#------------------------------------------------------------------------------
#$Date: 2019-11-03 15:33:54 +0200 (Sun, 03 Nov 2019) $
#$Revision: 221766 $
#$URL: file:///home/coder/svn-repositories/cod/cif/4/12/86/4128685.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_4128685
loop_
_publ_author_name
'Gong, Wei'
'Chen, Xu'
'Jiang, Hong'
'Chu, Dandan'
'Cui, Yong'
'Liu, Yan'
_publ_section_title
;
 Highly Stable Zr(IV)-Based Metal-Organic Frameworks with Chiral
 Phosphoric Acids for Catalytic Asymmetric Tandem Reactions.
;
_journal_issue                   18
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              7498
_journal_page_last               7508
_journal_paper_doi               10.1021/jacs.9b02294
_journal_volume                  141
_journal_year                    2019
_chemical_absolute_configuration rm
_chemical_formula_moiety         '0.17(C810 H468 O360 P18 Zr54)'
_chemical_formula_sum            'C135 H78 O60 P3 Zr9'
_chemical_formula_weight         3573.86
_space_group_crystal_system      hexagonal
_space_group_IT_number           180
_space_group_name_Hall           'P 62 2 (0 0 4)'
_space_group_name_H-M_alt        'P 62 2 2'
_atom_sites_solution_hydrogens   geom
_audit_creation_date             2018-08-02
_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            6
_cell_length_a                   38.1622(9)
_cell_length_b                   38.1622(9)
_cell_length_c                   45.5859(15)
_cell_measurement_reflns_used    9688
_cell_measurement_temperature    173(2)
_cell_measurement_theta_max      43.13
_cell_measurement_theta_min      2.35
_cell_volume                     57495(3)
_computing_cell_refinement       'Bruker SMART'
_computing_data_collection       'Bruker SMART'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'XL (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      173(2)
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54178
_diffrn_reflns_av_R_equivalents  0.1803
_diffrn_reflns_av_unetI/netI     0.1128
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.997
_diffrn_reflns_limit_h_max       34
_diffrn_reflns_limit_h_min       -34
_diffrn_reflns_limit_k_max       32
_diffrn_reflns_limit_k_min       -34
_diffrn_reflns_limit_l_max       40
_diffrn_reflns_limit_l_min       -41
_diffrn_reflns_number            163520
_diffrn_reflns_point_group_measured_fraction_full 0.997
_diffrn_reflns_point_group_measured_fraction_max 0.997
_diffrn_reflns_theta_full        44.727
_diffrn_reflns_theta_max         44.727
_diffrn_reflns_theta_min         2.510
_exptl_absorpt_coefficient_mu    2.346
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    0.619
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             10638
_exptl_crystal_size_max          0.25
_exptl_crystal_size_mid          0.22
_exptl_crystal_size_min          0.18
_refine_diff_density_max         0.791
_refine_diff_density_min         -0.923
_refine_diff_density_rms         0.077
_refine_ls_abs_structure_details
;
 Flack x determined using 3712 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   0.060(10)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.026
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     802
_refine_ls_number_reflns         15251
_refine_ls_number_restraints     2025
_refine_ls_restrained_S_all      0.980
_refine_ls_R_factor_all          0.1096
_refine_ls_R_factor_gt           0.0755
