#------------------------------------------------------------------------------
#$Date: 2020-01-24 01:36:44 +0200 (Fri, 24 Jan 2020) $
#$Revision: 247125 $
#$URL: file:///home/coder/svn-repositories/cod/cif/4/13/39/4133989.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_4133989
loop_
_publ_author_name
'Wang, Li-Juan'
'Li, Xin'
'Bai, Sha'
'Wang, Yaoyu'
'Han, Ying-Feng'
_publ_section_title
;
 Self-Assembly, Structural Transformation and Guest-Binding Properties of
 Supramolecular Assemblies with Triangular Metal-Metal Bonded Units.
;
_journal_name_full               'Journal of the American Chemical Society'
_journal_paper_doi               10.1021/jacs.9b12309
_journal_year                    2020
_chemical_formula_moiety         'C224 H198 N24 Pt12 S12 B6 F24'
_chemical_formula_sum            'C224 H198 B6 F24 N24 Pt12 S12'
_chemical_formula_weight         6472.62
_space_group_crystal_system      trigonal
_space_group_IT_number           167
_space_group_name_Hall           '-R 3 2"c'
_space_group_name_H-M_alt        'R -3 c :H'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     iterative
_audit_creation_date             2019-11-04
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                120
_cell_formula_units_Z            18
_cell_length_a                   43.390(2)
_cell_length_b                   43.390(2)
_cell_length_c                   75.917(4)
_cell_measurement_reflns_used    9688
_cell_measurement_temperature    153(2)
_cell_measurement_theta_max      24.36
_cell_measurement_theta_min      2.23
_cell_volume                     123780(10)
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_computing_structure_solution    'olex2.solve (Bourhis et al., 2015)'
_diffrn_ambient_temperature      153.38
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.998
_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  0.0755
_diffrn_reflns_av_unetI/netI     0.0187
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_limit_h_max       52
_diffrn_reflns_limit_h_min       -52
_diffrn_reflns_limit_k_max       52
_diffrn_reflns_limit_k_min       -52
_diffrn_reflns_limit_l_max       91
_diffrn_reflns_limit_l_min       -91
_diffrn_reflns_number            1241724
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         25.367
_diffrn_reflns_theta_min         2.229
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    6.230
_exptl_absorpt_correction_T_max  0.7452
_exptl_absorpt_correction_T_min  0.4899
_exptl_absorpt_correction_type   multi-scan
_exptl_crystal_colour            red
_exptl_crystal_colour_primary    red
_exptl_crystal_density_diffrn    1.563
_exptl_crystal_description       block
_exptl_crystal_F_000             55512
_exptl_crystal_size_max          0.25
_exptl_crystal_size_mid          0.24
_exptl_crystal_size_min          0.24
_refine_diff_density_max         1.823
_refine_diff_density_min         -1.629
_refine_diff_density_rms         0.147
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.058
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1407
_refine_ls_number_reflns         25216
_refine_ls_number_restraints     2594
_refine_ls_restrained_S_all      1.061
_refine_ls_R_factor_all          0.0705
_refine_ls_R_factor_gt           0.0506
_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)+(0.0737P)²+2585.9495P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1325
_refine_ls_wR_factor_ref         0.1544
_reflns_Friedel_coverage         0.000
_reflns_number_gt                19376
_reflns_number_total             25216
_reflns_threshold_expression     'I > 2σ(I)'
_cod_data_source_file            ja9b12309_si_011.cif
_cod_data_source_block           Complex_5b
_cod_original_cell_volume        123778(15)
_cod_original_sg_symbol_H-M      'R -3 c'
_cod_original_formula_sum        'C224 H198 N24 Pt12 S12 B6 F24'
_cod_database_code               4133989
_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   0.057
_shelx_estimated_absorpt_t_min   0.054
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
2. Restrained distances
 C25-C24
 1.2 with sigma of 0.02
 C52-C53
 1.54 with sigma of 0.02
 C94-C95
 1.2 with sigma of 0.02
 C65-C64
 1.2 with sigma of 0.02
 C51-N4
 1.48 with sigma of 0.02
 N1-C26
 1.48 with sigma of 0.02
 N6-C63
 1.48 with sigma of 0.02
