#------------------------------------------------------------------------------
#$Date: 2019-11-26 05:33:46 +0200 (Tue, 26 Nov 2019) $
#$Revision: 242724 $
#$URL: file:///home/coder/svn-repositories/cod/cif/4/13/28/4132826.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_4132826
loop_
_publ_author_name
'Zhang, Yuanyuan'
'Zhang, Xuan'
'Lyu, Jiafei'
'Otake, Ken-Ichi'
'Wang, Xingjie'
'Redfern, Louis R.'
'Malliakas, Christos D.'
'Li, Zhanyong'
'Islamoglu, Timur'
'Wang, Bo'
'Farha, Omar K.'
_publ_section_title
;
 A Flexible Metal-Organic Framework with 4-Connected Zr₆ Nodes.
;
_journal_issue                   36
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              11179
_journal_page_last               11183
_journal_paper_doi               10.1021/jacs.8b06789
_journal_volume                  140
_journal_year                    2018
_chemical_formula_moiety         '0.13(C104 H40 O128 Zr24)'
_chemical_formula_sum            'C13 H5 O16 Zr3'
_chemical_formula_weight         690.83
_space_group_crystal_system      orthorhombic
_space_group_IT_number           74
_space_group_name_Hall           '-I 2b 2'
_space_group_name_H-M_alt        'I m m a'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_audit_creation_date             2018-05-29
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.18 svn.r3508 for OlexSys, GUI svn.r5497)
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   25.347(2)
_cell_length_b                   28.534(4)
_cell_length_c                   13.8822(15)
_cell_measurement_reflns_used    1984
_cell_measurement_temperature    250
_cell_measurement_theta_max      22.72
_cell_measurement_theta_min      2.15
_cell_volume                     10040.3(19)
_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 (Sheldrick, 2015)'
_diffrn_ambient_temperature      249.98
_diffrn_detector                 'Bruker APEX2 area detector'
_diffrn_detector_area_resol_mean 7.9
_diffrn_detector_type            'CCD area detector'
_diffrn_measured_fraction_theta_full 0.841
_diffrn_measured_fraction_theta_max 0.923
_diffrn_measurement_device       'three-circle diffractometer'
_diffrn_measurement_device_type  'Bruker SMART APEX2 area detector'
_diffrn_measurement_method       'ω and φ scans'
_diffrn_radiation_monochromator  'mirror optics'
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.1200
_diffrn_reflns_av_unetI/netI     0.1121
_diffrn_reflns_Laue_measured_fraction_full 0.841
_diffrn_reflns_Laue_measured_fraction_max 0.923
_diffrn_reflns_limit_h_max       29
_diffrn_reflns_limit_h_min       -29
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -32
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_number            18396
_diffrn_reflns_point_group_measured_fraction_full 0.841
_diffrn_reflns_point_group_measured_fraction_max 0.923
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         24.401
_diffrn_reflns_theta_min         1.607
_diffrn_source                   'microfocus sealed X-ray tube'
_diffrn_source_type              'Incoatec I\ms'
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.644
_exptl_absorpt_correction_T_max  0.7451
_exptl_absorpt_correction_T_min  0.4990
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
'SADABS-2016/2 (Bruker,2016/2) was used for absorption correction. wR2(int) was 0.1028 before and 0.0664 after correction. The Ratio of minimum to maximum transmission is 0.6697. The λ/2 correction factor is Not present.'
