#------------------------------------------------------------------------------
#$Date: 2019-11-26 05:33:10 +0200 (Tue, 26 Nov 2019) $
#$Revision: 242722 $
#$URL: file:///home/coder/svn-repositories/cod/cif/4/13/28/4132824.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_4132824
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(C88 H40 O128 Zr24)'
_chemical_formula_sum            'C11 H5 O16 Zr3'
_chemical_formula_weight         666.81
_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             2018-08-09
_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                90
_cell_formula_units_Z            8
_cell_length_a                   25.385(3)
_cell_length_b                   30.661(3)
_cell_length_c                   8.2771(9)
_cell_measurement_reflns_used    2449
_cell_measurement_temperature    200
_cell_measurement_theta_max      26.26
_cell_measurement_theta_min      2.55
_cell_volume                     6442.3(12)
_computing_cell_refinement       'SAINT v8.34A (Bruker, 2013)'
_computing_data_reduction        'SAINT v8.34A (Bruker, 2013)'
_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      200
_diffrn_detector                 'Bruker APEX2 area detector'
_diffrn_detector_area_resol_mean 7.9
_diffrn_detector_type            'CCD area detector'
_diffrn_measured_fraction_theta_full 0.911
_diffrn_measured_fraction_theta_max 0.996
_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  0.0769
_diffrn_reflns_av_unetI/netI     0.0812
_diffrn_reflns_Laue_measured_fraction_full 0.911
_diffrn_reflns_Laue_measured_fraction_max 0.996
_diffrn_reflns_limit_h_max       26
_diffrn_reflns_limit_h_min       -29
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       -35
_diffrn_reflns_limit_l_max       7
_diffrn_reflns_limit_l_min       -9
_diffrn_reflns_number            11037
_diffrn_reflns_point_group_measured_fraction_full 0.911
_diffrn_reflns_point_group_measured_fraction_max 0.996
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         24.404
_diffrn_reflns_theta_min         2.083
_diffrn_source                   'microfocus sealed X-ray tube'
_diffrn_source_type              'Incoatec I\ms'
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    1.001
_exptl_absorpt_correction_T_max  0.7454
_exptl_absorpt_correction_T_min  0.5770
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
'SADABS-2012/1 (Bruker,2012) was used for absorption correction. wR2(int) was 0.0816 before and 0.0589 after correction. The Ratio of minimum to maximum transmission is 0.7741. The λ/2 correction factor is 0.0015.'
_exptl_crystal_colour            colourless
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.375
_exptl_crystal_description       block
_exptl_crystal_F_000             2552
_exptl_crystal_size_max          0.03
_exptl_crystal_size_mid          0.02
_exptl_crystal_size_min          0.02
_refine_diff_density_max         1.938
_refine_diff_density_min         -1.319
_refine_diff_density_rms         0.183
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.037
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     148
_refine_ls_number_reflns         2783
_refine_ls_number_restraints     36
_refine_ls_restrained_S_all      1.035
_refine_ls_R_factor_all          0.1164
_refine_ls_R_factor_gt           0.0882
_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)+(0.1317P)²+70.2411P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2212
_refine_ls_wR_factor_ref         0.2390
_reflns_Friedel_coverage         0.000
_reflns_number_gt                1856
_reflns_number_total             2783
_reflns_threshold_expression     'I > 2σ(I)'
_cod_data_source_file            ja8b06789_si_008.cif
_cod_data_source_block           imma_a
_cod_original_cell_volume        6442.4(12)
_cod_database_code               4132824
_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   0.980
_shelx_estimated_absorpt_t_min   0.971
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
2. Uiso/Uaniso restraints and constraints
Uanis(C7) \\sim Ueq, Uanis(C7A) \\sim Ueq: with sigma of 0.1 and sigma for
terminal atoms of 0.2
Uanis(O3) \\sim Ueq: with sigma of 0.1 and sigma for terminal atoms of 0.2
Uanis(O5) \\sim Ueq, Uanis(O6) \\sim Ueq: with sigma of 0.1 and sigma for
terminal atoms of 0.2
Uanis(C4) \\sim Ueq: with sigma of 0.1 and sigma for terminal atoms of 0.2
Uanis(C7A) = Uanis(C7)
3. Others
 Fixed Sof: C7(0.5) H7(0.5) C7A(0.5) H7A(0.5)
4.a Aromatic/amide H refined with riding coordinates:
 C7(H7), C2(H2), C4(H4), C7A(H7A)
;
_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
Zr2 Zr 0.33619(4) 0.2500 0.60968(15) 0.0307(4) Uani 1 2 d S T P
O5 O 0.2648(6) 0.1627(9) 0.374(2) 0.252(13) Uani 1 1 d . U .
O2 O 0.2079(3) 0.1935(3) 0.8212(11) 0.072(3) Uani 1 1 d . . .
