#------------------------------------------------------------------------------
#$Date: 2020-01-24 01:40:32 +0200 (Fri, 24 Jan 2020) $
#$Revision: 247129 $
#$URL: file:///home/coder/svn-repositories/cod/cif/4/13/39/4133993.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_4133993
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         'C212 H188 B4 F16 N36 Pt12 S12'
_chemical_formula_sum            'C212 H188 B4 F16 N36 Pt12 S12'
_chemical_formula_weight         6312.92
_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
_audit_creation_date             2019-10-27
_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                   42.847(5)
_cell_length_b                   42.847(5)
_cell_length_c                   76.037(9)
_cell_measurement_reflns_used    9848
_cell_measurement_temperature    164(2)
_cell_measurement_theta_max      24.21
_cell_measurement_theta_min      2.30
_cell_volume                     120892(2)
_computing_cell_refinement       'SAINT V8.38A (?, 2016)'
_computing_data_reduction        'SAINT V8.38A (?, 2016)'
_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    'SHELXT 2014/5 (Sheldrick, 2014)'
_diffrn_ambient_temperature      163.76
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.997
_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  0.0910
_diffrn_reflns_av_unetI/netI     0.0282
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.997
_diffrn_reflns_limit_h_max       51
_diffrn_reflns_limit_h_min       -51
_diffrn_reflns_limit_k_max       51
_diffrn_reflns_limit_k_min       -51
_diffrn_reflns_limit_l_max       91
_diffrn_reflns_limit_l_min       -91
_diffrn_reflns_number            990245
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.997
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         25.402
_diffrn_reflns_theta_min         2.390
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    6.374
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    1.561
_exptl_crystal_description       block
_exptl_crystal_F_000             54072
_exptl_crystal_size_max          0.32
_exptl_crystal_size_mid          0.30
_exptl_crystal_size_min          0.29
_refine_diff_density_max         2.652
_refine_diff_density_min         -1.495
_refine_diff_density_rms         0.173
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.046
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1209
_refine_ls_number_reflns         24670
_refine_ls_number_restraints     422
_refine_ls_restrained_S_all      1.051
_refine_ls_R_factor_all          0.0964
_refine_ls_R_factor_gt           0.0597
_refine_ls_shift/su_max          0.004
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[σ²(Fo²)+(0.1024P)²+3135.6072P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1601
_refine_ls_wR_factor_ref         0.2032
_reflns_Friedel_coverage         0.000
_reflns_number_gt                16305
_reflns_number_total             24670
_reflns_threshold_expression     'I > 2σ(I)'
_cod_data_source_file            ja9b12309_si_010.cif
_cod_data_source_block           Complex_5a
_cod_original_cell_volume        120890(31)
_cod_original_sg_symbol_H-M      'R -3 c'
_cod_database_code               4133993
_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.
;
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
2. Restrained distances
 C99-C102
 1.34 with sigma of 0.02
 C98-C59
 1.54 with sigma of 0.02
 C101-C98
 1.34 with sigma of 0.02
 C62-C61 = C45-C83
 1.34 with sigma of 0.02
 C98-C59 = C62-C37 = C99-C60
 1.54 with sigma of 0.02
 C74-C103
 1.54 with sigma of 0.02
 C107-C103 = C108-C103
 1.34 with sigma of 0.02
 C105-C104
 1.34 with sigma of 0.02
 C100-C104
 1.54 with sigma of 0.02
 C105-C104 = C106-C104
 1.34 with sigma of 0.02
 C107-C103 \\sim C108-C103
 with sigma of 0.02
 C106-C104 \\sim C105-C104
 with sigma of 0.02
 C100-C105 \\sim C100-C106
 with sigma of 0.04
 N14-C8 \\sim N13-C8
 with sigma of 0.02
 C28-C10 \\sim C21-C10
 with sigma of 0.02
 C36-C28 \\sim C21-C17
 with sigma of 0.02
 C10-C17 \\sim C10-C36
 with sigma of 0.04
 C76-C65 \\sim C71-C76 \\sim C71-C80 \\sim C81-C80 \\sim C79-C81 \\sim C63-C79
\\sim C65-C63
 with sigma of 0.02
 C86-C70 \\sim C78-C86 \\sim C78-C75 \\sim C77-C75 \\sim C92-C77 \\sim C72-C92