_exptl_crystal_colour            colourless
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    0.914
_exptl_crystal_description       block
_exptl_crystal_F_000             2648
_exptl_crystal_size_max          0.05
_exptl_crystal_size_mid          0.04
_exptl_crystal_size_min          0.03
_refine_diff_density_max         2.075
_refine_diff_density_min         -1.223
_refine_diff_density_rms         0.164
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.177
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     154
_refine_ls_number_reflns         4010
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.177
_refine_ls_R_factor_all          0.2331
_refine_ls_R_factor_gt           0.1297
_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)+(0.2000P)²] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.3353
_refine_ls_wR_factor_ref         0.4277
_reflns_Friedel_coverage         0.000
_reflns_number_gt                1435
_reflns_number_total             4010
_reflns_threshold_expression     'I > 2σ(I)'
_cod_data_source_file            ja8b06789_si_005.cif
_cod_data_source_block           xz21ayz_0ma_a
_cod_database_code               4132826
_shelxl_version_number           2014/6
_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   0.981
_shelx_estimated_absorpt_t_min   0.969
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
2.a Aromatic/amide H refined with riding coordinates:
 C4(H4), C5(H5), C8(H8)
;
_olex2_submission_special_instructions 'No special instructions were received'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, -y+1/2, z'
'-x, y+1/2, -z'
'x, -y, -z'
'x+1/2, y+1/2, z+1/2'
'-x+1/2, -y+1, z+1/2'
'-x+1/2, y+1, -z+1/2'
'x+1/2, -y+1/2, -z+1/2'
'-x, -y, -z'
'x, y-1/2, -z'
'x, -y-1/2, z'
'-x, y, z'
'-x+1/2, -y+1/2, -z+1/2'
'x+1/2, y, -z+1/2'
'x+1/2, -y, z+1/2'
'-x+1/2, y+1/2, z+1/2'
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
Zr1 Zr 0.66119(6) 0.7500 0.8198(2) 0.0961(12) Uani 1 2 d S T P
Zr2 Zr 0.72193(5) 0.68838(8) 0.6340(2) 0.1225(12) Uani 1 1 d . . .
O9 O 0.5990(3) 0.7017(4) 0.7569(11) 0.099(5) Uani 1 1 d . . .
O3 O 0.7339(6) 0.7500 0.9022(19) 0.151(9) Uani 1 2 d S T P
O5 O 0.6797(7) 0.7500 0.6628(15) 0.126(8) Uani 1 2 d S T P
O4 O 0.7074(4) 0.6916(5) 0.7773(15) 0.150(7) Uani 1 1 d . . .
O6 O 0.7224(5) 0.6097(7) 0.6519(16) 0.198(9) Uani 1 1 d . . .
O8 O 0.6390(4) 0.6658(6) 0.6400(15) 0.185(9) Uani 1 1 d . . .
C2 C 0.5982(6) 0.6766(7) 0.684(2) 0.130(10) Uani 1 1 d . . .
O1 O 0.6398(5) 0.7989(6) 0.9280(15) 0.151(7) Uani 1 1 d . . .
O2 O 0.7171(6) 0.8388(9) 0.9718(14) 0.206(10) Uani 1 1 d . . .
C4 C 0.5000 0.6757(9) 0.7058(19) 0.094(10) Uani 1 2 d S T P
H4 H 0.5000 0.7016 0.7476 0.113 Uiso 1 2 calc RS T P
C5 C 0.5472(7) 0.6111(10) 0.625(2) 0.194(15) Uani 1 1 d . . .
H5 H 0.5791 0.5964 0.6082 0.233 Uiso 1 1 calc R . .
C3 C 0.5478(5) 0.6539(14) 0.671(3) 0.26(2) Uani 1 1 d . . .
O7 O 0.6882(5) 0.7017(9) 0.4867(17) 0.263(14) Uani 1 1 d . . .
C6 C 0.5000 0.5897(17) 0.603(5) 0.27(3) Uani 1 2 d S T P
C7 C 0.5000 0.5449(12) 0.560(4) 0.174(18) Uani 1 2 d S T P
C1 C 0.6650(9) 0.8257(16) 0.9836(19) 0.22(2) Uani 1 1 d . . .
C8 C 0.4615(7) 0.5273(15) 0.495(6) 0.50(5) Uani 1 1 d . . .
H8 H 0.4402 0.5451 0.4529 0.600 Uiso 1 1 calc R . .
