Single-crystal-to-single-crystal metalation of a metal-organic framework: a route toward structurally well-defined catalysts.
Gonzalez, Miguel I.; Bloch, Eric D.; Mason, Jarad A.; Teat, Simon J.; Long, Jeffrey R.; Inorganic chemistry 54 (2015) 2995–3005; doi:10.1021/acs.inorgchem.5b00096

data_4346043
_publ_section_title
;
 Single-crystal-to-single-crystal metalation of a metal-organic framework:
 a route toward structurally well-defined catalysts.
;
_journal_issue                   6
_journal_name_full               'Inorganic chemistry'
_journal_page_first              2995
_journal_page_last               3005
_journal_paper_doi               10.1021/acs.inorgchem.5b00096
_journal_volume                  54
_journal_year                    2015
_chemical_formula_sum            'C83.76 H65.17 Cl10.44 Cu5.22 N21 O32 Zr6'
_chemical_formula_weight         3126.95
_chemical_name_common            Zr6O4(OH)4(bpydc)5.22(CuCl2)5.22(CH3CN)10.56
_space_group_crystal_system      cubic
_space_group_IT_number           205
_space_group_name_Hall           '-P 2ac 2ab 3'
_space_group_name_H-M_alt        'P a -3'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-2014
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   26.0483(7)
_cell_length_b                   26.0483(7)
_cell_length_c                   26.0483(7)
_cell_measurement_reflns_used    9948
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      35.91
_cell_measurement_theta_min      2.81
_cell_volume                     17674.1(8)
_computing_cell_refinement       'Bruker SAINT v8.18c'
_computing_data_collection       'Bruker APEX 2'
_computing_data_reduction        'Bruker SAINT v8.18c'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL-2014 (Sheldrick, 2014)'
_computing_structure_solution    SHELXS-2014
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 1.000
_diffrn_measurement_device_type  'Bruker APEX II CCD diffractometer'
_diffrn_measurement_method       '\w/\q scans'
_diffrn_radiation_type           synchrotron
_diffrn_radiation_wavelength     0.7749
_diffrn_reflns_av_R_equivalents  0.0825
_diffrn_reflns_av_unetI/netI     0.0252
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 1.000
_diffrn_reflns_limit_h_max       38
_diffrn_reflns_limit_h_min       -38
_diffrn_reflns_limit_k_max       38
_diffrn_reflns_limit_k_min       -38
_diffrn_reflns_limit_l_max       38
_diffrn_reflns_limit_l_min       -38
_diffrn_reflns_number            232855
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 1.000
_diffrn_reflns_theta_full        27.706
_diffrn_reflns_theta_max         35.377
_diffrn_reflns_theta_min         1.205
_diffrn_source                   'Advanced Light Source station 11.3.1'
_exptl_absorpt_coefficient_mu    1.464
_exptl_absorpt_correction_T_max  0.944
_exptl_absorpt_correction_T_min  0.815
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS 2008/1 Bruker AXS Madison WI USA'
_exptl_crystal_colour            Green
_exptl_crystal_density_diffrn    1.175
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       octahedron
_exptl_crystal_F_000             6158
_exptl_crystal_size_max          0.040
_exptl_crystal_size_mid          0.040
_exptl_crystal_size_min          0.040
_refine_diff_density_max         2.329
_refine_diff_density_min         -1.267
_refine_diff_density_rms         0.124
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.059
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     321
_refine_ls_number_reflns         10593
_refine_ls_number_restraints     48
_refine_ls_restrained_S_all      1.059
_refine_ls_R_factor_all          0.0428
_refine_ls_R_factor_gt           0.0380
_refine_ls_shift/su_max          0.003
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0726P)^2^+21.8758P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1134
_refine_ls_wR_factor_ref         0.1189
_reflns_Friedel_coverage         0.000
_reflns_number_gt                9788
_reflns_number_total             10593
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ic5b00096_si_007.cif
_cod_data_source_block           mig028s_0m
_cod_depositor_comments
;
The following automatic conversions were performed:

data item '_atom_sites_solution_primary' value 'Direct' was changed
to 'direct' in accordance with the
/home/saulius/struct/COD-crude-data/automatic-downloads/DataCite-retrospective/ACS/depositions/lib/dictionaries/cif_core.dic
dictionary named 'cif_core.dic' version 2.4.2 last updated on
2011-04-26.

Automatic conversion script
Id: cif_fix_values 6909 2019-04-08 15:41:33Z antanas 
;
_cod_original_cell_volume        17674.1(14)
_cod_database_code               4346043
_shelx_estimated_absorpt_t_min   0.944
_shelx_estimated_absorpt_t_max   0.944
_shelxl_version_number           2014-3
_shelx_res_checksum              76458
_shelx_hkl_checksum              75771