Bioinspired Metal-Organic Framework Catalysts for Selective Methane Oxidation to Methanol.
Baek, Jayeon; Rungtaweevoranit, Bunyarat; Pei, Xiaokun; Park, Myeongkee; Fakra, Sirine C.; Liu, Yi-Sheng; Matheu, Roc; Alshmimri, Sultan A.; Alshehri, Saeed; Trickett, Christopher A.; Somorjai, Gabor A.; Yaghi, Omar M.; Journal of the American Chemical Society 140 (2018) 18208–18216; doi:10.1021/jacs.8b11525

data_4133595
_publ_section_title
;
 Bioinspired Metal-Organic Framework Catalysts for Selective Methane
 Oxidation to Methanol.
;
_journal_issue                   51
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              18208
_journal_page_last               18216
_journal_paper_doi               10.1021/jacs.8b11525
_journal_volume                  140
_journal_year                    2018
_chemical_formula_moiety         'C1.9 H0.5 O2.67 Zr0.5, 0.11(O1)'
_chemical_formula_sum            'C1.9 H0.55 O2.77 Zr0.5'
_chemical_formula_weight         113.34
_space_group_crystal_system      cubic
_space_group_IT_number           227
_space_group_name_Hall           '-F 4vw 2vw 3'
_space_group_name_H-M_alt        'F d -3 m :2'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     'dual space'
_atom_sites_solution_secondary   difmap
_audit_creation_date             2018-07-13
_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            192
_cell_length_a                   35.0221(15)
_cell_length_b                   35.0221(15)
_cell_length_c                   35.0221(15)
_cell_measurement_reflns_used    9747
_cell_measurement_temperature    100
_cell_measurement_theta_max      34.049
_cell_measurement_theta_min      3.402
_cell_volume                     42956(3)
_computing_cell_refinement       'SAINT V8.38A Bruker-AXS, Madison WI'
_computing_data_collection       'Bruker APEX3 Bruker-AXS, Madison WI'
_computing_data_reduction        'SAINT V8.38A Bruker-AXS, Madison WI'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL-2014/7 2014/7 Bruker-AXS, Madison WI'
_computing_structure_solution    'SHELXT 2014/5 Bruker-AXS, Madison WI'
_diffrn_ambient_temperature      100
_diffrn_detector_area_resol_mean 7.39
_diffrn_detector_type            CMOS
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device       'Bruker D8 with PHOTON II detector'
_diffrn_measurement_method       '\f and \w shutterless scans'
_diffrn_radiation_monochromator  'silicon 111'
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           synchrotron
_diffrn_radiation_wavelength     0.9538
_diffrn_reflns_av_R_equivalents  0.1312
_diffrn_reflns_av_unetI/netI     0.0341
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_limit_h_max       41
_diffrn_reflns_limit_h_min       -41
_diffrn_reflns_limit_k_max       41
_diffrn_reflns_limit_k_min       -41
_diffrn_reflns_limit_l_max       41
_diffrn_reflns_limit_l_min       -41
_diffrn_reflns_number            110295
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_theta_full        34.247
_diffrn_reflns_theta_max         34.247
_diffrn_reflns_theta_min         2.589
_diffrn_source
;
Advanced Light Source, station 11.3.1
;
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    1.281
_exptl_absorpt_correction_T_max  0.7467
_exptl_absorpt_correction_T_min  0.6575
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
'SADABS-2016/2 (Bruker,2016/2) was used for absorption correction. wR2(int) was 0.1574 before and 0.0970 after correction. The Ratio of minimum to maximum transmission is 0.8805. The \l/2 correction factor is Not present.'
_exptl_crystal_colour            'clear light colourless'
_exptl_crystal_density_diffrn    0.841
_exptl_crystal_description       octahedral
_exptl_crystal_F_000             10393
_exptl_crystal_size_max          0.03
_exptl_crystal_size_mid          0.03
_exptl_crystal_size_min          0.03
_refine_diff_density_max         1.247
_refine_diff_density_min         -0.609
_refine_diff_density_rms         0.170
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.158
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     110
_refine_ls_number_reflns         1795
_refine_ls_number_restraints     105
_refine_ls_restrained_S_all      1.128
_refine_ls_R_factor_all          0.0650
_refine_ls_R_factor_gt           0.0570
_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^)+(0.1472P)^2^+643.8709P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2085
_refine_ls_wR_factor_ref         0.2224
_reflns_Friedel_coverage         0.000
_reflns_number_gt                1593
_reflns_number_total             1795
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ja8b11525_si_004.cif
_cod_data_source_block           MOF-808-BZZ
_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        42956(6)
_cod_original_sg_symbol_H-M      'F d -3 m'
_cod_original_formula_sum        'C1.90 H0.55 O2.77 Zr0.50'
_cod_database_code               4133595
_shelx_shelxl_version_number     2014/7
_shelx_estimated_absorpt_t_max   0.963
_shelx_estimated_absorpt_t_min   0.963
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
2. Restrained distances
 C7-C6 \\sim C5-C6_$1 \\sim C7_$1-C8
 with sigma of 0.02
 C6-C5 \\sim C6_$1-C7_$1 \\sim C8-C7
 with sigma of 0.02
 C7-C6 \\sim C6-C5
 with sigma of 0.02
 C7_$1-C7 \\sim C7-C5
 with sigma of 0.02
 C8-C6 \\sim C6-C6_$1
 with sigma of 0.02
 C8-C6 \\sim C7-C5
 with sigma of 0.02
3. Restrained planarity
 C7, C6, C5, C6_$1, C7_$1, C8, O4A, C4, O4A_$1
 with sigma of 0.1
4. Rigid body (RIGU) restrains
 O4A, Zr1, O1, O2A, O3A, C1, C4, C2, C3, H3
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 O4A, C4, O4B, C5, C6, C8, C7
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
5. Others
 Fixed Sof: O2A(0.25) O3A(0.08333) O4A(0.5) C4(0.2) O5(0.05556) O6(0.05)
 O3B(0.08333) O2B(0.25) O4B(0.5) C5(0.075) C6(0.05) C8(0.025) C7(0.05)
6.a Aromatic/amide H refined with riding coordinates:
 C3(H3)
;
_olex2_date_sample_data_collection 2017-12-02
_olex2_submission_original_sample_id MOF-808-BZZ
_olex2_submission_special_instructions 'No special instructions were received'