Zr1 Zr 0.21658(4) 0.19283(5) 0.56699(16) 0.0599(5) Uani 1 1 d . . .
C5 C 0.5000 0.4088(6) 0.913(4) 0.121(12) Uani 1 2 d S T P
O8 O 0.4001(2) 0.2928(2) 0.6965(10) 0.0431(19) Uani 1 1 d . . .
O7 O 0.3589(5) 0.2096(6) 0.4050(13) 0.174(8) Uani 1 1 d . . .
O9 O 0.3647(3) 0.3327(3) 0.8951(13) 0.086(3) Uani 1 1 d . . .
O6 O 0.2616(4) 0.2500 0.496(2) 0.105(5) Uani 1 2 d S TU P
C7 C 0.5413(11) 0.4722(10) 1.048(6) 0.110(13) Uani 0.5 1 d . U .
H7 H 0.5719 0.4555 1.0711 0.132 Uiso 0.5 1 calc R . .
C1 C 0.4026(4) 0.3215(4) 0.8021(19) 0.061(4) Uani 1 1 d . . .
O1 O 0.1764(6) 0.2500 0.6293(14) 0.074(4) Uani 1 2 d S T P
C3 C 0.4530(4) 0.3451(4) 0.825(2) 0.078(5) Uani 1 1 d . . .
O3 O 0.2251(4) 0.1210(4) 0.618(3) 0.241(13) Uani 1 1 d . U .
C2 C 0.5000 0.3243(5) 0.795(3) 0.065(6) Uani 1 2 d S T P
H2 H 0.5000 0.2954 0.7535 0.078 Uiso 1 2 calc RS T P
O4 O 0.1769(4) 0.2011(6) 0.3332(14) 0.143(6) Uani 1 1 d . . .
C4 C 0.4532(4) 0.3870(4) 0.885(2) 0.112(7) Uani 1 1 d . U .
H4 H 0.4207 0.4010 0.9085 0.134 Uiso 1 1 calc R . .
C6 C 0.5000 0.4541(6) 0.965(4) 0.100(9) Uani 1 2 d S T P
C7A C 0.5377(11) 0.4830(10) 0.900(6) 0.110(13) Uani 0.5 1 d . U .
H7A H 0.5612 0.4726 0.8190 0.132 Uiso 0.5 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
O2 Zr2 O2 108.1(5) 7_546 13_556
O2 Zr2 Zr1 34.3(2) 13_556 11_565
O2 Zr2 Zr1 35.2(2) 7_546 7_546
O2 Zr2 Zr1 90.1(3) 13_556 7_546
O2 Zr2 Zr1 88.8(2) 13_556 .
O2 Zr2 Zr1 34.3(2) 7_546 .
O2 Zr2 Zr1 88.8(2) 7_546 11_565
O2 Zr2 Zr1 90.1(3) 7_546 13_556
O2 Zr2 Zr1 35.2(2) 13_556 13_556
O2 Zr2 O8 79.4(3) 7_546 11_565
O2 Zr2 O8 79.4(3) 13_556 .
O2 Zr2 O8 141.1(3) 7_546 .
O2 Zr2 O8 141.1(3) 13_556 11_565
O2 Zr2 O7 143.8(5) 7_546 11_565
O2 Zr2 O7 143.8(5) 13_556 .
O2 Zr2 O7 83.4(6) 7_546 .
O2 Zr2 O7 83.4(6) 13_556 11_565
O2 Zr2 O1 70.1(3) 13_556 13_556
O2 Zr2 O1 70.1(3) 7_546 13_556
Zr1 Zr2 Zr1 89.77(4) 7_546 11_565
Zr1 Zr2 Zr1 59.66(5) 11_565 .
Zr1 Zr2 Zr1 89.77(4) 13_556 .
Zr1 Zr2 Zr1 60.71(5) 13_556 7_546
Zr1 Zr2 Zr1 59.55(4) 7_546 .
Zr1 Zr2 Zr1 59.55(4) 13_556 11_565
O8 Zr2 Zr1 164.13(19) 11_565 11_565
O8 Zr2 Zr1 164.13(19) . .
O8 Zr2 Zr1 74.47(18) . 13_556
O8 Zr2 Zr1 74.46(18) 11_565 7_546
O8 Zr2 Zr1 109.4(2) . 7_546
O8 Zr2 Zr1 111.75(17) 11_565 .
O8 Zr2 Zr1 109.4(2) 11_565 13_556
O8 Zr2 Zr1 111.75(17) . 11_565
O8 Zr2 O8 72.9(4) . 11_565
O7 Zr2 Zr1 114.5(5) 11_565 13_556
O7 Zr2 Zr1 114.5(5) . 7_546
O7 Zr2 Zr1 82.4(4) . .
