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_7249258
_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
'C40 H28 Cu3.8 I2 N8 S3.8 W0.95, 0.05(Cu4 S4 W), 3(C3 H7 N O)'
_chemical_formula_sum            'C49 H49 Cu4 I2 N11 O3 S4 W'
_chemical_formula_weight         1660.04
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2yn'
_space_group_name_H-M_alt        'P 1 21/n 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_audit_creation_date             2024-03-01
_audit_creation_method
;
Olex2 1.5
(compiled 2023.08.24 svn.re1ec1418 for OlexSys, GUI svn.r6817)
;
_audit_update_record
;
2024-05-14 deposited with the CCDC.	2024-08-28 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 93.475(2)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   13.5150(4)
_cell_length_b                   17.6465(7)
_cell_length_c                   28.1103(9)
_cell_measurement_reflns_used    9976
_cell_measurement_temperature    193.00
_cell_measurement_theta_max      68.316
_cell_measurement_theta_min      2.957
_cell_volume                     6691.8(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  'SHELXL 2018/3 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT 2018/2 (Sheldrick, 2018)'
_diffrn_ambient_temperature      193.00
_diffrn_measured_fraction_theta_full 0.994
_diffrn_measured_fraction_theta_max 0.991
_diffrn_measurement_device_type  'Bruker D8 VENTURE'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54178
_diffrn_reflns_av_R_equivalents  0.0665
_diffrn_reflns_av_unetI/netI     0.0526
_diffrn_reflns_Laue_measured_fraction_full 0.994
_diffrn_reflns_Laue_measured_fraction_max 0.991
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       21
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_l_max       33
_diffrn_reflns_limit_l_min       -32
_diffrn_reflns_number            55773
_diffrn_reflns_point_group_measured_fraction_full 0.994
_diffrn_reflns_point_group_measured_fraction_max 0.991
_diffrn_reflns_theta_full        67.679
_diffrn_reflns_theta_max         68.434
_diffrn_reflns_theta_min         2.958
_diffrn_source_current           1.1
_diffrn_source_power             0.05500000000000001
_diffrn_source_voltage           50.0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    13.253
_exptl_absorpt_correction_T_max  0.1665
_exptl_absorpt_correction_T_min  0.0562
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2016/2 (Bruker,2016/2) was used for absorption correction.
wR2(int) was 0.1304 before and 0.0642 after correction.
The Ratio of minimum to maximum transmission is 0.3375.
The \l/2 correction factor is Not present.
;
_exptl_crystal_density_diffrn    1.648
_exptl_crystal_description       block
_exptl_crystal_F_000             3216
_exptl_crystal_size_max          0.13
_exptl_crystal_size_mid          0.11
_exptl_crystal_size_min          0.1
_refine_diff_density_max         1.713
_refine_diff_density_min         -1.027
_refine_diff_density_rms         0.130
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.049
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     754
_refine_ls_number_reflns         12202
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.049
_refine_ls_R_factor_all          0.0622
_refine_ls_R_factor_gt           0.0497
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0715P)^2^+13.8737P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1370
_refine_ls_wR_factor_ref         0.1454
_reflns_Friedel_coverage         0.000
_reflns_number_gt                9523
_reflns_number_total             12202
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d4ce00493k2.cif
_cod_data_source_block           2
_cod_depositor_comments
'Adding full bibliography for 7249257--7249263.cif.'
_cod_database_code               7249258
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   0.351
_shelx_estimated_absorpt_t_min   0.278
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Uiso/Uaniso restraints and constraints
W2 \\sim Cu6 \\sim Cu8 \\sim S5 \\sim S6 \\sim S7 \\sim S8: within 2A with
sigma of 0.001 and sigma for terminal atoms of 0.002 within 2A
Cu5 \\sim Cu7 \\sim Cu8 \\sim S5 \\sim S6 \\sim S7 \\sim S8: within 2A with
sigma of 0.001 and sigma for terminal atoms of 0.002 within 2A
3. Others
 Fixed Sof: W1(0.95) Cu1(0.95) Cu2(0.95) Cu3(0.95) Cu4(0.95) S1(0.95) S2(0.95)
 S3(0.95) S4(0.95) W2(0.05) Cu5(0.05) Cu6(0.05) Cu7(0.05) Cu8(0.05) S5(0.05)
 S6(0.05) S7(0.05) S8(0.05)
4.a Aromatic/amide H refined with riding coordinates:
 C1(H1), C2(H2), C3(H3), C4(H4), C5(H5), C6(H6), C7(H7), C14(H14), C15(H15),
 C16(H16), C17(H17), C18(H18), C19(H19), C20(H20), C30(H30), C31(H31), C32(H32),
  C33(H33), C34(H34), C35(H35), C38(H38), C43(H43), C44(H44), C45(H45),
 C46(H46), C47(H47), C48(H48), C49(H49), C29(H29), C25(H25), C23(H23)
4.b Idealised Me refined as rotating group:
 C27(H27A,H27B,H27C), C28(H28B,H28A,H28C), C24(H24A,H24B,H24C), C26(H26A,H26B,
 H26C), C21(H21A,H21B,H21C), C22(H22A,H22B,H22C)
;
_smtbx_masks_void_probe_radius   1.2
_smtbx_masks_void_truncation_radius 1.2
_shelx_res_checksum              92031
_shelx_hkl_checksum              66650
_shelx_fab_checksum              75792
_olex2_submission_special_instructions 'No special instructions were received'