\\sim C70-C72
 with sigma of 0.02
 C73-C66 \\sim C52-C73 \\sim C64-C52 \\sim C85-C64 \\sim C82-C85 \\sim C82-C84
\\sim C66-C84
 with sigma of 0.02
 C87-C91 \\sim C91-C95 \\sim C95-C93 \\sim C93-C94 \\sim C96-C94 \\sim C96-C97
\\sim C97-C87
 with sigma of 0.02
3. Rigid bond restraints
 C72, C92, C75, C78
 with sigma for 1-2 distances of 0.02 and sigma for 1-3 distances of 0.01
 C72, C70, C86
 with sigma for 1-2 distances of 0.02 and sigma for 1-3 distances of 0.01
 N11, C60
 with sigma for 1-2 distances of 0.02 and sigma for 1-3 distances of 0.01
 N9, C90, C61, C62, C101, C98
 with sigma for 1-2 distances of 0.02 and sigma for 1-3 distances of 0.01
 Pt2, C71
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.02
4. Uiso/Uaniso restraints and constraints
C94 \\sim C93 \\sim C95 \\sim C91 \\sim C87 \\sim C97 \\sim C96: within 2A with
sigma of 0.01 and sigma for terminal atoms of 0.02
C60 \\sim C99 \\sim C102: within 2A with sigma of 0.01 and sigma for terminal
atoms of 0.02
C74: within 2A with sigma of 0.01 and sigma for terminal atoms of 0.02
C59 \\sim C98 \\sim C101: within 2A with sigma of 0.01 and sigma for terminal
atoms of 0.02
C103 \\sim C107 \\sim C108 \\sim C74: within 2A with sigma of 0.01 and sigma
for terminal atoms of 0.02
C100 \\sim C104 \\sim C106 \\sim C105: within 2A with sigma of 0.01 and sigma
for terminal atoms of 0.02
C80 \\sim C71 \\sim C76 \\sim C65 \\sim C63 \\sim C79 \\sim C81: within 2A with
sigma of 0.01 and sigma for terminal atoms of 0.02
Uanis(C83) \\sim Ueq, Uanis(C64) \\sim Ueq, Uanis(C85) \\sim Ueq, Uanis(C82)
\\sim Ueq, Uanis(C84) \\sim Ueq, Uanis(C66) \\sim Ueq, Uanis(C92) \\sim Ueq,
Uanis(C78) \\sim Ueq, Uanis(C77) \\sim Ueq: with sigma of 0.01 and sigma for
terminal atoms of 0.02
Uanis(C102) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
Uanis(C88) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
Uanis(C98) \\sim Ueq, Uanis(C101) \\sim Ueq: with sigma of 0.01 and sigma for
terminal atoms of 0.02
Uanis(C103) \\sim Ueq, Uanis(C107) \\sim Ueq, Uanis(C108) \\sim Ueq: with sigma
of 0.01 and sigma for terminal atoms of 0.02
Uanis(C106) \\sim Ueq, Uanis(C104) \\sim Ueq, Uanis(C105) \\sim Ueq: with sigma
of 0.01 and sigma for terminal atoms of 0.02
Uanis(C71) \\sim Ueq, Uanis(C80) \\sim Ueq, Uanis(C81) \\sim Ueq, Uanis(C79)
\\sim Ueq, Uanis(C63) \\sim Ueq, Uanis(C65) \\sim Ueq, Uanis(C76) \\sim Ueq:
with sigma of 0.01 and sigma for terminal atoms of 0.02
5. Others
 Sof(H10G)=Sof(C108)=Sof(H10O)=Sof(H10P)=1-FVAR(1)
 Sof(H103)=Sof(C107)=Sof(H10M)=Sof(H10N)=FVAR(1)
 Sof(H10H)=Sof(C106)=Sof(H10K)=Sof(H10L)=1-FVAR(2)
 Sof(H104)=Sof(C105)=Sof(H10I)=Sof(H10J)=FVAR(2)
6.a Ternary CH refined with riding coordinates:
 C52(H52), C63(H63), C64(H64), C65(H65), C66(H66), C70(H70), C71(H71),
 C72(H72), C73(H73), C75(H75), C76(H76), C77(H77), C78(H78), C79(H79), C80(H80),
  C81(H81), C84(H84), C85(H85), C86(H86), C87(H87), C91(H91), C92(H92),
 C93(H93), C94(H94), C95(H95), C96(H96), C97(H97)
6.b Secondary CH2 refined with riding coordinates:
 C37(H37A,H37B), C44(H44A,H44B), C59(H59A,H59B), C60(H60A,H60B), C74(H74A,
 H74B), C100(H10A,H10B)
6.c Aromatic/amide H refined with riding coordinates:
 C6(H6), C7(H7), C12(H12), C13(H13), C15(H15), C16(H16), C17(H17), C18(H18),
 C19(H19), C21(H21), C23(H23), C24(H24), C26(H26), C27(H27), C28(H28), C31(H31),
  C32(H32), C34(H34), C35(H35), C36(H36), C39(H39), C40(H40), C42(H42),
 C43(H43), C45(H45), C46(H46), C48(H48), C49(H49), C51(H51), C53(H53), C55(H55),
  C56(H56), C58(H58), C62(H62), C67(H67), C69(H69), C82(H82), C88(H88),
 C89(H89), C98(H98), C99(H99), C103(H103), C103(H10G), C104(H104), C104(H10H)
6.d Fitted pentagon refined as free rotating group:
 C5(N3,C6,C7,N4), N8(C18,C19,N7,C20), C30(N1,C31,C32,N2), C33(N5,C34,C35,N6),
 C67(N11,C68,N12,C69), C88(C89,N9,C90,N10)
6.e Fitted hexagon refined as free rotating group:
 N16(C1,N15,C2,N17,C3), C11(C12,C13,C14,C15,C16), C22(C23,C24,C25,C26,C27),
 C38(C39,C40,C41,C42,C43), C46(C47,C48,C49,C50,C51), C53(C54,C55,C56,C57,C58)
6.f X=CH2 refined with riding coordinates:
 C61(H61A,H61B), C83(H83A,H83B), C101(H10C,H10D), C102(H10E,H10F), C105(H10I,
 H10J), C106(H10K,H10L), C107(H10M,H10N), C108(H10O,H10P)
;
