Construction of cluster-based supramolecular wire and rectangle
Tan, Yi; Wang, Zhi-Kang; Lang, Fei-Fan; Yu, Hui-Min; Chen, Cao; Ni, Chun-Yan; Wang, Meng-Yi; Song, Ying-Lin; Lang, Jian-Ping; Dalton Transactions  (2022) –; doi:10.1039/D2DT00344A

data_7709825
_publ_section_title
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 Construction of cluster-based supramolecular wire and rectangle
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_journal_name_full               'Dalton Transactions'
_journal_paper_doi               10.1039/D2DT00344A
_journal_year                    2022
_chemical_formula_moiety         'C44 H52 B2 Cl2 Cu4 N16 S8 W2, 1.6(C H Cl3)'
_chemical_formula_sum            'C45.6 H53.6 B2 Cl6.8 Cu4 N16 S8 W2'
_chemical_formula_weight         1966.86
_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
_audit_creation_date             2022-02-28
_audit_creation_method
;
Olex2 1.3
(compiled 2020.06.28 svn.raecde09e for OlexSys, GUI svn.r6132)
;
_audit_update_record
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2022-03-17 deposited with the CCDC.	2022-03-22 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 113.8940(10)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   16.8463(9)
_cell_length_b                   17.3053(10)
_cell_length_c                   12.4887(8)
_cell_measurement_reflns_used    9506
_cell_measurement_temperature    296.15
_cell_measurement_theta_max      27.25
_cell_measurement_theta_min      2.35
_cell_volume                     3328.8(3)
_computing_cell_refinement       'SAINT v8.37A (Bruker, 2015)'
_computing_data_collection       'Bruker APEX2'
_computing_data_reduction        'SAINT v8.37A (Bruker, 2015)'
_computing_molecular_graphics    'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2018/3 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT 2018/2 (Sheldrick, 2018)'
_diffrn_ambient_temperature      296.15
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.1021
_diffrn_reflns_av_unetI/netI     0.0662
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_limit_h_max       20
_diffrn_reflns_limit_h_min       -20
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_l_max       14
_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_number            42912
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_theta_full        24.999
_diffrn_reflns_theta_max         24.999
_diffrn_reflns_theta_min         2.354
_diffrn_source_current           1.0
_diffrn_source_power             0.05
_diffrn_source_voltage           50.0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    5.267
_exptl_absorpt_correction_T_max  0.7456
_exptl_absorpt_correction_T_min  0.3421
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2014/5 (Bruker,2014/5) was used for absorption correction.
wR2(int) was 0.1806 before and 0.1128 after correction.
The Ratio of minimum to maximum transmission is 0.4588.
The \l/2 correction factor is Not present.
;
_exptl_crystal_colour            black
_exptl_crystal_colour_primary    black
_exptl_crystal_density_diffrn    1.962
_exptl_crystal_description       block
_exptl_crystal_F_000             1914
_exptl_crystal_size_max          0.2
_exptl_crystal_size_mid          0.1
_exptl_crystal_size_min          0.05
_refine_diff_density_max         1.123
_refine_diff_density_min         -1.259
_refine_diff_density_rms         0.134
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.017
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     394
_refine_ls_number_reflns         5854
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.017
_refine_ls_R_factor_all          0.0567
_refine_ls_R_factor_gt           0.0342
_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/[\s^2^(Fo^2^)+(0.0003P)^2^+8.5847P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0692
_refine_ls_wR_factor_ref         0.0766
_reflns_Friedel_coverage         0.000
_reflns_number_gt                4557
_reflns_number_total             5854
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d2dt00344a2.cif
_cod_data_source_block           b201126c_0ma_a
_cod_original_formula_sum        'C45.60 H53.60 B2 Cl6.80 Cu4 N16 S8 W2'
_cod_database_code               7709825
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   0.779
_shelx_estimated_absorpt_t_min   0.419
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All B(H) groups, All C(H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Others
 Fixed Sof: Cl2(0.8) Cl4(0.8) Cl3(0.8) C23(0.8) H23(0.8)
3.a Ternary CH refined with riding coordinates:
 B1(H1), C23(H23)
3.b Aromatic/amide H refined with riding coordinates:
 C17(H17), C19(H19), C13(H13), C8(H8), C3(H3), C18(H18), C16(H16)
3.c Idealised Me refined as rotating group:
 C15(H15A,H15B,H15C), C10(H10A,H10B,H10C), C6(H6A,H6B,H6C), C1(H1A,H1B,H1C),
 C5(H5A,H5B,H5C), C12(H12A,H12B,H12C)
;
_shelx_res_checksum              21568
_shelx_hkl_checksum              17558
_olex2_submission_special_instructions 'No special instructions were received'