 C68-N7
 1.48 with sigma of 0.02
 N12-C105
 1.48 with sigma of 0.02
 N10-C93
 1.48 with sigma of 0.02
 C51-C52
 1.54 with sigma of 0.02
 C64-C63
 1.54 with sigma of 0.02
 C106-C105
 1.54 with sigma of 0.02
 C68-C67
 1.54 with sigma of 0.02
 C93-C94
 1.54 with sigma of 0.02
 C105-C106
 1.54 with sigma of 0.02
 C107-C106
 1.2 with sigma of 0.02
 C22-C21
 1.4 with sigma of 0.02
 H66A-H68B
 2.5 with sigma of 0.02
 C67-C66
 1.42 with sigma of 0.02
 C52-C53 = C66-C67
 1.5 with sigma of 0.02
 F6-F7
 2.23 with sigma of 0.02
 B3-F9
 1.38 with sigma of 0.02
 B3-F10
 1.38 with sigma of 0.02
 F11-B3
 1.38 with sigma of 0.02
 Pt8-S0AA \\sim Pt4-S3
 with sigma of 0.02
 S0AA-C60 \\sim S3-C60
 with sigma of 0.02
3. Rigid bond restraints
 C24, C25
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.02
 N6, C61
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.02
 F1, F2, F3, F4, F5, F6, F7, F8, F9, F10, F11, F12
 with sigma for 1-2 distances of 0.005 and sigma for 1-3 distances of 0.005
 Pt6, C108
 with sigma for 1-2 distances of 0.005 and sigma for 1-3 distances of 0.01
 S3, C60
 with sigma for 1-2 distances of 0.001 and sigma for 1-3 distances of 0.002
4. Uiso/Uaniso restraints and constraints
C1 \\sim C2 \\sim C3 \\sim C4 \\sim C5 \\sim C6 \\sim C7 \\sim C8 \\sim C9
\\sim C10 \\sim C11 \\sim C12 \\sim C13 \\sim C14 \\sim C15 \\sim C16 \\sim C17
\\sim C18 \\sim C19 \\sim C20 \\sim C21 \\sim C22 \\sim C23 \\sim C24 \\sim C25
\\sim C26 \\sim C27 \\sim C28 \\sim C29 \\sim C30 \\sim C31 \\sim C32 \\sim C33
\\sim C34 \\sim C35 \\sim C36 \\sim C37 \\sim C38 \\sim C39 \\sim C40 \\sim C41
\\sim C42 \\sim C43 \\sim C44 \\sim C45 \\sim C46 \\sim C47 \\sim C48 \\sim C49
\\sim C50 \\sim C51 \\sim C52 \\sim C53 \\sim C54 \\sim C55 \\sim C56 \\sim C57
\\sim C58 \\sim C59 \\sim C60 \\sim C61 \\sim C62 \\sim C63 \\sim C64 \\sim C65
\\sim C66 \\sim C67 \\sim C68 \\sim C69 \\sim C70 \\sim C71 \\sim C72 \\sim C73
\\sim C74 \\sim C75 \\sim C76 \\sim C77 \\sim C78 \\sim C79 \\sim C80 \\sim C81
\\sim C82 \\sim C83 \\sim C84 \\sim C85 \\sim C86 \\sim C87 \\sim C88 \\sim C89
\\sim C90 \\sim C91 \\sim C92 \\sim C93 \\sim C94 \\sim C95 \\sim C96 \\sim C97
\\sim C98 \\sim C99 \\sim C100 \\sim C101 \\sim C102 \\sim C103 \\sim C104
\\sim C105 \\sim C106 \\sim C107 \\sim C108 \\sim C109 \\sim C110 \\sim C111
\\sim C112: within 3.8A with sigma of 0.01 and sigma for terminal atoms of 0.02
Pt3 \\sim Pt10: within 2A with sigma of 0.01 and sigma for terminal atoms of
0.02
Pt5 \\sim Pt9 \\sim Pt4 \\sim Pt8 \\sim Pt6 \\sim Pt7: within 2A with sigma of
0.01 and sigma for terminal atoms of 0.02
S0AA \\sim S3: within 2A with sigma of 0.01 and sigma for terminal atoms of 0.02
Uanis(C66) \\sim Ueq, Uanis(C67) \\sim Ueq, Uanis(C64) \\sim Ueq, Uanis(C65)
\\sim Ueq, Uanis(C95) \\sim Ueq, Uanis(C94) \\sim Ueq, Uanis(C53) \\sim Ueq,
Uanis(C52) \\sim Ueq, Uanis(B3) \\sim Ueq: with sigma of 0.01 and sigma for
terminal atoms of 0.02
Uanis(S0AA) \\sim Ueq, Uanis(S3) \\sim Ueq: with sigma of 0.01 and sigma for
terminal atoms of 0.02
5. Others
 Sof(Pt7)=Sof(Pt8)=Sof(Pt9)=Sof(S0AA)=1-FVAR(1)
 Sof(Pt4)=Sof(Pt5)=Sof(Pt6)=Sof(S3)=FVAR(1)
 Sof(Pt10)=1-FVAR(2)
 Sof(Pt3)=FVAR(2)
6.a Secondary CH2 refined with riding coordinates:
 C26(H26A,H26B), C51(H51A,H51B), C63(H63A,H63B), C68(H68A,H68B), C93(H93A,
 H93B), C105(H10A,H10B)
6.b Aromatic/amide H refined with riding coordinates:
 C1(H1), C2(H2), C3(H3), C4(H4), C5(H5), C6(H6), C7(H7), C8(H8), C9(H9),
 C10(H10), C11(H11), C12(H12), C13(H13), C14(H14), C15(H15), C16(H16), C17(H17),
  C18(H18), C19(H19), C20(H20), C21(H21), C22(H22), C23(H23), C25(H25),
 C27(H27), C28(H28), C31(H31), C34(H34), C35(H35), C37(H37), C39(H39), C41(H41),
  C43(H43), C44(H44), C46(H46), C47(H47), C49(H49), C50(H50), C52(H52),
 C54(H54), C55(H55), C57(H57), C58(H58), C61(H61), C62(H62), C64(H64), C67(H67),
  C70(H70), C71(H71), C73(H73), C74(H74), C76(H76), C77(H77), C79(H79),
 C81(H81), C83(H83), C85(H85), C86(H86), C88(H88), C89(H89), C91(H91), C92(H92),
  C94(H94), C97(H97), C98(H98), C100(H100), C101(H101), C103(H103), C104(H104),
 C106(H106), C108(H108), C109(H109), C110(H110), C111(H111), C112(H112)
6.c X=CH2 refined with riding coordinates:
 C24(H24A,H24B), C53(H53A,H53B), C65(H65A,H65B), C66(H66A,H66B), C95(H95A,
 H95B), C107(H10C,H10D)
;