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Zr Zr -2.9673 0.5597 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
Zr2 Zr1 Zr2 60.24(8) 13_666 7_646
Zr2 Zr1 Zr2 60.68(10) . 11_575
Zr2 Zr1 Zr2 60.54(9) 11_575 13_666
Zr2 Zr1 Zr2 90.87(7) . 13_666
Zr2 Zr1 Zr2 60.54(9) . 7_646
Zr2 Zr1 Zr2 90.87(7) 11_575 7_646
O9 Zr1 Zr2 109.2(4) . 11_575
O9 Zr1 Zr2 73.5(3) 11_575 11_575
O9 Zr1 Zr2 110.7(3) . 7_646
O9 Zr1 Zr2 73.5(3) . .
O9 Zr1 Zr2 110.7(3) 11_575 13_666
O9 Zr1 Zr2 109.2(4) 11_575 .
O9 Zr1 Zr2 164.3(3) 11_575 7_646
O9 Zr1 Zr2 164.3(3) . 13_666
O9 Zr1 O9 74.8(6) 11_575 .
O3 Zr1 Zr2 90.9(6) . .
O3 Zr1 Zr2 35.4(3) . 13_666
O3 Zr1 Zr2 35.4(3) . 7_646
O3 Zr1 Zr2 90.9(6) . 11_575
O3 Zr1 O9 142.5(3) . 11_575
O3 Zr1 O9 142.5(3) . .
O3 Zr1 O5 109.7(8) . .
O5 Zr1 Zr2 35.2(2) . .
O5 Zr1 Zr2 90.0(4) . 13_666
O5 Zr1 Zr2 35.2(2) . 11_575
O5 Zr1 Zr2 90.0(4) . 7_646
O5 Zr1 O9 76.7(5) . 11_575
O5 Zr1 O9 76.7(5) . .
O4 Zr1 Zr2 32.0(5) 11_575 11_575
O4 Zr1 Zr2 32.0(5) . .
O4 Zr1 Zr2 86.9(5) . 11_575
O4 Zr1 Zr2 35.9(5) . 7_646
O4 Zr1 Zr2 86.9(5) 11_575 .
O4 Zr1 Zr2 88.8(4) 11_575 7_646
O4 Zr1 Zr2 88.8(4) . 13_666
O4 Zr1 Zr2 35.9(5) 11_575 13_666
O4 Zr1 O9 138.9(6) . 11_575
O4 Zr1 O9 78.4(5) 11_575 11_575
O4 Zr1 O9 138.9(6) 11_575 .
O4 Zr1 O9 78.4(5) . .
O4 Zr1 O3 71.2(6) . .
O4 Zr1 O3 71.2(6) 11_575 .
O4 Zr1 O5 67.1(6) . .
O4 Zr1 O5 67.1(6) 11_575 .
O4 Zr1 O4 103.6(8) . 11_575
O4 Zr1 O1 79.7(7) 11_575 .
O4 Zr1 O1 148.8(7) . .
O4 Zr1 O1 148.8(7) 11_575 11_575
O4 Zr1 O1 79.7(7) . 11_575
O1 Zr1 Zr2 107.8(5) . 11_575
O1 Zr1 Zr2 166.0(4) . .
O1 Zr1 Zr2 166.0(4) 11_575 11_575
O1 Zr1 Zr2 75.9(4) . 13_666
O1 Zr1 Zr2 114.7(4) 11_575 13_666
O1 Zr1 Zr2 107.8(5) 11_575 .
O1 Zr1 Zr2 75.9(4) 11_575 7_646
O1 Zr1 Zr2 114.7(4) . 7_646
O1 Zr1 O9 72.3(6) 11_575 .
O1 Zr1 O9 72.3(6) . 11_575
O1 Zr1 O9 119.6(5) 11_575 11_575
O1 Zr1 O9 119.6(5) . .
O1 Zr1 O3 81.0(6) . .
O1 Zr1 O3 81.0(6) 11_575 .
O1 Zr1 O5 138.3(5) 11_575 .
O1 Zr1 O5 138.3(5) . .
O1 Zr1 O1 82.3(11) 11_575 .
