A Flexible Metal-Organic Framework with 4-Connected Zr<sub>6</sub> Nodes.
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.; Journal of the American Chemical Society 140 (2018) 11179–11183; doi:10.1021/jacs.8b06789

data_4132823
_publ_section_title
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 A Flexible Metal-Organic Framework with 4-Connected Zr<sub>6</sub> 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 H24 O128 Zr24), 0.25(Zr7.2)'
_chemical_formula_sum            'C13 H3 O16 Zr4.8'
_chemical_formula_weight         853.01
_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             2018-06-27
_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                90
_cell_formula_units_Z            8
_cell_length_a                   25.1305(9)
_cell_length_b                   26.1041(11)
_cell_length_c                   18.9051(9)
_cell_measurement_reflns_used    6645
_cell_measurement_temperature    200
_cell_measurement_theta_max      22.66
_cell_measurement_theta_min      2.25
_cell_volume                     12401.9(9)
_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      200.0
_diffrn_detector                 'Bruker APEX2 area detector'
_diffrn_detector_area_resol_mean 7.9
_diffrn_detector_type            'CCD area detector'
_diffrn_measured_fraction_theta_full 0.714
_diffrn_measured_fraction_theta_max 0.988
_diffrn_measurement_device       'three-circle diffractometer'
_diffrn_measurement_device_type  'Bruker SMART APEX2 area detector'
_diffrn_measurement_method       '\w and \f 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  0.1592
_diffrn_reflns_av_unetI/netI     0.0924
_diffrn_reflns_Laue_measured_fraction_full 0.714
_diffrn_reflns_Laue_measured_fraction_max 0.988
_diffrn_reflns_limit_h_max       25
_diffrn_reflns_limit_h_min       -27
_diffrn_reflns_limit_k_max       28
_diffrn_reflns_limit_k_min       -28
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            38439
_diffrn_reflns_point_group_measured_fraction_full 0.714
_diffrn_reflns_point_group_measured_fraction_max 0.988
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         22.464
_diffrn_reflns_theta_min         1.330
_diffrn_source                   'microfocus sealed X-ray tube'
_diffrn_source_type              'Incoatec I\ms'
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.808
_exptl_absorpt_correction_T_max  0.7448
_exptl_absorpt_correction_T_min  0.5860
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
'SADABS-2012/1 (Bruker,2012) was used for absorption correction. wR2(int) was 0.1207 before and 0.0720 after correction. The Ratio of minimum to maximum transmission is 0.7868. The \l/2 correction factor is 0.0015.'
_exptl_crystal_colour            colourless
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    0.914
_exptl_crystal_description       block
_exptl_crystal_F_000             3208
_exptl_crystal_size_max          0.09
_exptl_crystal_size_mid          0.03
_exptl_crystal_size_min          0.03
_refine_diff_density_max         3.298
_refine_diff_density_min         -3.047
_refine_diff_density_rms         0.327
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.834
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     181
_refine_ls_number_reflns         4212
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.834
_refine_ls_R_factor_all          0.2184
_refine_ls_R_factor_gt           0.1547
_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/[\s^2^(Fo^2^)+(0.2000P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.4405
_refine_ls_wR_factor_ref         0.4817
_reflns_Friedel_coverage         0.000
_reflns_number_gt                2614
_reflns_number_total             4212
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ja8b06789_si_009.cif
_cod_data_source_block           sad_a
_cod_original_formula_sum        'C13 H3 O16 Zr4.80'
_cod_database_code               4132823
_shelxl_version_number           2014/6
_shelx_estimated_absorpt_t_max   0.976
_shelx_estimated_absorpt_t_min   0.931
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
2. Uiso/Uaniso restraints and constraints
Uanis(C7) = Uanis(C8) = Uanis(C8A)
3. Others
 Fixed Sof: C8A(0.5) C8(0.5) Zr0A(0.3) Zr1A(0.15) Zr3A(0.15) Zr2A(0.3)
4.a Aromatic/amide H refined with riding coordinates:
 C4(H4), C5(H5)
;
_olex2_submission_special_instructions 'No special instructions were received'