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_4127347
_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 O124.8 V2.4 Zr18)'
_chemical_formula_sum            'C10.62 H7 O5.2 V0.1 Zr0.75'
_chemical_formula_weight         291.37
_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
_atom_sites_solution_primary     dual
_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                   28.2644(4)
_cell_length_b                   28.2644(4)
_cell_length_c                   28.2644(4)
_cell_measurement_reflns_used    9182
_cell_measurement_temperature    200
_cell_measurement_theta_max      65.17
_cell_measurement_theta_min      3.50
_cell_volume                     22579.8(6)
_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)'
_computing_structure_solution    'ShelXT (Sheldrick, 2015)'
_diffrn_ambient_temperature      200.0
_diffrn_detector_area_resol_mean 7.9
_diffrn_detector_type            'CCD area detector'
_diffrn_measured_fraction_theta_full 0.950
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device       'three-circle diffractometer'
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54178
_diffrn_reflns_av_R_equivalents  0.0581
_diffrn_reflns_av_unetI/netI     0.0207
_diffrn_reflns_Laue_measured_fraction_full 0.950
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_limit_h_max       28
_diffrn_reflns_limit_h_min       -33
_diffrn_reflns_limit_k_max       32
_diffrn_reflns_limit_k_min       -33
_diffrn_reflns_limit_l_max       32
_diffrn_reflns_limit_l_min       -33
_diffrn_reflns_number            98182
_diffrn_reflns_point_group_measured_fraction_full 0.950
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_theta_full        67.679
_diffrn_reflns_theta_max         65.212
_diffrn_reflns_theta_min         2.211
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    2.085
_exptl_absorpt_correction_T_max  0.7526
_exptl_absorpt_correction_T_min  0.6191
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
'SADABS-2012/1 (Bruker,2012) was used for absorption correction. wR2(int) was 0.0955 before and 0.0762 after correction. The Ratio of minimum to maximum transmission is 0.8226. The \l/2 correction factor is Not present.'
_exptl_crystal_colour            brown
_exptl_crystal_colour_primary    brown
_exptl_crystal_density_diffrn    0.514
_exptl_crystal_description       bock
_exptl_crystal_F_000             3472
_exptl_crystal_size_max          0.21
_exptl_crystal_size_mid          0.21
_exptl_crystal_size_min          0.1
_refine_diff_density_max         2.317
_refine_diff_density_min         -1.655
_refine_diff_density_rms         0.111
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   2.692
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     112
_refine_ls_number_reflns         3769
_refine_ls_number_restraints     32
_refine_ls_restrained_S_all      2.691
_refine_ls_R_factor_all          0.1608
_refine_ls_R_factor_gt           0.1458
_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          0.5059
_refine_ls_wR_factor_ref         0.5590
_reflns_Friedel_coverage         0.000
_reflns_number_gt                2917
_reflns_number_total             3769
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ja9b02603_si_003.cif
_cod_data_source_block           pm-3m_a
_cod_original_cell_volume        22579.8(10)
_cod_original_formula_sum        'C10.62 H7 O5.20 V0.10 Zr0.75'
_cod_database_code               4127347
_shelxl_version_number           2014/6
_shelx_estimated_absorpt_t_max   0.819
_shelx_estimated_absorpt_t_min   0.669
_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
 C11-C13
 1.4 with sigma of 0.02
 O4-C12
 2.35 with sigma of 0.04
 C11-C12
 1.5 with sigma of 0.04
 C13-C12
 2.5 with sigma of 0.04
 V1_$1-O6_$1
 1.6 with sigma of 0.04
 V1-O4 = V1-O5
 2.1 with sigma of 0.04
 O6-V1 \\sim O6A-V1
 with sigma of 0.02
3. Uiso/Uaniso restraints and constraints
Uanis(C13) \\sim Ueq, Uanis(C11) \\sim Ueq, Uanis(C12) \\sim Ueq: with sigma of
0.1 and sigma for terminal atoms of 0.2
Uanis(V1) \\sim Ueq: with sigma of 0.1 and sigma for terminal atoms of 0.2
Uanis(C1) = Uanis(C12) = Uanis(C11) = Uanis(C13)
Uanis(O6) = Uanis(O2) = Uanis(O5) = Uanis(O6A)
4. Others
 Sof(O6A)=0.5*(1-FVAR(2))
 Sof(O6)=0.5*FVAR(2)
 Fixed Sof: H10A(0.5) H10B(0.5) H10C(0.5) C11(0.125) C13(0.0625) C12(0.125)
 V1(0.05) O5(0.1)
5.a Aromatic/amide H refined with riding coordinates:
 C7(H7), C6(H6), C3(H3), C4(H4)
5.b Idealised Me refined as rotating group:
 C10(H10A,H10B,H10C)
;
_olex2_submission_special_instructions 'No special instructions were received'