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_7249257
_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         'C66 H42.818 Cu4 I2 N12 S4 W, 2[C3H7NO]'
_chemical_formula_sum            'C72 H56.82 Cu4 I2 N14 O2 S4 W'
_chemical_formula_weight         1970.18
_chemical_name_systematic        123
_space_group_crystal_system      monoclinic
_space_group_IT_number           15
_space_group_name_Hall           '-C 2yc'
_space_group_name_H-M_alt        'C 1 2/c 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                90
_cell_angle_beta                 114.7000(10)
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   45.2038(8)
_cell_length_b                   19.0461(3)
_cell_length_c                   28.9481(5)
_cell_measurement_reflns_used    9883
_cell_measurement_temperature    193.00
_cell_measurement_theta_max      68.22
_cell_measurement_theta_min      3.14
_cell_volume                     22642.8(7)
_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    'SHELXT 2018/2 (Sheldrick, 2018)'
_diffrn_ambient_temperature      193.00
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.994
_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_R_equivalents  0.0706
_diffrn_reflns_av_unetI/netI     0.0594
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.994
_diffrn_reflns_limit_h_max       54
_diffrn_reflns_limit_h_min       -52
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -22
_diffrn_reflns_limit_l_max       33
_diffrn_reflns_limit_l_min       -34
_diffrn_reflns_number            79065
_diffrn_reflns_point_group_measured_fraction_full 0.997
_diffrn_reflns_point_group_measured_fraction_max 0.994
_diffrn_reflns_theta_full        67.679
_diffrn_reflns_theta_max         68.294
_diffrn_reflns_theta_min         2.557
_diffrn_source_current           1.1
_diffrn_source_power             0.05500000000000001
_diffrn_source_voltage           50.0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    7.914
_exptl_absorpt_correction_T_max  0.7531
_exptl_absorpt_correction_T_min  0.5352
_exptl_absorpt_correction_type   none
_exptl_absorpt_process_details
;
SADABS-2016/2 (Bruker,2016/2) was used for absorption correction.
wR2(int) was 0.1174 before and 0.0605 after correction.
The Ratio of minimum to maximum transmission is 0.7107.
The \l/2 correction factor is Not present.
;
_exptl_crystal_colour            'clear light colourless'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   light
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.156
_exptl_crystal_description       block
_exptl_crystal_F_000             7703
_exptl_crystal_size_max          0.13
_exptl_crystal_size_mid          0.12
_exptl_crystal_size_min          0.11
_refine_diff_density_max         1.980
_refine_diff_density_min         -1.860
_refine_diff_density_rms         0.112
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.061
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     830
_refine_ls_number_reflns         20651
_refine_ls_number_restraints     174
_refine_ls_restrained_S_all      1.059
_refine_ls_R_factor_all          0.0672
_refine_ls_R_factor_gt           0.0479
_refine_ls_shift/su_max          0.003
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0827P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1390
_refine_ls_wR_factor_ref         0.1506
_reflns_Friedel_coverage         0.000
_reflns_number_gt                14255
_reflns_number_total             20651
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d4ce00493k2.cif
_cod_data_source_block           cu_20230719_zm_ngd_lzz_8_0m
_cod_depositor_comments
'Adding full bibliography for 7249257--7249263.cif.'
_cod_database_code               7249257
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   0.476
_shelx_estimated_absorpt_t_min   0.426
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
2. Restrained distances
 Cu2-N12 \\sim Cu2-N12A
 with sigma of 0.02
 N12-C63 \\sim N12A-C63A
 with sigma of 0.02
 N12-C62 \\sim N12A-C62A
 with sigma of 0.02
 C63-N11 \\sim C63A-N11A
 with sigma of 0.02
 N11-C57 \\sim N11A-C57
 with sigma of 0.02
 N11-C61 \\sim N11A-C61A
 with sigma of 0.02
 C61-C62 \\sim C61A-C62A
 with sigma of 0.02
 Cu2-C63 \\sim Cu2-C63A
 with sigma of 0.04
 Cu2-C62 \\sim Cu2-C62A
 with sigma of 0.04
 N12-N11 \\sim N12A-N11A
 with sigma of 0.04
 N12-C61 \\sim N12A-C61A
 with sigma of 0.04
 C63-C57 \\sim C63A-C57
 with sigma of 0.04
 C63-C61 \\sim C63A-C61A
 with sigma of 0.04
 C63-C62 \\sim C63A-C62A
 with sigma of 0.04
 N11-C62 \\sim N11A-C62A
 with sigma of 0.04
 C57-C61 \\sim C57-C61A
 with sigma of 0.04
3. Rigid bond restraints
 N10, C46
 with sigma for 1-2 distances of 0.001 and sigma for 1-3 distances of 0.002
 N9, C46
 with sigma for 1-2 distances of 0.001 and sigma for 1-3 distances of 0.002
4. Uiso/Uaniso restraints and constraints
N11 \\sim N12 \\sim C61 \\sim C62 \\sim C63 \\sim N11A \\sim N12A \\sim C61A
\\sim C62A \\sim C63A: within 2A with sigma of 0.001 and sigma for terminal
atoms of 0.002 within 2A
Uanis(C46) \\sim Ueq: with sigma of 0.001 and sigma for terminal atoms of 0.002
5. Others
 Sof(N11A)=Sof(N12A)=Sof(C61A)=Sof(H61A)=Sof(H61B)=Sof(C62A)=Sof(H62A)=
 Sof(H62B)=Sof(C63A)=Sof(H63A)=1-FVAR(1)
 Sof(N11)=Sof(N12)=Sof(C61)=Sof(H61)=Sof(C62)=Sof(H62)=Sof(C63)=Sof(H63)=FVAR(1)
6.a Everything fixed:
 C63, N12A
6.b Secondary CH2 refined with riding coordinates:
 C61A(H61A,H61B), C62A(H62A,H62B)
6.c Aromatic/amide H refined with riding coordinates:
 C2(H2), C3(H3), C5(H5), C6(H6), C10(H10), C11(H11), C15(H15), C16(H16),
 C18(H18), C19(H19), C20(H20), C21(H21), C22(H22), C23(H23), C24(H24), C25(H25),
  C27(H27), C28(H28), C33(H33), C34(H34), C35(H35), C36(H36), C39(H39),
 C40(H40), C41(H41), C42(H42), C43(H43), C44(H44), C45(H45), C46(H46), C49(H49),
  C50(H50), C54(H54), C55(H55), C56(H56), C59(H59), C60(H60), C64(H64),
 C65(H65), C61(H61), C62(H62), C63(H63), C63A(H63A)
;
_smtbx_masks_void_probe_radius   1.2
_smtbx_masks_void_truncation_radius 1.2
_shelx_res_checksum              21537
_shelx_hkl_checksum              53182
_shelx_fab_checksum              96108
_olex2_submission_special_instructions 'No special instructions were received'