Zr1 Zr2 Zr1 89.13(7) . 13_666
Zr1 Zr2 Zr2 59.66(5) . 11_575
Zr1 Zr2 Zr2 59.41(6) 13_666 7_646
Zr1 Zr2 Zr2 60.06(8) . 7_646
Zr1 Zr2 Zr2 59.88(4) 13_666 11_575
Zr2 Zr2 Zr2 90.0 11_575 7_646
O3 Zr2 Zr1 89.5(6) 13_666 .
O3 Zr2 Zr1 35.9(5) 13_666 13_666
O3 Zr2 Zr2 34.9(4) 13_666 11_575
O3 Zr2 Zr2 90.2(7) 13_666 7_646
O3 Zr2 O4 70.6(7) 13_666 7_646
O3 Zr2 O6 146.9(5) 13_666 .
O3 Zr2 O8 138.4(6) 13_666 .
O3 Zr2 O2 76.9(7) 13_666 13_666
O3 Zr2 O7 81.2(9) 13_666 .
O5 Zr2 Zr1 37.8(6) . .
O5 Zr2 Zr1 88.6(4) . 13_666
O5 Zr2 Zr2 91.8(6) . 7_646
O5 Zr2 Zr2 33.0(4) . 11_575
O5 Zr2 O3 67.9(6) . 13_666
O5 Zr2 O4 106.1(7) . 7_646
O5 Zr2 O6 144.7(5) . .
O5 Zr2 O8 75.6(6) . .
O5 Zr2 O2 139.3(9) . 13_666
O5 Zr2 O7 80.6(8) . .
O4 Zr2 Zr1 33.7(3) . .
O4 Zr2 Zr1 87.2(4) . 13_666
O4 Zr2 Zr1 85.6(5) 7_646 .
O4 Zr2 Zr1 34.8(4) 7_646 13_666
O4 Zr2 Zr2 34.4(3) . 7_646
O4 Zr2 Zr2 31.8(5) 7_646 7_646
O4 Zr2 Zr2 87.4(4) . 11_575
O4 Zr2 Zr2 87.6(4) 7_646 11_575
O4 Zr2 O3 106.7(8) . 13_666
O4 Zr2 O5 71.4(6) . .
O4 Zr2 O4 65.9(6) . 7_646
O4 Zr2 O6 88.6(6) 7_646 .
O4 Zr2 O6 86.5(7) . .
O4 Zr2 O8 78.6(6) . .
O4 Zr2 O8 141.0(8) 7_646 .
O4 Zr2 O2 79.6(7) 7_646 13_666
O4 Zr2 O2 140.9(7) . 13_666
O4 Zr2 O7 145.1(7) 7_646 .
O4 Zr2 O7 144.7(5) . .
O6 Zr2 Zr1 118.3(4) . 13_666
O6 Zr2 Zr1 115.0(5) . .
O6 Zr2 Zr2 84.1(5) . 7_646
O6 Zr2 Zr2 173.7(6) . 11_575
O6 Zr2 O2 74.2(8) . 13_666
O8 Zr2 Zr1 72.4(5) . .
O8 Zr2 Zr1 161.4(5) . 13_666
O8 Zr2 Zr2 107.0(5) . 11_575
O8 Zr2 Zr2 110.6(6) . 7_646
O8 Zr2 O6 73.2(6) . .
O8 Zr2 O2 125.1(7) . 13_666
O8 Zr2 O7 73.8(7) . .
O2 Zr2 Zr1 73.4(5) 13_666 13_666
O2 Zr2 Zr1 162.5(5) 13_666 .
O2 Zr2 Zr2 110.0(7) 13_666 11_575
O2 Zr2 Zr2 108.5(5) 13_666 7_646
O7 Zr2 Zr1 114.8(5) . .
O7 Zr2 Zr1 113.7(5) . 13_666
O7 Zr2 Zr2 80.2(6) . 11_575
O7 Zr2 Zr2 170.2(6) . 7_646
O7 Zr2 O6 105.7(8) . .
