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_7249261
_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
'C27 H45 Br Cl4 Cu4 N6 S4 W, C27 H44 Br Cl4 Cu4 N6 S4 W, 6(C2 H6 O S)'
_chemical_formula_sum            'C66 H125 Br2 Cl8 Cu8 N12 O6 S14 W2'
_chemical_formula_weight         2951.05
_space_group_crystal_system      monoclinic
_space_group_IT_number           4
_space_group_name_Hall           'P 2yb'
_space_group_name_H-M_alt        'P 1 21 1'
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     dual
_audit_creation_date             2024-02-26
_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                 90.112(3)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   11.3261(7)
_cell_length_b                   13.5698(8)
_cell_length_c                   33.110(2)
_cell_measurement_reflns_used    9987
_cell_measurement_temperature    193.00
_cell_measurement_theta_max      68.17
_cell_measurement_theta_min      3.52
_cell_volume                     5088.8(5)
_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 0.987
_diffrn_measured_fraction_theta_max 0.985
_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  0.0450
_diffrn_reflns_av_unetI/netI     0.0480
_diffrn_reflns_Laue_measured_fraction_full 0.987
_diffrn_reflns_Laue_measured_fraction_max 0.985
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       39
_diffrn_reflns_limit_l_min       -39
_diffrn_reflns_number            58436
_diffrn_reflns_point_group_measured_fraction_full 0.970
_diffrn_reflns_point_group_measured_fraction_max 0.967
_diffrn_reflns_theta_full        67.679
_diffrn_reflns_theta_max         68.290
_diffrn_reflns_theta_min         3.520
_diffrn_source_current           1.1
_diffrn_source_power             0.05500000000000001
_diffrn_source_voltage           50.0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    11.766
_exptl_absorpt_correction_T_max  0.190
_exptl_absorpt_correction_T_min  0.175
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2016/2 (Bruker,2016/2) was used for absorption correction.
wR2(int) was 0.1238 before and 0.0765 after correction.
The Ratio of minimum to maximum transmission is 0.5136.
The \l/2 correction factor is Not present.
;
_exptl_crystal_colour            'dark red'
_exptl_crystal_colour_modifier   dark
_exptl_crystal_colour_primary    red
_exptl_crystal_density_diffrn    1.926
_exptl_crystal_description       block
_exptl_crystal_F_000             2926
_exptl_crystal_size_max          0.2
_exptl_crystal_size_mid          0.2
_exptl_crystal_size_min          0.15
_refine_diff_density_max         2.184
_refine_diff_density_min         -2.053
_refine_diff_density_rms         0.172
_refine_ls_abs_structure_details
;
 Refined as an inversion twin.
;
_refine_ls_abs_structure_Flack   0.023(11)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.052
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1064
_refine_ls_number_reflns         18050
_refine_ls_number_restraints     1037
_refine_ls_restrained_S_all      1.071
_refine_ls_R_factor_all          0.0501
_refine_ls_R_factor_gt           0.0467
_refine_ls_shift/su_max          0.004
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0982P)^2^+4.2915P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1346
_refine_ls_wR_factor_ref         0.1390
_reflns_Friedel_coverage         0.877
_reflns_Friedel_fraction_full    0.952
_reflns_Friedel_fraction_max     0.947
_reflns_number_gt                16772
_reflns_number_total             18050
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d4ce00493k2.cif
_cod_data_source_block           3
_cod_depositor_comments
'Adding full bibliography for 7249257--7249263.cif.'
_cod_original_cell_volume        5088.7(5)
_cod_database_code               7249261
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   0.271
_shelx_estimated_absorpt_t_min   0.202
_olex2_refinement_description
;
1. Twinned data refinement
 Scales: 0.977(11)
 0.023(11)
2. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups
3. Rigid bond restraints
 All non-hydrogen atoms
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
4. Uiso/Uaniso restraints and constraints
All non-hydrogen atoms have similar U: within 2A with sigma of 0.04 and sigma
for terminal atoms of 0.08 within 2A
5. Same fragment restrains
{S101, O101, C101, C102} sigma for 1-2: 0.02, 1-3: 0.04
as in
{S102, O102, C103, C104}
{S101, O101, C101, C102} sigma for 1-2: 0.02, 1-3: 0.04
as in
{S104, O104, C107, C108}
{S101, O101, C101, C102} sigma for 1-2: 0.02, 1-3: 0.04
as in
{S105, O105, C109, C110}
{S101, O101, C101, C102} sigma for 1-2: 0.02, 1-3: 0.04
as in
{S103, O103, C105, C106}
{S101, O101, C101, C102} sigma for 1-2: 0.02, 1-3: 0.04
as in
{S106, O106, C111, C112}
6.a Riding coordinates:
 C104(H10J,H10K,H10L), C109(H10Y,H,HA), C110(H11A,H11B,H11C)
6.b Secondary CH2 refined with riding coordinates:
 C1(H1A,H1B), C2(H2A,H2B), C3(H3A,H3B), C4(H4A,H4B), C5(H5A,H5B), C6(H6A,H6B),
 C7(H7A,H7B), C14(H14A,H14B), C15(H15A,H15B), C16(H16A,H16B), C17(H17A,H17B),
 C18(H18A,H18B), C19(H19A,H19B), C20(H20A,H20B), C21(H21A,H21B), C22(H22A,H22B),
  C23(H23A,H23B), C24(H24A,H24B), C25(H25A,H25B), C26(H26A,H26B), C27(H27A,
 H27B), C28(H28A,H28B), C29(H29A,H29B), C31(H31A,H31B), C32(H32A,H32B),
 C33(H33A,H33B), C34(H34A,H34B), C41(H41A,H41B), C42(H42A,H42B), C43(H43A,H43B),
  C44(H44A,H44B), C45(H45A,H45B), C46(H46A,H46B), C47(H47A,H47B), C48(H48A,
 H48B), C49(H49A,H49B), C50(H50A,H50B), C51(H51A,H51B), C52(H52A,H52B),
 C53(H53A,H53B), C54(H54A,H54B)
6.c Me refined with riding coordinates:
 C101(H10A,H10B,H10C), C102(H10D,H10E,H10F), C103(H10G,H10H,H10I), C105(H10M,
 H10N,H10O), C106(H10P,H10Q,H10R), C107(H10S,H10T,H10U), C108(H10V,H10W,H10X),
 C111(H11D,H11E,H11F), C112(H11G,H11H,H11I)
6.d Aromatic/amide H refined with riding coordinates:
 C9(H9), C11(H11), C13(H13), C30(H30), C36(H36), C38(H38), C40(H40)
;
_smtbx_masks_void_probe_radius   1.2
_smtbx_masks_void_truncation_radius 1.2
_shelx_res_checksum              54435
_shelx_hkl_checksum              89967
_shelx_fab_checksum              91245
_olex2_submission_special_instructions 'No special instructions were received'