Zr- and Hf-Based Metal‒Organic Frameworks: Tracking Down the Polymorphism
Bon, Volodymyr; Senkovska, Irena; Baburin, Igor A.; Kaskel, Stefan; Crystal Growth & Design 13 (2013) 1231–; doi:10.1021/cg301691d

data_4507519
_publ_section_title
;
 Zr- and Hf-Based Metal--Organic Frameworks: Tracking Down the
 Polymorphism
;
_journal_issue                   3
_journal_name_full               'Crystal Growth &amp; Design'
_journal_page_first              1231
_journal_paper_doi               10.1021/cg301691d
_journal_volume                  13
_journal_year                    2013
_chemical_formula_sum            'C26.4 H8 O32.6 S4.4 Zr6.07'
_chemical_formula_weight         1541.72
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           229
_symmetry_cell_setting           cubic
_symmetry_space_group_name_Hall  '-I 4 2 3'
_symmetry_space_group_name_H-M   'I m -3 m'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                90.00
_cell_formula_units_Z            60
_cell_length_a                   53.680(6)
_cell_length_b                   53.680(6)
_cell_length_c                   53.680(6)
_cell_measurement_reflns_used    586
_cell_measurement_temperature    296(2)
_cell_measurement_theta_max      29.76
_cell_measurement_theta_min      2.76
_cell_volume                     154681(3)
_computing_cell_refinement       'mosflm 1.0.5'
_computing_data_collection       'marCCD 1994-2002'
_computing_data_reduction        scala
_computing_molecular_graphics    'Diamond 3.1'
_computing_publication_material  WinGX
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1997)'
_diffrn_ambient_temperature      296(2)
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device_type  'MX-225 CCD'
_diffrn_measurement_method       '\D\f scans'
_diffrn_radiation_monochromator  'Si 111'
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           synchrotron
_diffrn_radiation_wavelength     0.88561
_diffrn_reflns_av_R_equivalents  0.0819
_diffrn_reflns_av_sigmaI/netI    0.1284
_diffrn_reflns_limit_h_max       38
_diffrn_reflns_limit_h_min       0
_diffrn_reflns_limit_k_max       68
_diffrn_reflns_limit_k_min       1
_diffrn_reflns_limit_l_max       68
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_number            28373
_diffrn_reflns_theta_full        34.14
_diffrn_reflns_theta_max         34.14
_diffrn_reflns_theta_min         3.21
_diffrn_source                   synchrotron
_diffrn_source_type              'BESSY BL MX-14.2'
_exptl_absorpt_coefficient_mu    1.305
_exptl_absorpt_correction_T_max  0.9619
_exptl_absorpt_correction_T_min  0.9619
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   Scala
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    0.993
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       cubic
_exptl_crystal_F_000             44424
_exptl_crystal_size_max          0.03
_exptl_crystal_size_mid          0.03
_exptl_crystal_size_min          0.03
_refine_diff_density_max         2.655
_refine_diff_density_min         -1.305
_refine_diff_density_rms         0.225
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.056
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     473
_refine_ls_number_reflns         14841
_refine_ls_number_restraints     71
_refine_ls_restrained_S_all      1.055
_refine_ls_R_factor_all          0.0845
_refine_ls_R_factor_gt           0.0795
_refine_ls_shift/su_max          0.020
_refine_ls_shift/su_mean         0.001
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.1277P)^2^+1818.4890P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2328
_refine_ls_wR_factor_ref         0.2403
_reflns_number_gt                13340
_reflns_number_total             14841
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            cg301691d_si_001.cif
_cod_data_source_block           DUT-68(Zr)
_cod_original_cell_volume        154681(31)
_cod_original_sg_symbol_H-M      Im-3m
_cod_original_formula_sum        'C26.40 H8 O32.60 S4.40 Zr6.07'
_cod_database_code               4507519