O7 Zr2 Zr1 115.7(4) . 11_565
O7 Zr2 Zr1 172.1(4) 11_565 7_546
O7 Zr2 Zr1 115.7(4) 11_565 .
O7 Zr2 Zr1 82.4(4) 11_565 11_565
O7 Zr2 Zr1 172.1(4) . 13_556
O7 Zr2 O8 113.4(4) . .
O7 Zr2 O8 73.8(5) 11_565 .
O7 Zr2 O8 73.8(5) . 11_565
O7 Zr2 O8 113.4(4) 11_565 11_565
O7 Zr2 O7 69.4(10) 11_565 .
O7 Zr2 O1 143.9(5) 11_565 13_556
O7 Zr2 O1 143.9(5) . 13_556
O6 Zr2 O2 69.6(3) . 7_546
O6 Zr2 O2 69.6(3) . 13_556
O6 Zr2 Zr1 89.9(4) . 7_546
O6 Zr2 Zr1 35.3(2) . .
O6 Zr2 Zr1 35.3(2) . 11_565
O6 Zr2 Zr1 89.9(4) . 13_556
O6 Zr2 O8 143.45(18) . 11_565
O6 Zr2 O8 143.45(18) . .
O6 Zr2 O7 83.7(5) . .
O6 Zr2 O7 83.7(5) . 11_565
O6 Zr2 O1 108.1(6) . 13_556
O1 Zr2 Zr1 88.5(3) 13_556 11_565
O1 Zr2 Zr1 34.94(19) 13_556 7_546
O1 Zr2 Zr1 88.5(3) 13_556 .
O1 Zr2 Zr1 34.94(19) 13_556 13_556
O1 Zr2 O8 77.6(4) 13_556 11_565
O1 Zr2 O8 77.6(4) 13_556 .
Zr1 O2 Zr2 111.2(4) 7_546 13_556
Zr1 O2 Zr2 109.1(4) . 13_556
Zr1 O2 Zr1 109.8(4) . 7_546
Zr2 Zr1 Zr2 90.23(4) 13_556 .
Zr2 Zr1 Zr1 59.64(3) 13_556 11_565
Zr2 Zr1 Zr1 61.02(4) 13_556 7_546
O5 Zr1 Zr2 78.7(5) . .
O5 Zr1 Zr2 168.8(5) . 13_556
O5 Zr1 Zr1 114.7(8) . 11_565
O5 Zr1 Zr1 111.0(4) . 7_546
O5 Zr1 O9 117.8(6) . 13_556
O5 Zr1 O3 71.0(9) . .
O2 Zr1 Zr2 89.1(2) . .
O2 Zr1 Zr2 90.4(3) 7_546 13_556
O2 Zr1 Zr2 34.5(2) 7_546 .
O2 Zr1 Zr2 35.7(2) . 13_556
O2 Zr1 O5 141.1(7) . .
O2 Zr1 O5 79.6(5) 7_546 .
O2 Zr1 O2 70.2(4) . 7_546
O2 Zr1 Zr1 35.2(2) . 7_546
O2 Zr1 Zr1 89.5(3) . 11_565
O2 Zr1 Zr1 89.5(3) 7_546 11_565
O2 Zr1 Zr1 35.0(2) 7_546 7_546
O2 Zr1 O9 76.5(3) . 13_556
O2 Zr1 O9 140.9(4) 7_546 13_556
O2 Zr1 O6 68.8(4) 7_546 .
O2 Zr1 O6 108.5(5) . .
O2 Zr1 O3 80.8(4) 7_546 .
O2 Zr1 O3 80.4(6) . .
O2 Zr1 O4 142.7(4) 7_546 .
O2 Zr1 O4 145.9(4) . .
Zr1 Zr1 Zr2 59.43(3) 7_546 .
Zr1 Zr1 Zr2 60.17(2) 11_565 .
Zr1 Zr1 Zr1 90.0 7_546 11_565
O9 Zr1 Zr2 163.4(2) 13_556 .
O9 Zr1 Zr2 73.2(2) 13_556 13_556
O9 Zr1 Zr1 109.3(3) 13_556 7_546
O9 Zr1 Zr1 110.5(2) 13_556 11_565
O9 Zr1 O3 73.7(4) 13_556 .
O6 Zr1 Zr2 90.3(4) . 13_556
O6 Zr1 Zr2 34.2(3) . .
O6 Zr1 O5 81.4(8) . .
O6 Zr1 Zr1 88.9(4) . 7_546
O6 Zr1 Zr1 36.3(3) . 11_565
O6 Zr1 O9 143.9(4) . 13_556
O6 Zr1 O3 142.0(4) . .
O6 Zr1 O4 84.8(6) . .
O1 Zr1 Zr2 36.7(3) . 13_556
O1 Zr1 Zr2 88.8(4) . .
