#------------------------------------------------------------------------------
#$Date: 2022-03-24 01:59:53 +0200 (Thu, 24 Mar 2022) $
#$Revision: 273944 $
#$URL: file:///home/coder/svn-repositories/cod/cif/7/70/98/7709827.cif $
#------------------------------------------------------------------------------
#
# This file is available in the Crystallography Open Database (COD),
# http://www.crystallography.net/
#
# All data on this site have been placed in the public domain by the
# contributors.
#
data_7709827
loop_
_publ_author_name
'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'
_publ_section_title
;
 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 H120 B4 Cl6 Cu12 N28 S12 W4, 2(C F3 O3 S), 1.4(C3 H7 N O), C H2 Cl2'
_chemical_formula_sum
'C113.2 H131.8 B4 Cl8 Cu12 F6 N29.4 O7.4 S14 W4'
_chemical_formula_weight         4410.23
_space_group_crystal_system      trigonal
_space_group_IT_number           147
_space_group_name_Hall           '-P 3'
_space_group_name_H-M_alt        'P -3'
_atom_sites_solution_hydrogens   geom
_audit_creation_date             2022-03-05
_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                90
_cell_angle_beta                 90
_cell_angle_gamma                120
_cell_formula_units_Z            3
_cell_length_a                   26.3933(10)
_cell_length_b                   26.3933(10)
_cell_length_c                   25.7305(10)
_cell_measurement_reflns_used    9902
_cell_measurement_temperature    120.01
_cell_measurement_theta_max      25.46
_cell_measurement_theta_min      25.46
_cell_volume                     15522.7(10)
_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      120.01
_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       'φ and ω scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.1135
_diffrn_reflns_av_unetI/netI     0.0322
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_limit_h_max       31
_diffrn_reflns_limit_h_min       -31
_diffrn_reflns_limit_k_max       31
_diffrn_reflns_limit_k_min       -31
_diffrn_reflns_limit_l_max       30
_diffrn_reflns_limit_l_min       -30
_diffrn_reflns_number            502784
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_theta_full        24.996
_diffrn_reflns_theta_max         24.996
_diffrn_reflns_theta_min         2.211
_diffrn_source_current           1.0
_diffrn_source_power             0.05
_diffrn_source_voltage           50.0
_exptl_absorpt_coefficient_mu    3.710
_exptl_absorpt_correction_T_max  0.7456
_exptl_absorpt_correction_T_min  0.4998
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2016/2 (Bruker,2016/2) was used for absorption correction.
wR2(int) was 0.1467 before and 0.1046 after correction.
The Ratio of minimum to maximum transmission is 0.6703.
The λ/2 correction factor is Not present.
;
_exptl_crystal_colour            red
_exptl_crystal_colour_primary    red
_exptl_crystal_density_diffrn    1.415
_exptl_crystal_description       BLOCK
_exptl_crystal_F_000             6462
_exptl_crystal_size_max          0.44
_exptl_crystal_size_mid          0.25
_exptl_crystal_size_min          0.25
_refine_diff_density_max         2.614
_refine_diff_density_min         -1.214
_refine_diff_density_rms         0.152
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.115
