Robust Corrole-Based Metal-Organic Frameworks with Rare 9-Connected Zr/Hf-Oxo Clusters.
Zhao, Yanming; Qi, Shibo; Niu, Zheng; Peng, Yunlei; Shan, Chuan; Verma, Gaurav; Wojtas, Lukasz; Zhang, Zhenjie; Zhang, Bao; Feng, Yaqing; Chen, Yu-Sheng; Ma, Shengqian; Journal of the American Chemical Society 141 (2019) 14443–14450; doi:10.1021/jacs.9b07700

data_4128776
_publ_section_title
;
 Robust Corrole-Based Metal-Organic Frameworks with Rare 9-Connected
 Zr/Hf-Oxo Clusters.
;
_journal_issue                   36
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              14443
_journal_page_last               14450
_journal_paper_doi               10.1021/jacs.9b07700
_journal_volume                  141
_journal_year                    2019
_chemical_formula_moiety         'C120 H60 N12 O32 Zr6'
_chemical_formula_sum            'C120 H60 N12 O32 Zr6'
_chemical_formula_weight         2729.12
_space_group_crystal_system      hexagonal
_space_group_IT_number           194
_space_group_name_Hall           '-P 6c 2c'
_space_group_name_H-M_alt        'P 63/m m c'
_atom_sites_solution_hydrogens   geom
_audit_creation_date             2019-01-31
_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            2
_cell_length_a                   28.6282(14)
_cell_length_b                   28.6282(14)
_cell_length_c                   25.6439(12)
_cell_measurement_reflns_used    9847
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      74.22
_cell_measurement_theta_min      2.48
_cell_volume                     18201.3(15)
_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  'XL (Sheldrick, 2008)'
_computing_structure_solution    'SHELXT 2014/5 (Sheldrick, 2014)'
_diffrn_ambient_temperature      100.02
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measurement_device_type  'Bruker D8 Venture PHOTON II CPAD'
_diffrn_measurement_method       'omega scans'
_diffrn_radiation_monochromator  mirrors
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54178
_diffrn_reflns_av_R_equivalents  0.1269
_diffrn_reflns_av_unetI/netI     0.0256
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.997
_diffrn_reflns_limit_h_max       35
_diffrn_reflns_limit_h_min       -34
_diffrn_reflns_limit_k_max       35
_diffrn_reflns_limit_k_min       -35
_diffrn_reflns_limit_l_max       31
_diffrn_reflns_limit_l_min       -32
_diffrn_reflns_number            259551
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.997
_diffrn_reflns_theta_full        67.679
_diffrn_reflns_theta_max         74.608
_diffrn_reflns_theta_min         2.479
_diffrn_source                   'INCOATEC Imus micro-focus source'
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    1.587
_exptl_absorpt_correction_T_max  1.0000
_exptl_absorpt_correction_T_min  0.8338
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2016/2 (Bruker,2016/2) was used for absorption correction.
wR2(int) was 0.1078 before and 0.0764 after correction.
The Ratio of minimum to maximum transmission is 0.8338.
The \l/2 correction factor is Not present.
;
_exptl_crystal_density_diffrn    0.498
_exptl_crystal_description       plate
_exptl_crystal_F_000             2720
_exptl_crystal_size_max          0.07
_exptl_crystal_size_mid          0.06
_exptl_crystal_size_min          0.06
_refine_diff_density_max         0.714
_refine_diff_density_min         -0.848
_refine_diff_density_rms         0.058
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.192
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     274
_refine_ls_number_reflns         6739
_refine_ls_number_restraints     81
_refine_ls_restrained_S_all      1.208
_refine_ls_R_factor_all          0.1144
_refine_ls_R_factor_gt           0.0871
_refine_ls_shift/su_max          0.001
_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          0.2788
_refine_ls_wR_factor_ref         0.3285
_reflns_Friedel_coverage         0.000
_reflns_number_gt                4084
_reflns_number_total             6739
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ja9b07700_si_002.cif
_cod_data_source_block           zym_corrole_mof_def_0m_sq
_cod_original_cell_volume        18201(2)
_cod_database_code               4128776
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   0.911
_shelx_estimated_absorpt_t_min   0.897
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
2. Others
 Fixed Sof: Zr1(0.5) O3(0.5) O4(0.5) C12(0.5) C17(0.5) C16(0.5) H16(0.5)
 C15(0.5) H15(0.5) C14(0.5) C19(0.5) H19(0.5) C18(0.5) H18(0.5) C20(0.5)
 N22(0.5) C23(0.5) C24(0.5) H24(0.5) C25(0.5) H25(0.5) C21(0.5) C26(0.5)
 C27(0.5) H27(0.5) C28(0.5) H28(0.5) C29(0.5) N30(0.5) C31(0.25) C32(0.25)
 C33(0.25) H33(0.25) C34(0.25) H34(0.25) C35(0.25) C36(0.25) H36(0.25)
 C37(0.25) H37(0.25) C38(0.25) O39(0.5)
3.a Aromatic/amide H refined with riding coordinates:
 C16(H16), C15(H15), C19(H19), C18(H18), C24(H24), C25(H25), C27(H27),
 C28(H28), C33(H33), C34(H34), C36(H36), C37(H37)
;
_shelx_res_checksum              96736
_shelx_hkl_checksum              28517
_shelx_fab_checksum              24721
_olex2_submission_special_instructions 'No special instructions were received'