O1 Zr1 O5 142.9(8) . .
O1 Zr1 O2 72.3(4) . .
O1 Zr1 O2 108.9(5) . 7_546
O1 Zr1 Zr1 91.3(4) . 7_546
O1 Zr1 Zr1 33.1(3) . 11_565
O1 Zr1 O9 78.9(4) . 13_556
O1 Zr1 O6 69.4(4) . .
O1 Zr1 O3 145.0(5) . .
O1 Zr1 O4 84.1(6) . .
O3 Zr1 Zr2 112.6(3) . .
O3 Zr1 Zr2 112.7(5) . 13_556
O3 Zr1 Zr1 167.8(5) . 11_565
O3 Zr1 Zr1 77.8(5) . 7_546
O4 Zr1 Zr2 115.2(4) . .
O4 Zr1 Zr2 116.4(3) . 13_556
O4 Zr1 O5 70.5(6) . .
O4 Zr1 Zr1 83.4(4) . 11_565
O4 Zr1 Zr1 173.2(4) . 7_546
O4 Zr1 O9 74.9(5) . 13_556
O4 Zr1 O3 108.8(7) . .
C4 C5 C4 118.6(16) . 12_655
C4 C5 C6 120.7(8) . .
C4 C5 C6 120.7(8) 12_655 .
C1 O8 Zr2 133.5(6) . .
C1 O9 Zr1 133.4(7) . 13_556
Zr2 O6 Zr1 110.4(5) . 11_565
Zr2 O6 Zr1 110.4(5) . .
Zr1 O6 Zr1 107.4(6) 11_565 .
C6 C7 C7A 119(3) . 4_567
O8 C1 O9 125.1(10) . .
O8 C1 C3 118.6(11) . .
O9 C1 C3 116.3(11) . .
Zr1 O1 Zr2 108.4(4) 11_565 13_556
Zr1 O1 Zr2 108.4(4) . 13_556
Zr1 O1 Zr1 113.7(5) 11_565 .
C2 C3 C1 120.1(11) . .
C2 C3 C4 119.6(10) . .
C4 C3 C1 120.2(10) . .
C3 C2 C3 120.5(15) . 12_655
C3 C4 C5 120.8(11) . .
C7 C6 C5 122.4(17) . .
C7 C6 C5 122.4(17) 12_655 .
C7 C6 C7 100(3) . 12_655
C7 C6 C7A 55(2) . .
C7 C6 C7A 117.2(19) 12_655 .
C7 C6 C7A 117.3(19) . 12_655
C7 C6 C7A 55(2) 12_655 12_655
C7A C6 C5 119(2) . .
C7A C6 C5 119(2) 12_655 .
C7A C6 C7A 85(3) . 12_655
C6 C7A C7 122(4) . 4_567
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
Zr2 O2 2.142(8) 7_546
Zr2 O2 2.142(8) 13_556
Zr2 Zr1 3.5237(14) .
Zr2 Zr1 3.4682(15) 7_546
Zr2 Zr1 3.5236(14) 11_565
Zr2 Zr1 3.4682(15) 13_556
Zr2 O8 2.206(7) .
Zr2 O8 2.206(7) 11_565
Zr2 O7 2.178(11) 11_565
Zr2 O7 2.178(11) .
Zr2 O6 2.116(12) .
Zr2 O1 2.183(11) 13_556
O5 Zr1 2.215(12) .
O2 Zr2 2.142(8) 13_556
O2 Zr1 2.116(9) .
O2 Zr1 2.128(8) 7_546
Zr1 Zr2 3.4682(15) 13_556
Zr1 O2 2.128(8) 7_546
Zr1 Zr1 3.506(3) 11_565
Zr1 Zr1 3.472(2) 7_546
Zr1 O9 2.228(8) 13_556
Zr1 O6 2.175(8) .
Zr1 O1 2.093(6) .
Zr1 O3 2.251(16) .
Zr1 O4 2.196(11) .
C5 C4 1.382(14) 12_655
C5 C4 1.382(14) .
C5 C6 1.46(2) .
O8 C1 1.243(14) .
O9 Zr1 2.228(8) 13_556
O9 C1 1.279(14) .
O6 Zr1 2.175(8) 11_565
C7 C6 1.37(3) .
C7 C7A 1.44(3) 4_567
C1 C3 1.482(15) .
O1 Zr2 2.183(11) 13_556
O1 Zr1 2.093(6) 11_565
C3 C2 1.374(13) .
C3 C4 1.379(16) .
C2 C3 1.374(13) 12_655
C6 C7 1.37(3) 12_655
C6 C7A 1.41(4) .
C6 C7A 1.41(4) 12_655
C7A C7 1.44(3) 4_567
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 -0.743 -0.246 -0.036 3436.0 489.3