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     969
_refine_ls_number_reflns         18219
_refine_ls_number_restraints     212
_refine_ls_restrained_S_all      1.120
_refine_ls_R_factor_all          0.0778
_refine_ls_R_factor_gt           0.0535
_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/[σ²(Fo²)+(0.0635P)²+146.0746P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1346
_refine_ls_wR_factor_ref         0.1665
_reflns_Friedel_coverage         0.000
_reflns_number_gt                13944
_reflns_number_total             18219
_reflns_threshold_expression     'I > 2σ(I)'
_cod_data_source_file            d2dt00344a2.cif
_cod_data_source_block           mo_b210407b_0m_a
_cod_original_cell_volume        15522.7(13)
_cod_original_formula_sum
'C113.20 H131.80 B4 Cl8 Cu12 F6 N29.40 O7.40 S14 W4'
_cod_database_code               7709827
_shelx_shelxl_version_number     2018/3
_shelx_space_group_comment
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;
_shelx_estimated_absorpt_t_max   0.457
_shelx_estimated_absorpt_t_min   0.292
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All B(H) groups, All C(H) groups, All C(H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Restrained distances
 C59-N16
 1.36 with sigma of 0.02
 N16-C57
 1.45 with sigma of 0.02
 C61A-F2A = C61A-F1A = C61A-F3A
 1.33 with sigma of 0.02
 N16-C58
 1.46 with sigma of 0.02
 C59-O5
 1.22 with sigma of 0.02
 C61A-S7A
 1.82 with sigma of 0.02
 S7A-O3A = S7A-O1A = S7A-O2A
 1.44 with sigma of 0.02
 C61B-F3B = C61B-F2B = C61B-F1B
 1.33 with sigma of 0.02
 C61B-S7B
 1.82 with sigma of 0.02
 S7B-O1B = S7B-O3B = S7B-O2B
 1.44 with sigma of 0.02
 Cl5A-Cl4A
 2.916 with sigma of 0.03
 Cl5A-C60A
 1.78 with sigma of 0.02
 Cl5A-C60A = Cl4A-C60A
 1.771 with sigma of 0.01
 Cl4A-C60A
 1.77 with sigma of 0.02
 N15-C54
 1.45 with sigma of 0.02
 N15-C55
 1.46 with sigma of 0.02
 C56-O4
 1.22 with sigma of 0.02
 C56-N15
 1.36 with sigma of 0.02
 Cl4B-C60B
 1.78 with sigma of 0.02
 Cl4B-Cl5B
 2.916 with sigma of 0.03
 Cl5B-C60B
 1.77 with sigma of 0.02
 Cl4B-C60B = Cl5B-C60B
 1.771 with sigma of 0.01
 C59-C58
 2.45 with sigma of 0.04
 C59-C57
 2.46 with sigma of 0.04
 C61A-O1A
 2.56 with sigma of 0.04
 C61A-O3A
 2.58 with sigma of 0.04
 C61A-O2A
 2.57 with sigma of 0.04
 C61B-O3B
 2.56 with sigma of 0.04
 C61B-O1B
 2.58 with sigma of 0.04
 C61B-O2B
 2.57 with sigma of 0.04
 Cl5A-Cl4A
 2.92 with sigma of 0.04
 C56-C54
 2.46 with sigma of 0.04
 C56-C55
 2.45 with sigma of 0.04
 Cl4B-Cl5B
 2.92 with sigma of 0.04
 S7A-O3A \\sim S7A-O1A \\sim S7A-O2A
 with sigma of 0.02
 N16-C57 \\sim N16-C58
 with sigma of 0.02
 C61A-O3A \\sim C61A-O1A \\sim C61A-O2A
 with sigma of 0.04
 S7A-F2A \\sim S7A-F1A \\sim S7A-F3A
 with sigma of 0.04
 O3A-O1A \\sim O1A-O2A \\sim O3A-O2A
 with sigma of 0.04
 C61A-F2A \\sim C61A-F1A \\sim C61A-F3A
 with sigma of 0.02
 F2A-F1A \\sim F1A-F3A \\sim F3A-F2A
 with sigma of 0.04
 C61B-O1B \\sim C61B-O3B \\sim C61B-O2B
 with sigma of 0.04
 F3B-F2B \\sim F2B-F1B \\sim F1B-F3B
 with sigma of 0.04
 S7B-F3B \\sim S7B-F2B \\sim S7B-F1B
 with sigma of 0.04
 C61B-F3B \\sim C61B-F2B \\sim C61B-F1B
 with sigma of 0.02
 S7B-O1B \\sim S7B-O3B \\sim S7B-O2B
 with sigma of 0.02
 O1B-O3B \\sim O3B-O2B \\sim O1B-O2B
 with sigma of 0.04
 N15-C54 \\sim N15-C55
 with sigma of 0.02
