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_4346049
_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         '0.5(C123.84 H74.24 N20.64 O56 Zr12), 4(O)'
_chemical_formula_sum            'C61.92 H37.05 N10.32 O32 Zr6'
_chemical_formula_weight         1984.90
_chemical_name_common            Zr6O4(OH)4(bpydc)5.16
_space_group_crystal_system      cubic
_space_group_IT_number           225
_space_group_name_Hall           '-F 4 2 3'
_space_group_name_H-M_alt        'F m -3 m'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_date             2014-11-06
_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                   26.520(2)
_cell_length_b                   26.520(2)
_cell_length_c                   26.520(2)
_cell_measurement_reflns_used    5088
_cell_measurement_temperature    100(2)
_cell_volume                     18652(2)
_computing_cell_refinement       'Bruker SAINT v8.27b'
_computing_data_reduction        'Bruker SAINT v8.27b'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL-2014/6 (Sheldrick, 2014)'
_computing_structure_solution    SHELXS-2014
_diffrn_ambient_temperature      100(2)
_diffrn_detector_area_resol_mean 8.366
_diffrn_measured_fraction_theta_full 0.944
_diffrn_measured_fraction_theta_max 0.940
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0708
_diffrn_reflns_av_unetI/netI     0.0344
_diffrn_reflns_Laue_measured_fraction_full 0.944
_diffrn_reflns_Laue_measured_fraction_max 0.940
_diffrn_reflns_limit_h_max       26
_diffrn_reflns_limit_h_min       -29
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -27
_diffrn_reflns_limit_l_max       26
_diffrn_reflns_limit_l_min       -30
_diffrn_reflns_number            14200
_diffrn_reflns_point_group_measured_fraction_full 0.944
_diffrn_reflns_point_group_measured_fraction_max 0.940
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         25.325
_diffrn_reflns_theta_min         1.330
_diffrn_source                   'micro focus sealed tube'
_exptl_absorpt_coefficient_mu    0.360
_exptl_absorpt_correction_T_max  0.4901
_exptl_absorpt_correction_T_min  0.4534
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2008/1 (Bruker,2008) was used for absorption correction.
wR2(int) was 0.0624 before and 0.0511 after correction.
The Ratio of minimum to maximum transmission is 0.9251.
The \l/2 correction factor is 0.0000.
;
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    0.707
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       octahedral
_exptl_crystal_F_000             3907
_exptl_crystal_size_max          0.04
_exptl_crystal_size_mid          0.04
_exptl_crystal_size_min          0.04
_refine_diff_density_max         0.284
_refine_diff_density_min         -0.755
_refine_diff_density_rms         0.068
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.084
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     47
_refine_ls_number_reflns         866
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.084
_refine_ls_R_factor_all          0.0396
_refine_ls_R_factor_gt           0.0329
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0639P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0984
_refine_ls_wR_factor_ref         0.0997
_reflns_Friedel_coverage         0.000
_reflns_number_gt                704
_reflns_number_total             866
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ic5b00096_si_001.cif
_cod_data_source_block           mig006_0m
_cod_depositor_comments
;
The following automatic conversions were performed:

data item '_atom_sites_solution_secondary' value 'diffmap' was
changed to 'difmap'.

Automatic conversion script
Id: cif_fix_values 6909 2019-04-08 15:41:33Z antanas 
;
_cod_original_cell_volume        18652(4)
_cod_database_code               4346049
_shelxl_version_number           2014/6
_shelx_estimated_absorpt_t_max   0.986
_shelx_estimated_absorpt_t_min   0.986
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
2. Shared sites
{N9, C9}
3. Rigid bond restraints
 O3
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
4. Uiso/Uaniso restraints and constraints
O3: within 2.5A with sigma of 0.04 and sigma for terminal atoms of 0.08
Uanis(N9) = Uanis(C9)
5. Others
 Fixed Sof: O2B(0.08333) O1(0.43) C4(0.215) C5(0.215) C8(0.215) C9(0.215)
 H9(0.215) N9(0.215) C10(0.43) H10(0.25) O2A(0.08333) O3(0.07)
6.a Aromatic/amide H refined with riding coordinates:
 C9(H9), C10(H10), C10(H10A)
;
_shelx_res_checksum              67512
_shelx_hkl_checksum              94231
_olex2_submission_special_instructions 'No special instructions were received'