,
 H19B), C58(H58A,H58B), C31(H31A,H31B), C28(H28A,H28B), C55(H55A,H55B),
 C60(H60A,H60B), C56(H56A,H56B), C16(H16A,H16B), C20(H20A,H20B)
6.b Aromatic/amide H refined with riding coordinates:
 C38(H38), C36(H36), C9(H9), C13(H13), C11(H11), C40(H40)
6.c Fitted hexagon refined as free rotating group:
 C9(C8,C13,C12,C11,C10)
;
_smtbx_masks_void_probe_radius   1.2
_smtbx_masks_void_truncation_radius 1.2
_shelx_res_checksum              68256
_shelx_hkl_checksum              67881
_shelx_fab_checksum              68990
_olex2_submission_special_instructions 'No special instructions were received'