3. Restrained planarity
 C59, O5, N16, C57, C58
 with sigma of 0.1
 C56, O4, N15, C54, C55
 with sigma of 0.1
4. Uiso/Uaniso restraints and constraints
C59 \\sim O5 \\sim N16 \\sim C57 \\sim C58: within 2A with sigma of 0.04 and
sigma for terminal atoms of 0.08 within 2A
N16 \\sim C58: within 1.7A with sigma of 0.002 and sigma for terminal atoms of
0.004 within 1.7A
C59 \\sim O5: within 1.7A with sigma of 0.002 and sigma for terminal atoms of
0.004 within 1.7A
N16 \\sim C57: within 1.7A with sigma of 0.002 and sigma for terminal atoms of
0.004 within 1.7A
C61A \\sim F2A \\sim F1A \\sim F3A \\sim S7A \\sim O3A \\sim O1A \\sim O2A:
within 2A with sigma of 0.04 and sigma for terminal atoms of 0.08 within 2A
C61B \\sim F3B \\sim F2B \\sim F1B \\sim S7B \\sim O1B \\sim O3B \\sim O2B:
within 2A with sigma of 0.04 and sigma for terminal atoms of 0.08 within 2A
Cl5A \\sim Cl4A \\sim C60A: within 2A with sigma of 0.04 and sigma for terminal
atoms of 0.08 within 2A
C56 \\sim O4 \\sim N15 \\sim C54 \\sim C55: within 2A with sigma of 0.04 and
sigma for terminal atoms of 0.08 within 2A
Cl4B \\sim Cl5B \\sim C60B: within 2A with sigma of 0.04 and sigma for terminal
atoms of 0.08 within 2A
C56 \\sim O4: within 1.7A with sigma of 0.01 and sigma for terminal atoms of
0.02 within 1.7A
Uanis(C59) \\sim Ueq, Uanis(N16) \\sim Ueq: with sigma of 0.005 and sigma for
terminal atoms of 0.01
5. Rigid body (RIGU) restrains
 C59, O5, N16, C57, C58
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 C61A, F2A, F1A, F3A, S7A, O3A, O1A, O2A
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 C61B, F3B, F2B, F1B, S7B, O1B, O3B, O2B
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 Cl5A, Cl4A, C60A
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 C56, O4, N15, C54, C55
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 Cl4B, Cl5B, C60B
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
6. Others
 Fixed Sof: C61A(0.5) F2A(0.5) F1A(0.5) F3A(0.5) S7A(0.5) O3A(0.5) O1A(0.5)
 O2A(0.5) C61B(0.5) F3B(0.5) F2B(0.5) F1B(0.5) S7B(0.5) O1B(0.5) O3B(0.5)
 O2B(0.5) C59(0.4) H59(0.4) O5(0.4) N16(0.4) C57(0.4) H57A(0.4) H57B(0.4)
 H57C(0.4) C58(0.4) H58A(0.4) H58B(0.4) H58C(0.4) Cl5A(0.15) Cl4A(0.15)
 C60A(0.15) H60A(0.15) H60B(0.15) C56(0.3) H56(0.3) O4(0.3) N15(0.3) C54(0.3)
 H54A(0.3) H54B(0.3) H54C(0.3) C55(0.3) H55A(0.3) H55B(0.3) H55C(0.3)
 Cl4B(0.35) Cl5B(0.35) C60B(0.35) H60C(0.35) H60D(0.35)
7.a Ternary CH refined with riding coordinates:
 B2(H2), B1(H1)
7.b Secondary CH2 refined with riding coordinates:
 C27(H27A,H27B), C60A(H60A,H60B), C60B(H60C,H60D)
7.c Aromatic/amide H refined with riding coordinates:
 C3(H3), C13(H13), C8(H8), C46(H46), C20(H20), C22(H22), C51(H51), C41(H41),
 C25(H25), C19(H19), C35(H35), C33(H33), C30(H30), C32(H32), C26(H26), C17(H17),
  C36(H36), C16(H16), C37(H37), C38(H38), C59(H59), C56(H56)
7.d Idealised Me refined as rotating group:
 C5(H5A,H5B,H5C), C10(H10A,H10B,H10C), C11(H11A,H11B,H11C), C15(H15A,H15B,
 H15C), C53(H53A,H53B,H53C), C6(H6A,H6B,H6C), C1(H1A,H1B,H1C), C39(H39A,H39B,
 H39C), C48(H48A,H48B,H48C), C43(H43A,H43B,H43C), C49(H49A,H49B,H49C), C44(H44A,
 H44B,H44C), C57(H57A,H57B,H57C), C58(H58A,H58B,H58C), C54(H54A,H54B,H54C),
 C55(H55A,H55B,H55C)
;
_smtbx_masks_void_probe_radius   1.2
_smtbx_masks_void_truncation_radius 1.2
