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_7709826
_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
'C106 H116 B4 Cl6 Cu12 N28 O2 S12 W4, 2(C F3 O3 S)'
_chemical_formula_sum            'C108 H116 B4 Cl6 Cu12 F6 N28 O8 S14 W4'
_chemical_formula_weight         4250.94
_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                91.961(2)
_cell_angle_beta                 91.493(2)
_cell_angle_gamma                104.795(2)
_cell_formula_units_Z            1
_cell_length_a                   9.8327(7)
_cell_length_b                   16.2223(12)
_cell_length_c                   25.3788(17)
_cell_measurement_reflns_used    9923
_cell_measurement_temperature    120.03
_cell_measurement_theta_max      27.477
_cell_measurement_theta_min      2.204
_cell_volume                     3909.1(5)
_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      120.03
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.997
_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  0.0736
_diffrn_reflns_av_unetI/netI     0.0794
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.997
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       30
_diffrn_reflns_limit_l_min       -30
_diffrn_reflns_number            46694
_diffrn_reflns_point_group_measured_fraction_full 0.997
_diffrn_reflns_point_group_measured_fraction_max 0.997
_diffrn_reflns_theta_full        25.000
_diffrn_reflns_theta_max         25.000
_diffrn_reflns_theta_min         2.144
_diffrn_source_current           1.0
_diffrn_source_power             0.05
_diffrn_source_voltage           50.0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    4.874
_exptl_absorpt_correction_T_max  0.7456
_exptl_absorpt_correction_T_min  0.5282
_exptl_absorpt_correction_type   multi-scan
_exptl_crystal_colour            brown
_exptl_crystal_colour_primary    brown
_exptl_crystal_density_diffrn    1.806
_exptl_crystal_description       block
_exptl_crystal_F_000             2068
_exptl_crystal_size_max          0.2
_exptl_crystal_size_mid          0.1
_exptl_crystal_size_min          0.05
_refine_diff_density_max         2.341
_refine_diff_density_min         -1.600
_refine_diff_density_rms         0.183
_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     868
_refine_ls_number_reflns         13713
_refine_ls_number_restraints     1021
_refine_ls_restrained_S_all      1.010
_refine_ls_R_factor_all          0.0748
_refine_ls_R_factor_gt           0.0516
_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^)+(0.0542P)^2^+12.3578P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1155
_refine_ls_wR_factor_ref         0.1242
_reflns_Friedel_coverage         0.000
_reflns_number_gt                10246
_reflns_number_total             13713
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d2dt00344a2.cif
_cod_data_source_block           mo_b210908d_0m_a
_cod_database_code               7709826
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   0.793
_shelx_estimated_absorpt_t_min   0.442
_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. Restrained distances
 C54-F2 = C54-F1 = C54-F3
 1.33 with sigma of 0.02
 C54-S7
 1.82 with sigma of 0.02
 S7-O2 = S7-O4 = S7-O3
 1.44 with sigma of 0.02
 C54-O3
 2.57 with sigma of 0.04
 C54-O2
 2.58 with sigma of 0.04
 C54-O4
 2.56 with sigma of 0.04
 C54-O2 \\sim C54-O4 \\sim C54-O3
 with sigma of 0.04
 C54-F2 \\sim C54-F1 \\sim C54-F3
 with sigma of 0.02
 F2-F1 \\sim F1-F3 \\sim F3-F2
 with sigma of 0.04
 S7-F2 \\sim S7-F1 \\sim S7-F3
 with sigma of 0.04
 S7-O2 \\sim S7-O4 \\sim S7-O3
 with sigma of 0.02
 O2-O4 \\sim O4-O3 \\sim O2-O3
 with sigma of 0.04
3. Uiso/Uaniso restraints and constraints
C54 \\sim F2 \\sim F1 \\sim F3 \\sim S7 \\sim O2 \\sim O4 \\sim O3: within 2A
with sigma of 0.04 and sigma for terminal atoms of 0.08 within 2A
Uanis(F2) \\sim Ueq, Uanis(F1) \\sim Ueq, Uanis(F3) \\sim Ueq: with sigma of
0.005 and sigma for terminal atoms of 0.01
4. Rigid body (RIGU) restrains
 C54, F2, F1, F3, S7, O2, O4, O3
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 W2, W1, Cu5, Cu2, Cu4, Cu3, Cu6, Cu1, S5, Cl2, S1, S2, S6, S4, S3, Cl1, Cl3,
 N4, N12, N6, N2, N10, N9, N8, N3, N14, N7, N11, N5, N1, O1, N13, C41, H41, C52,
  C42, C4, C18, H18, C32, H32, C9, C51, H51, C34, C50, C37, H37, C8, H8, C33,
 C35, H35, C19, H19, C40, C46, H46, B2, H2, C45, C53, H53A, H53B, H53C, C48,
 H48A, H48B, H48C, C15, H15A, H15B, H15C, C47, C25, C22, H22, C21, C43, H43A,
 H43B, H43C, C26, C7, C20, C23, H23, B1, H1, C31, H31, C3, H3, C5, H5A, H5B,
 H5C, C24, H24, C36, H36, C38, H38, C2, C49, H49A, H49B, H49C, C10, H10A, H10B,
 H10C, C17, H17, C29, C39, H39A, H39B, H39C, C12, C13, H13, C14, C16, H16, C30,
 H30, C28, C27, C44, H44A, H44B, H44C, C6, H6A, H6B, H6C, C1, H1A, H1B, H1C,
 C11, H11A, H11B, H11C, C54, F2, F1, F3, S7, O2, O4, O3
 with sigma for 1-2 distances of 0.001 and sigma for 1-3 distances of 0.002
5.a Ternary CH refined with riding coordinates:
 B2(H2), B1(H1)
5.b Aromatic/amide H refined with riding coordinates:
 C41(H41), C18(H18), C32(H32), C51(H51), C37(H37), C8(H8), C35(H35), C19(H19),
 C46(H46), C22(H22), C23(H23), C31(H31), C3(H3), C24(H24), C36(H36), C38(H38),
 C17(H17), C13(H13), C16(H16), C30(H30)
5.c Idealised Me refined as rotating group:
 C53(H53A,H53B,H53C), C48(H48A,H48B,H48C), C15(H15A,H15B,H15C), C43(H43A,H43B,
 H43C), C5(H5A,H5B,H5C), C49(H49A,H49B,H49C), C10(H10A,H10B,H10C), C39(H39A,
 H39B,H39C), C44(H44A,H44B,H44C), C6(H6A,H6B,H6C), C1(H1A,H1B,H1C), C11(H11A,
 H11B,H11C)
;
_smtbx_masks_void_probe_radius   1.2
_smtbx_masks_void_truncation_radius 1.2
_shelx_res_checksum              49964
_shelx_hkl_checksum              66987
_shelx_fab_checksum              39081
_olex2_submission_special_instructions 'No special instructions were received'