Cross-linking Zr-based Metal-Organic Polyhedra via Postsynthetic Polymerization
Nam, Dongsik; Huh, Jihyun; Lee, Jiyoung; Kwak, Ja Hun; Jeong, Hu Young; Choi, Kyungmin; Choe, Wonyoung; Chem. Sci.  (2017) –; doi:10.1039/C7SC03847J

data_1547341
_publ_section_title
;
 Cross-linking Zr-based Metal-Organic Polyhedra via Postsynthetic
 Polymerization
;
_journal_name_full               'Chem. Sci.'
_journal_paper_doi               10.1039/C7SC03847J
_journal_year                    2017
_chemical_formula_sum            'C149.6 H188 Cl6 N8 O47.4 Zr12'
_chemical_formula_weight         4164.01
_chemical_name_systematic        CLMOP-1c
_space_group_crystal_system      trigonal
_space_group_IT_number           166
_space_group_name_Hall           '-R 3 2"'
_space_group_name_H-M_alt        'R -3 m :H'
_symmetry_space_group_name_Hall  '-R 3 2"'
_symmetry_space_group_name_H-M   'R -3 m :H'
_atom_sites_solution_hydrogens   geom
_audit_creation_method           SHELXL-2014/7
_audit_update_record
;
2016-11-30 deposited with the CCDC.
2017-09-25 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                120
_cell_formula_units_Z            6
_cell_length_a                   26.221(4)
_cell_length_b                   26.221(4)
_cell_length_c                   60.059(12)
_cell_measurement_reflns_used    301451
_cell_measurement_temperature    134(2)
_cell_measurement_theta_max      24.996
_cell_measurement_theta_min      1.044
_cell_volume                     35761(11)
_computing_cell_refinement       HKL2000
_computing_data_collection       MxDC
_computing_data_reduction        HKL2000
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_structure_solution    'Bruker SHELXTL-XS'
_diffrn_ambient_temperature      134(2)
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device_type  'Rayonix Ms225-HS'
_diffrn_measurement_method       'Omega scan'
_diffrn_radiation_type           Synchrotron
_diffrn_radiation_wavelength     0.660
_diffrn_reflns_av_R_equivalents  0.1121
_diffrn_reflns_av_unetI/netI     0.0751
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_limit_h_max       33
_diffrn_reflns_limit_h_min       -33
_diffrn_reflns_limit_k_max       33
_diffrn_reflns_limit_k_min       -28
_diffrn_reflns_limit_l_max       44
_diffrn_reflns_limit_l_min       -76
_diffrn_reflns_number            49471
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_theta_full        23.328
_diffrn_reflns_theta_max         24.996
_diffrn_reflns_theta_min         1.044
_diffrn_source                   'Bending magnet'
_exptl_absorpt_coefficient_mu    2.715
_exptl_absorpt_correction_T_max  0.899
_exptl_absorpt_correction_T_min  0.876
_exptl_absorpt_correction_type   multi-scans
_exptl_absorpt_process_details   HKL2000
_exptl_crystal_colour            'pale yellow'
_exptl_crystal_density_diffrn    1.160
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       cubic
_exptl_crystal_F_000             12617
_exptl_crystal_size_max          0.050
_exptl_crystal_size_mid          0.050
_exptl_crystal_size_min          0.040
_refine_diff_density_max         0.999
_refine_diff_density_min         -0.991
_refine_diff_density_rms         0.093
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.874
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     270
_refine_ls_number_reflns         9345
_refine_ls_number_restraints     3
_refine_ls_restrained_S_all      0.874
_refine_ls_R_factor_all          0.1439
_refine_ls_R_factor_gt           0.0787
_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          0.2562
_refine_ls_wR_factor_ref         0.2949
_reflns_Friedel_coverage         0.000
_reflns_number_gt                4118
_reflns_number_total             9345
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c7sc03847j2.cif
_cod_data_source_block           CLMOP-1c
_cod_original_cell_volume        35760(12)
_cod_original_formula_sum        'C149.60 H188 Cl6 N8 O47.40 Zr12'
_cod_database_code               1547341
_shelx_shelxl_version_number     2014/7
_shelx_res_checksum              20278
_shelx_fab_checksum              43005
_platon_squeeze_void_probe_radius 1.20