Vanadium Catalyst on Isostructural Transition Metal, Lanthanide, and Actinide Based Metal-Organic Frameworks for Alcohol Oxidation.
Wang, Xingjie; Zhang, Xuan; Li, Peng; Otake, Ken-Ichi; Cui, Yuexing; Lyu, Jiafei; Krzyaniak, Matthew D.; Zhang, Yuanyuan; Li, Zhanyong; Liu, Jian; Buru, Cassandra T.; Islamoglu, Timur; Wasielewski, Michael R.; Li, Zhong; Farha, Omar K.; Journal of the American Chemical Society 141 (2019) 8306–8314; doi:10.1021/jacs.9b02603

data_4127345
_publ_section_title
;
 Vanadium Catalyst on Isostructural Transition Metal, Lanthanide, and
 Actinide Based Metal-Organic Frameworks for Alcohol Oxidation.
;
_journal_issue                   20
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              8306
_journal_page_last               8314
_journal_paper_doi               10.1021/jacs.9b02603
_journal_volume                  141
_journal_year                    2019
_chemical_formula_moiety         '0.04(C255 H168 Hf18 O120 V2.4)'
_chemical_formula_sum            'C10.62 H7 Hf0.75 O5 V0.1'
_chemical_formula_weight         353.62
_space_group_crystal_system      cubic
_space_group_IT_number           221
_space_group_name_Hall           '-P 4 2 3'
_space_group_name_H-M_alt        'P m -3 m'
_symmetry_space_group_name_Hall  '-P 4 2 3'
_symmetry_space_group_name_H-M   'P m -3 m'
_atom_sites_solution_hydrogens   geom
_audit_creation_date             2019-02-19
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            24
_cell_length_a                   28.2300(3)
_cell_length_b                   28.2300(3)
_cell_length_c                   28.2300(3)
_cell_measurement_reflns_used    9686
_cell_measurement_temperature    250
_cell_measurement_theta_max      50.44
_cell_measurement_theta_min      5.86
_cell_volume                     22497.4(4)
_computing_cell_refinement       'SAINT v8.34A (Bruker, 2013)'
_computing_data_reduction        'SAINT v8.34A (Bruker, 2013)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_diffrn_ambient_temperature      250
_diffrn_detector                 'Bruker APEX2 area detector'
_diffrn_detector_area_resol_mean 7.9
_diffrn_detector_type            'CCD area detector'
_diffrn_measured_fraction_theta_full 0.593
_diffrn_measured_fraction_theta_max 0.994
_diffrn_measurement_device       'three-circle diffractometer'
_diffrn_measurement_device_type  'Bruker SMART APEX2 area detector'
_diffrn_measurement_method       '\w and \f scans'
_diffrn_radiation_monochromator  'mirror optics'
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54178
_diffrn_reflns_av_R_equivalents  0.0756
_diffrn_reflns_av_unetI/netI     0.0202
_diffrn_reflns_Laue_measured_fraction_full 0.593
_diffrn_reflns_Laue_measured_fraction_max 0.994
_diffrn_reflns_limit_h_max       24
_diffrn_reflns_limit_h_min       -28
_diffrn_reflns_limit_k_max       28
_diffrn_reflns_limit_k_min       -28
_diffrn_reflns_limit_l_max       26
_diffrn_reflns_limit_l_min       -24
_diffrn_reflns_number            57996
_diffrn_reflns_point_group_measured_fraction_full 0.593
_diffrn_reflns_point_group_measured_fraction_max 0.994
_diffrn_reflns_theta_full        67.679
_diffrn_reflns_theta_max         50.437
_diffrn_reflns_theta_min         5.650
_diffrn_source                   'microfocus sealed X-ray tube'
_diffrn_source_type              'Incoatec I\ms'
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    4.142
_exptl_absorpt_correction_T_max  0.7500
_exptl_absorpt_correction_T_min  0.6390
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
'SADABS-2012/1 (Bruker,2012) was used for absorption correction. wR2(int) was 0.1781 before and 0.0603 after correction. The Ratio of minimum to maximum transmission is 0.8520. The \l/2 correction factor is 0.0015.'
_exptl_crystal_colour            green
_exptl_crystal_colour_primary    green
_exptl_crystal_density_diffrn    0.626
_exptl_crystal_description       block
_exptl_crystal_F_000             4009
_exptl_crystal_size_max          0.08
_exptl_crystal_size_mid          0.06
_exptl_crystal_size_min          0.05
_refine_diff_density_max         1.350
_refine_diff_density_min         -2.279
_refine_diff_density_rms         0.149
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   3.040
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     98
_refine_ls_number_reflns         2350
_refine_ls_number_restraints     65
_refine_ls_restrained_S_all      3.005
_refine_ls_R_factor_all          0.2150
_refine_ls_R_factor_gt           0.1894
_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^)+(0.2000P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.6168
_refine_ls_wR_factor_ref         0.6381
_reflns_Friedel_coverage         0.000
_reflns_number_gt                1759
_reflns_number_total             2350
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ja9b02603_si_004.cif
_cod_data_source_block           pm-3m_a
_cod_original_cell_volume        22497.4(7)
_cod_original_formula_sum        'C10.62 H7 Hf0.75 O5 V0.10'
_cod_database_code               4127345
_shelxl_version_number           2014/6
_shelx_estimated_absorpt_t_max   0.820
_shelx_estimated_absorpt_t_min   0.733
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Restrained distances
 C12_$1-C11_$1
 1.5 with sigma of 0.04
 O4-C11
 2.35 with sigma of 0.04
 V1-O4_$2
 2.1 with sigma of 0.04
 O5A-V1
 1.6 with sigma of 0.04
 V1-O5A \\sim V1-O5
 with sigma of 0.02
3. Restrained planarity
 C2, C7, C6, C5, C4, C3
 with sigma of 0.1
4. Rigid bond restraints
 C2, C7, C6, C5, C4, C3, C1
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
5. Uiso/Uaniso restraints and constraints
C2 \\sim C3 \\sim C4 \\sim C5 \\sim C6 \\sim C7 \\sim C1: within 2A with sigma
of 0.04 and sigma for terminal atoms of 0.08
: with sigma of 0.1 and sigma for terminal atoms of 0.2
Uanis(C12) = Uanis(C11) = Uanis(C13) = Uanis(C1)
Uanis(O4) = Uanis(O1) = Uanis(O2)
Uanis(O5A) = Uanis(O1) = Uanis(O5)
6. Others
 Sof(O5)=0.5*(1-FVAR(2))
 Sof(O5A)=0.5*FVAR(2)
 Fixed Sof: H10A(0.5) H10B(0.5) H10C(0.5) C12(0.125) C13(0.0625) C11(0.125)
 V1(0.05)
7.a Aromatic/amide H refined with riding coordinates:
 C7(H7), C6(H6), C4(H4), C3(H3)
7.b Idealised Me refined as rotating group:
 C10(H10A,H10B,H10C)
;
_olex2_submission_special_instructions 'No special instructions were received'