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_4346047
_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_moiety
'0.25(C338.11 H156.16 Cr19.8 N43.15 O197.5 Zr24), 0.89(C2 N H)'
_chemical_formula_sum            'C86.31 H39.04 Cr4.95 N11.68 O49.38 Zr6'
_chemical_formula_weight         2834.30
_chemical_name_common            Zr6O4(OH)4(bpydc)5.4(Co(CO)4)4.95(CH3CN)0.88
_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             2014-12-03
_audit_creation_method
;
Olex2 1.2
(compiled 2014.11.28 svn.r3107 for OlexSys, GUI svn.r4959)
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   26.0682(19)
_cell_length_b                   26.0682(19)
_cell_length_c                   26.0682(19)
_cell_measurement_reflns_used    9440
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      39.91
_cell_measurement_theta_min      2.83
_cell_volume                     17715(2)
_computing_cell_refinement       'Bruker SAINT v8.34A'
_computing_data_collection       'Bruker APEX 2'
_computing_data_reduction        'Bruker SAINT v8.34A'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'SHELXL-2014/4 (Sheldrick, 2014)'
_computing_structure_refinement  'SHELXL-2014/4 (Sheldrick, 2014)'
_computing_structure_solution    'SHELXS-2013/1 (Sheldrick, 2013)'
_diffrn_ambient_temperature      100(2)
_diffrn_detector_area_resol_mean 10.42
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 1.000
_diffrn_measurement_device_type  'Bruker PHOTON100 CMOS diffractometer'
_diffrn_measurement_method       '\w/\q scans'
_diffrn_radiation_type           synchrotron
_diffrn_radiation_wavelength     0.7749
_diffrn_reflns_av_R_equivalents  0.0876
_diffrn_reflns_av_unetI/netI     0.0405
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 1.000
_diffrn_reflns_limit_h_max       43
_diffrn_reflns_limit_h_min       -25
_diffrn_reflns_limit_k_max       42
_diffrn_reflns_limit_k_min       -43
_diffrn_reflns_limit_l_max       43
_diffrn_reflns_limit_l_min       -41
_diffrn_reflns_number            169670
_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         40.098
_diffrn_reflns_theta_min         2.556
_diffrn_source                   'Advanced Light Source Station 11.3.1'
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.874
_exptl_absorpt_correction_T_max  0.9283
_exptl_absorpt_correction_T_min  0.8343
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS 2008/1 Bruker AXS Madison WI USA'
_exptl_crystal_colour            'dark green'
_exptl_crystal_density_diffrn    1.060
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             5543
_exptl_crystal_size_max          0.06
_exptl_crystal_size_mid          0.06
_exptl_crystal_size_min          0.06
_refine_diff_density_max         2.472
_refine_diff_density_min         -0.874
_refine_diff_density_rms         0.179
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.088
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     287
_refine_ls_number_reflns         14578
_refine_ls_number_restraints     28
_refine_ls_restrained_S_all      1.089
_refine_ls_R_factor_all          0.0653
_refine_ls_R_factor_gt           0.0560
_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^)+(0.1007P)^2^+29.6922P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1659
_refine_ls_wR_factor_ref         0.1736
_reflns_Friedel_coverage         0.000
_reflns_number_gt                12852
_reflns_number_total             14578
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ic5b00096_si_005.cif
_cod_data_source_block           mig078sp
_cod_original_cell_volume        17715(4)
_cod_database_code               4346047
_shelxl_version_number           2014/6
_shelx_estimated_absorpt_t_max   0.949
_shelx_estimated_absorpt_t_min   0.949
_olex2_refinement_description
;
1. Twinned data refinement
 Scales: 0.5003(11) 0.4997(11)
2. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
3. Restrained distances
 N3-C17
 1.16 with sigma of 0.02
 C18-C17
 1.43 with sigma of 0.02
4. Rigid bond restraints
 O1B, O1A, O2A, O2B
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
 C15, O9, C16, O10
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
5. Uiso/Uaniso restraints and constraints
O1B \\sim O1A \\sim O2B \\sim O2A: within 1.7A with sigma of 0.04 and sigma for
terminal atoms of 0.08
C16 \\sim O10 \\sim C15 \\sim O9: within 2A with sigma of 0.02 and sigma for
terminal atoms of 0.04
6. Others
 Fixed Sof: O1A(0.16667) O2A(0.5) O1B(0.16667) O2B(0.5) O3(0.899) O4(0.899)
 O5(0.899) O6(0.899) C1(0.899) C2(0.899) H2(0.899) C3(0.899) H3(0.899)
 C4(0.899) C5(0.899) H5(0.899) C6(0.899) C7(0.899) H7(0.899) C8(0.899)
 H8(0.899) C9(0.899) C10(0.899) H10(0.899) C11(0.899) C12(0.899) N1(0.899)
 N2(0.899) Cr1(0.825) C13(0.825) C14(0.825) C15(0.825) C16(0.825) O7(0.825)
 O8(0.825) O9(0.825) O10(0.825) N3(0.14833) C17(0.14833) C18(0.14833)
7.a Aromatic/amide H refined with riding coordinates:
 C2(H2), C3(H3), C5(H5), C7(H7), C8(H8), C10(H10)
;
_shelx_res_checksum              72249
_shelx_hkl_checksum              98540
_olex2_submission_special_instructions 'No special instructions were received'