O7 Zr2 O2 74.2(7) . 13_666
C2 O9 Zr1 132.5(11) . .
Zr2 O3 Zr1 108.7(8) 13_666 .
Zr2 O3 Zr1 108.7(8) 7_646 .
Zr2 O3 Zr2 110.2(8) 13_666 7_646
Zr2 O5 Zr1 107.1(7) . .
Zr2 O5 Zr1 107.1(7) 11_575 .
Zr2 O5 Zr2 114.0(8) . 11_575
Zr1 O4 Zr2 109.3(8) . 7_646
Zr2 O4 Zr1 114.2(7) . .
Zr2 O4 Zr2 113.8(6) . 7_646
C2 O8 Zr2 138.1(15) . .
O9 C2 C3 112(2) . .
O8 C2 O9 122.0(16) . .
O8 C2 C3 124(2) . .
C1 O1 Zr1 134.6(13) . .
C1 O2 Zr2 129.4(16) . 13_666
C3 C4 H4 123.2 12_655 .
C3 C4 H4 123.2 . .
C3 C4 C3 114(3) 12_655 .
C3 C5 H5 119.9 . .
C6 C5 H5 119.9 . .
C6 C5 C3 120(2) . .
C2 C3 C4 120(2) . .
C5 C3 C2 117.8(17) . .
C5 C3 C4 122(2) . .
C5 C6 C5 121(3) 12_655 .
C5 C6 C7 119.7(17) . .
C5 C6 C7 119.7(17) 12_655 .
C6 C7 C8 126(3) . .
C6 C7 C8 126(3) . 12_655
C8 C7 C8 87(5) . 12_655
O1 C1 O2 125.2(19) . .
C7 C8 C8 107(7) . 4_566
C7 C8 H8 126.6 . .
C8 C8 H8 126.6 4_566 .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
Zr1 Zr2 3.481(3) .
Zr1 Zr2 3.481(3) 11_575
Zr1 Zr2 3.504(2) 13_666
Zr1 Zr2 3.504(2) 7_646
Zr1 O9 2.269(12) .
Zr1 O9 2.269(12) 11_575
Zr1 O3 2.168(19) .
Zr1 O5 2.23(2) .
Zr1 O4 2.120(13) 11_575
Zr1 O4 2.120(13) .
Zr1 O1 2.121(19) 11_575
Zr1 O1 2.121(19) .
Zr2 Zr1 3.504(2) 13_666
Zr2 Zr2 3.521(6) 7_646
Zr2 Zr2 3.517(5) 11_575
Zr2 O3 2.144(10) 13_666
Zr2 O5 2.096(9) .
Zr2 O4 2.03(2) .
Zr2 O4 2.176(14) 7_646
Zr2 O6 2.258(19) .
Zr2 O8 2.201(11) .
Zr2 O2 2.268(16) 13_666
Zr2 O7 2.25(2) .
O9 C2 1.24(2) .
O3 Zr2 2.144(10) 13_666
O3 Zr2 2.144(10) 7_646
O5 Zr2 2.096(9) 11_575
O4 Zr2 2.176(14) 7_646
O8 C2 1.24(2) .
C2 C3 1.45(3) .
O1 C1 1.26(3) .
O2 Zr2 2.268(16) 13_666
O2 C1 1.38(3) .
C4 H4 0.9400 .
C4 C3 1.45(2) .
C4 C3 1.45(2) 12_655
C5 H5 0.9400 .
C5 C3 1.38(3) .
C5 C6 1.38(3) .
C6 C5 1.38(3) 12_655
C6 C7 1.41(4) .
C7 C8 1.42(6) 12_655
C7 C8 1.42(6) .
C8 C8 1.57(9) 4_566
C8 H8 0.9400 .
loop_
_smtbx_masks_void_nr
_smtbx_masks_void_average_x
_smtbx_masks_void_average_y
_smtbx_masks_void_average_z
_smtbx_masks_void_volume
_smtbx_masks_void_count_electrons
1 -0.956 -0.311 -0.897 6907.0 742.5
