Post-synthetic exchange (PSE) of UiO-67 frameworks with Ru/Rh half-sandwich units for visible-light-driven H2 evolution and CO2 reduction
Liao, Wei-Ming; Zhang, Jian-Hua; Wang, Zheng; Yin, Shao-Yun; Pan, Mei; Wang, Hai-Ping; Su, Cheng-Yong; Journal of Materials Chemistry A 6 (2018) 11337–; doi:10.1039/C8TA02962H

data_7237143
_publ_section_title
;
 Post-synthetic exchange (PSE) of UiO-67 frameworks with Ru/Rh
 half-sandwich units for visible-light-driven H2 evolution and CO2
 reduction
;
_journal_issue                   24
_journal_name_full               'Journal of Materials Chemistry A'
_journal_page_first              11337
_journal_paper_doi               10.1039/C8TA02962H
_journal_volume                  6
_journal_year                    2018
_chemical_formula_moiety         'C22 H22 Cl N2 O4 Ru, Cl, H2 O'
_chemical_formula_sum            'C22 H24 Cl2 N2 O5 Ru'
_chemical_formula_weight         568.40
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_atom_sites_solution_hydrogens   mixed
_audit_creation_date             2018-03-01
_audit_creation_method
;
Olex2 1.2
(compiled 2016.08.25 svn.r3337 for OlexSys, GUI svn.r5221)
;
_audit_update_record
;
2018-03-21 deposited with the CCDC.
2018-05-21 downloaded from the CCDC.
;
_cell_angle_alpha                91.608(3)
_cell_angle_beta                 95.600(3)
_cell_angle_gamma                90.126(3)
_cell_formula_units_Z            2
_cell_length_a                   8.4046(3)
_cell_length_b                   10.7488(3)
_cell_length_c                   12.1752(4)
_cell_measurement_reflns_used    3352
_cell_measurement_temperature    150.00(10)
_cell_measurement_theta_max      64.7590
_cell_measurement_theta_min      4.0950
_cell_volume                     1094.21(6)
_computing_cell_refinement
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.32 (release 02-08-2013 CrysAlis171 .NET)
(compiled Aug  2 2013,16:46:58)
;
_computing_data_collection
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.32 (release 02-08-2013 CrysAlis171 .NET)
(compiled Aug  2 2013,16:46:58)
;
_computing_data_reduction
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.32 (release 02-08-2013 CrysAlis171 .NET)
(compiled Aug  2 2013,16:46:58)
;
_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      150.00(10)
_diffrn_detector_area_resol_mean 10.6525
_diffrn_measured_fraction_theta_full 0.953
_diffrn_measured_fraction_theta_max 0.953
_diffrn_measurement_details
;
  1 omega  -48.00   36.00   1.0000    1.0000
omega____ theta____ kappa____ phi______ frames
    -      -39.2748   38.0000 -180.0000 84

  2 omega -105.00  -10.00   1.0000    1.0000
omega____ theta____ kappa____ phi______ frames
    -      -39.2748  -57.0000   30.0000 95

  3 omega  -90.00   -2.00   1.0000    1.0000
omega____ theta____ kappa____ phi______ frames
    -      -39.2748  125.0000 -180.0000 88

  4 omega   25.00  108.00   1.0000    1.0000
omega____ theta____ kappa____ phi______ frames
    -       89.7658  -94.0000  -90.0000 83

  5 omega    7.00  108.00   1.0000    1.0000
omega____ theta____ kappa____ phi______ frames
    -       89.7658  -94.0000   30.0000 101

  6 omega   13.00  137.00   1.0000    1.0000
omega____ theta____ kappa____ phi______ frames
    -       89.7658  -15.0000   90.0000 124

  7 omega   30.00   98.00   1.0000    1.0000
omega____ theta____ kappa____ phi______ frames
    -       89.7658  -45.0000 -120.0000 68

  8 omega   62.00  155.00   1.0000    1.0000
omega____ theta____ kappa____ phi______ frames
    -       89.7658   45.0000   90.0000 93

  9 omega   12.00  122.00   1.0000    1.0000
omega____ theta____ kappa____ phi______ frames
    -       89.7658  -77.0000  120.0000 110
;
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at zero, Atlas'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_UB_11      -0.0984493000
_diffrn_orient_matrix_UB_12      -0.0872130000
_diffrn_orient_matrix_UB_13      0.0657986000
_diffrn_orient_matrix_UB_21      0.0349859000
_diffrn_orient_matrix_UB_22      0.0852427000
_diffrn_orient_matrix_UB_23      0.1034221000
_diffrn_orient_matrix_UB_31      -0.1516780000
_diffrn_orient_matrix_UB_32      0.0754061000
_diffrn_orient_matrix_UB_33      -0.0339393000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0263
_diffrn_reflns_av_unetI/netI     0.0305
_diffrn_reflns_Laue_measured_fraction_full 0.953
_diffrn_reflns_Laue_measured_fraction_max 0.953
_diffrn_reflns_limit_h_max       8
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -10
_diffrn_reflns_limit_l_max       10
_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_number            5573
_diffrn_reflns_point_group_measured_fraction_full 0.953
_diffrn_reflns_point_group_measured_fraction_max 0.953
_diffrn_reflns_theta_full        65.042
_diffrn_reflns_theta_max         65.042
_diffrn_reflns_theta_min         4.115
_diffrn_source                   'SuperNova (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    8.379
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.64856
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.32 (release 02-08-2013 CrysAlis171 .NET)
(compiled Aug  2 2013,16:46:58)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            orange
_exptl_crystal_density_diffrn    1.725
_exptl_crystal_description       block
_exptl_crystal_F_000             576
_exptl_crystal_size_max          0.2
_exptl_crystal_size_mid          0.14
_exptl_crystal_size_min          0.10
_refine_diff_density_max         1.057
_refine_diff_density_min         -1.318
_refine_diff_density_rms         0.134
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.022
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     297
_refine_ls_number_reflns         3558
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.022
_refine_ls_R_factor_all          0.0432
_refine_ls_R_factor_gt           0.0418
_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^)+(0.0852P)^2^+2.7624P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1193
_refine_ls_wR_factor_ref         0.1211
_reflns_Friedel_coverage         0.000
_reflns_number_gt                3388
_reflns_number_total             3558
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c8ta02962h2.cif
_cod_data_source_block           H2RuCl
_cod_database_code               7237143
_chemical_oxdiff_formula         'C H N O Ru'
_reflns_odcompleteness_completeness 98.61
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     61.08
_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, All O(H) groups, All O(H,H) groups
2.a Free rotating group:
 O5(H5A,H5B)
2.b Ternary CH refined with riding coordinates:
 C20(H20)
2.c Aromatic/amide H refined with riding coordinates:
 C17(H17), C15(H15), C18(H18), C16(H16), C3(H3), C10(H10), C9(H9), C8(H8),
 C5(H5), C4(H4)
2.d Idealised Me refined as rotating group:
 C22(H22A,H22B,H22C), C21(H21A,H21B,H21C), C13(H13A,H13B,H13C)
2.e Idealised tetrahedral OH refined as rotating group:
 O3(H3A), O1(H1)
;
_shelx_shelxl_version_number     2014/7
_olex2_submission_special_instructions 'No special instructions were received'