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_4346044
_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            'C67.2 H40.72 Br8.4 Fe4.2 N12.24 O29.36 Zr6'
_chemical_formula_weight         2942.45
_chemical_name_common            Zr6O4(OH)4(bpydc)5.34(FeBr2)4.20(CH3CN)1.56
_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_date             2014-11-16
_audit_creation_method
;
Olex2 1.2
(compiled 2014.08.28 svn.r2986 for OlexSys, GUI svn.r4874)
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   26.255(4)
_cell_length_b                   26.255(4)
_cell_length_c                   26.255(4)
_cell_measurement_reflns_used    9848
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      33.121
_cell_measurement_theta_min      3.384
_cell_volume                     18098(5)
_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 0.996
_diffrn_measured_fraction_theta_max 0.997
_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  0.0854
_diffrn_reflns_av_unetI/netI     0.0265
_diffrn_reflns_Laue_measured_fraction_full 0.996
_diffrn_reflns_Laue_measured_fraction_max 0.997
_diffrn_reflns_limit_h_max       34
_diffrn_reflns_limit_h_min       -34
_diffrn_reflns_limit_k_max       34
_diffrn_reflns_limit_k_min       -34
_diffrn_reflns_limit_l_max       34
_diffrn_reflns_limit_l_min       -34
_diffrn_reflns_number            165536
_diffrn_reflns_point_group_measured_fraction_full 0.996
_diffrn_reflns_point_group_measured_fraction_max 0.997
_diffrn_reflns_theta_full        27.706
_diffrn_reflns_theta_max         30.202
_diffrn_reflns_theta_min         2.675
_diffrn_source                   'Advanced Light Source station 11.3.1'
_exptl_absorpt_coefficient_mu    3.202
_exptl_absorpt_correction_T_max  0.9282
_exptl_absorpt_correction_T_min  0.8326
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS 2008/1 Bruker AXS Madison WI USA'
_exptl_crystal_colour            'red violet'
_exptl_crystal_density_diffrn    1.081
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       octahedron
_exptl_crystal_F_000             5596
_exptl_crystal_size_max          0.04
_exptl_crystal_size_mid          0.04
_exptl_crystal_size_min          0.04
_refine_diff_density_max         1.642
_refine_diff_density_min         -1.070
_refine_diff_density_rms         0.169
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.169
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     251
_refine_ls_number_reflns         7128
_refine_ls_number_restraints     54
_refine_ls_restrained_S_all      1.191
_refine_ls_R_factor_all          0.0742
_refine_ls_R_factor_gt           0.0683
_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^)+(0.1103P)^2^+68.6096P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2029
_refine_ls_wR_factor_ref         0.2074
_reflns_Friedel_coverage         0.000
_reflns_number_gt                6551
_reflns_number_total             7128
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ic5b00096_si_008.cif
_cod_data_source_block           mig060s
_cod_original_cell_volume        18098(8)
_cod_original_formula_sum
'C67.20 H40.72 Br8.40 Fe4.20 N12.24 O29.36 Zr6'
_cod_database_code               4346044
_shelxl_version_number           2014/6
_shelx_estimated_absorpt_t_max   0.883
_shelx_estimated_absorpt_t_min   0.883
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
2. Rigid bond restraints
 Fe1, Br1A, Br2A, Br2B, Br1B
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
3. Uiso/Uaniso restraints and constraints
Fe1 \\sim Br1A \\sim Br2A \\sim Br2B \\sim Br1B: within 2.6A with sigma of 0.02
and sigma for terminal atoms of 0.04
O2A \\sim O2B \\sim O1A \\sim O1B: within 0.7A with sigma of 0.04 and sigma for
terminal atoms of 0.08
4. Others
 Fixed Sof: O1A(0.5) O2A(0.16667) O1B(0.5) O2B(0.16667) O3(0.89) O4(0.89)
 O5(0.89) O6(0.89) C1(0.89) C2(0.89) H2(0.89) C3(0.89) H3(0.89) C4(0.89)
 C5(0.89) H5(0.89) C6(0.89) C7(0.89) H7(0.89) C8(0.89) H8(0.89) C9(0.89)
 C10(0.89) H10(0.89) C11(0.89) C12(0.89) N1(0.89) N2(0.89) Fe1(0.7) Br1A(0.52)
 Br2A(0.52) Br1B(0.18) Br2B(0.18) C13(0.26) C14(0.26) N3(0.26)
5.a Aromatic/amide H refined with riding coordinates:
 C2(H2), C3(H3), C5(H5), C7(H7), C8(H8), C10(H10)
;
_shelx_res_checksum              16903
_shelx_hkl_checksum              99954
_olex2_submission_special_instructions 'No special instructions were received'