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_7709824
_publ_section_title
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 Construction of cluster-based supramolecular wire and rectangle
;
_journal_name_full               'Dalton Transactions'
_journal_paper_doi               10.1039/D2DT00344A
_journal_year                    2022
_chemical_formula_moiety
'C104 H118 B4 Cl6 Cu12 N30 S12 W4, 2(C F3 O3 S)'
_chemical_formula_sum            'C106 H118 B4 Cl6 Cu12 F6 N30 O6 S14 W4'
_chemical_formula_weight         4224.96
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_atom_sites_solution_hydrogens   geom
_audit_creation_date             2022-03-15
_audit_creation_method
;
Olex2 1.3
(compiled 2020.06.28 svn.raecde09e for OlexSys, GUI svn.r6132)
;
_audit_update_record
;
2022-03-17 deposited with the CCDC.	2022-03-22 downloaded from the CCDC.
;
_cell_angle_alpha                101.575(2)
_cell_angle_beta                 97.944(2)
_cell_angle_gamma                97.164(2)
_cell_formula_units_Z            1
_cell_length_a                   10.0436(7)
_cell_length_b                   18.5322(14)
_cell_length_c                   25.0944(18)
_cell_measurement_reflns_used    9395
_cell_measurement_temperature    119.98
_cell_measurement_theta_max      27.48
_cell_measurement_theta_min      2.24
_cell_volume                     4475.6(6)
_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 2014/5 (Sheldrick, 2014)'
_diffrn_ambient_temperature      119.98
_diffrn_measured_fraction_theta_full 0.998
_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           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.1102
_diffrn_reflns_av_unetI/netI     0.1062
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.994
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       24
_diffrn_reflns_limit_k_min       -24
_diffrn_reflns_limit_l_max       32
_diffrn_reflns_limit_l_min       -32
_diffrn_reflns_number            77776
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.994
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.551
_diffrn_reflns_theta_min         1.808
_diffrn_source_current           1.0
_diffrn_source_power             0.05
_diffrn_source_voltage           50.0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    4.256
_exptl_absorpt_correction_T_max  0.7456
_exptl_absorpt_correction_T_min  0.4662
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2016/2 (Bruker,2016/2) was used for absorption correction.
wR2(int) was 0.1226 before and 0.0969 after correction.
The Ratio of minimum to maximum transmission is 0.6253.
The \l/2 correction factor is Not present.
;
_exptl_crystal_colour            brown
_exptl_crystal_colour_primary    brown
_exptl_crystal_density_diffrn    1.568
_exptl_crystal_description       block
_exptl_crystal_F_000             2056
_exptl_crystal_size_max          0.2
_exptl_crystal_size_mid          0.1
_exptl_crystal_size_min          0.05
_refine_diff_density_max         3.416
_refine_diff_density_min         -2.761
_refine_diff_density_rms         0.202
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.036
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     859
_refine_ls_number_reflns         20542
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.036
_refine_ls_R_factor_all          0.1030
_refine_ls_R_factor_gt           0.0677
_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^)+(0.0597P)^2^+33.6432P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1538
_refine_ls_wR_factor_ref         0.1694
_reflns_Friedel_coverage         0.000
_reflns_number_gt                13772
_reflns_number_total             20542
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d2dt00344a2.cif
_cod_data_source_block           mo_b210702d_0m_a
_cod_database_code               7709824
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   0.815
_shelx_estimated_absorpt_t_min   0.483
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All B(H) groups, All C(H) groups, All N(H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2.a Ternary CH refined with riding coordinates:
 B2(H2), B1(H1)
2.b Aromatic/amide H refined with riding coordinates:
 C13(H13), C40(H40), C3(H3), C50(H50), N8(H8), C45(H45), C25(H25), C36(H36),
 C34(H34), C29(H29), C16(H16), C17(H17), C8(H8A), C22(H22), C23(H23), C37(H37),
 C35(H35), C18(H18), C30(H30), C19(H19), C32(H32)
2.c Idealised Me refined as rotating group:
 C5(H5A,H5B,H5C), C15(H15A,H15B,H15C), C42(H42A,H42B,H42C), C52(H52A,H52B,
 H52C), C11(H11A,H11B,H11C), C38(H38A,H38B,H38C), C1(H1A,H1B,H1C), C47(H47A,
 H47B,H47C), C10(H10A,H10B,H10C), C43(H43A,H43B,H43C), C48(H48A,H48B,H48C),
 C6(H6A,H6B,H6C)
;
_smtbx_masks_void_probe_radius   1.2
_smtbx_masks_void_truncation_radius 1.2
_shelx_res_checksum              72619
_shelx_hkl_checksum              86479
_shelx_fab_checksum              48888
_olex2_submission_special_instructions 'No special instructions were received'