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[σ²(Fo²)+(0.0901P)²+139.4599P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1676
_refine_ls_wR_factor_ref         0.1797
_reflns_Friedel_coverage         0.789
_reflns_Friedel_fraction_full    0.997
_reflns_Friedel_fraction_max     0.997
_reflns_number_gt                11239
_reflns_number_total             15251
_reflns_threshold_expression     'I > 2σ(I)'
_cod_data_source_file            ja9b02294_si_002.cif
_cod_data_source_block           f
_cod_original_sg_symbol_Hall     'P 62 2c (0 0 1)'
_cod_database_code               4128685
_shelx_shelxl_version_number     2014/7
_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   0.678
_shelx_estimated_absorpt_t_min   0.592
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
2. Restrained distances
 C55-O7 = C63-O16
 1.27 with sigma of 0.02
3. Rigid bond restraints
 O1, O2, O3, O4, O5, O6, O7
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
 C16, C17
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
 O22, O23
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
 O23, O22
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
4. Uiso/Uaniso restraints and constraints
O1 \\sim O2 \\sim O3 \\sim O4 \\sim O5 \\sim O6 \\sim O7 \\sim O8 \\sim O9
\\sim O10 \\sim O11 \\sim O12 \\sim O13 \\sim O14 \\sim O15 \\sim O16 \\sim O17
\\sim O18 \\sim O19 \\sim O20 \\sim O21 \\sim O22 \\sim O23 \\sim O24 \\sim O25
\\sim O26 \\sim O27 \\sim O28 \\sim O29 \\sim O30: within 3.8A with sigma of
0.01 and sigma for terminal atoms of 0.02
C1 \\sim C2 \\sim C3 \\sim C4 \\sim C5 \\sim C6 \\sim C7 \\sim C12 \\sim C11
\\sim C10 \\sim C9 \\sim C8 \\sim C13 \\sim C18 \\sim C17 \\sim C16 \\sim C15
\\sim C14 \\sim C19 \\sim C24 \\sim C23 \\sim C22 \\sim C21 \\sim C20 \\sim C25
\\sim C30 \\sim C29 \\sim C28 \\sim C27 \\sim C26 \\sim C31 \\sim C36 \\sim C35
\\sim C34 \\sim C33 \\sim C32 \\sim C37 \\sim C42 \\sim C41 \\sim C40 \\sim C39
\\sim C38 \\sim C43 \\sim C44 \\sim C45 \\sim C46 \\sim C47 \\sim C48 \\sim C49
\\sim C54 \\sim C53 \\sim C52 \\sim C51 \\sim C50 \\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: within 3.8A with sigma of 0.01 and sigma for
terminal atoms of 0.02
C16 \\sim C17: within 2A with sigma of 0.04 and sigma for terminal atoms of 0.08
O1 \\sim O2 \\sim O3 \\sim O4 \\sim O5 \\sim O6 \\sim O7: within 2A with sigma
of 0.04 and sigma for terminal atoms of 0.08
O22 \\sim O23: within 2A with sigma of 0.04 and sigma for terminal atoms of 0.08
O23 \\sim O22: within 2A with sigma of 0.04 and sigma for terminal atoms of 0.08
Uanis(O28) \\sim Ueq: with sigma of 0.001 and sigma for terminal atoms of 0.002
Uanis(O1) = Uanis(O4) = Uanis(O12) = Uanis(O16)
Uanis(O23) = Uanis(O7)
5.a Secondary CH2 refined with riding coordinates:
 C58(H58A,H58B), C59(H59A,H59B), C61(H61A,H61B), C62(H62A,H62B), C66(H66A,
 H66B), C67(H67A,H67B)
5.b Aromatic/amide H refined with riding coordinates:
 C2(H2), C3(H3), C5(H5), C6(H6), C8(H8), C17(H17), C24(H24), C23(H23),
 C21(H21), C20(H20), C30(H30), C29(H29), C27(H27), C26(H26), C36(H36), C35(H35),
  C33(H33), C32(H32), C42(H42), C41(H41), C39(H39), C38(H38), C44(H44),
 C54(H54), C53(H53), C51(H51), C50(H50)
5.c Fitted hexagon refined as free rotating group:
 C1(C2,C3,C4,C5,C6), C7(C12,C11,C10,C9,C8), C13(C18,C17,C16,C15,C14), C19(C24,
 C23,C22,C21,C20), C25(C30,C29,C28,C27,C26), C31(C36,C35,C34,C33,C32), C37(C42,
 C41,C40,C39,C38), C43(C44,C45,C46,C47,C48), C49(C54,C53,C52,C51,C50)
;
