Electron Injection from Photoexcited Metal-Organic Framework Ligands to Ru<sub>2</sub> Secondary Building Units for Visible-Light-Driven Hydrogen Evolution.
Lan, Guangxu; Zhu, Yuan-Yuan; Veroneau, Samuel S.; Xu, Ziwan; Micheroni, Daniel; Lin, Wenbin; Journal of the American Chemical Society 140 (2018) 5326–5329; doi:10.1021/jacs.8b01601

data_4132101
_publ_section_title
;
 Electron Injection from Photoexcited Metal-Organic Framework Ligands to
 Ru<sub>2</sub> Secondary Building Units for Visible-Light-Driven Hydrogen
 Evolution.
;
_journal_issue                   16
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              5326
_journal_page_last               5329
_journal_paper_doi               10.1021/jacs.8b01601
_journal_volume                  140
_journal_year                    2018
_chemical_formula_moiety         'C11 H19 Cl N O9 Ru2'
_chemical_formula_sum            'C11 H19 Cl N O9 Ru2'
_chemical_formula_weight         546.86
_chemical_name_common            Ru-PD
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2yn'
_space_group_name_H-M_alt        'P 1 21/n 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_audit_creation_date             2018-01-24
_audit_creation_method
;
Olex2 1.2
(compiled 2017.08.10 svn.r3458 for OlexSys, GUI svn.r5381)
;
_cell_angle_alpha                90
_cell_angle_beta                 95.2950(10)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   8.1385(2)
_cell_length_b                   11.9075(4)
_cell_length_c                   18.1107(6)
_cell_measurement_reflns_used    9616
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      23.828
_cell_measurement_theta_min      2.342
_cell_volume                     1747.60(9)
_computing_cell_refinement       'SAINT v8.34A (Bruker, 2013)'
_computing_data_collection       '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  'XL (Sheldrick, 2008)'
_computing_structure_solution    'ShelXT (Sheldrick, 2015)'
_diffrn_ambient_temperature      100.15
_diffrn_detector                 'CCD area detector'
_diffrn_detector_type            'Bruker-Nonius APEXII CCD area detector'
_diffrn_measured_fraction_theta_full 0.966
_diffrn_measured_fraction_theta_max 0.959
_diffrn_measurement_device
'Bruker-Nonius APEXII CCD area detector and D8 diffractometer'
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_collimation    '0.2 mm sinlge-pinhole'
_diffrn_radiation_monochromator  'Silicon 111'
_diffrn_radiation_probe          x-ray
_diffrn_radiation_wavelength     0.41328
_diffrn_reflns_av_R_equivalents  0.1142
_diffrn_reflns_av_unetI/netI     0.0368
_diffrn_reflns_Laue_measured_fraction_full 0.966
_diffrn_reflns_Laue_measured_fraction_max 0.959
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_number            47449
_diffrn_reflns_point_group_measured_fraction_full 0.966
_diffrn_reflns_point_group_measured_fraction_max 0.959
_diffrn_reflns_theta_full        14.357
_diffrn_reflns_theta_max         15.566
_diffrn_reflns_theta_min         1.192
_diffrn_source                   synchrotron
_diffrn_source_type              'Bend magnet, Station 11.3.1, ALS, LBNL'
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    2.393
_exptl_absorpt_correction_T_max  0.5047
_exptl_absorpt_correction_T_min  0.4487
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2008/1 (Bruker,2008) was used for absorption correction.
wR2(int) was 0.0911 before and 0.0346 after correction.
The Ratio of minimum to maximum transmission is 0.8557.
The \l/2 correction factor is 0.0015.
;
_exptl_crystal_colour            'dark red'
_exptl_crystal_density_diffrn    2.078
_exptl_crystal_description       cubic
_exptl_crystal_F_000             1076
_exptl_crystal_size_max          0.02
_exptl_crystal_size_mid          0.02
_exptl_crystal_size_min          0.02
_refine_diff_density_max         0.657
_refine_diff_density_min         -1.147
_refine_diff_density_rms         0.156
_refine_ls_extinction_coef       0.084(2)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     'SHELXL-2014/7 (Sheldrick 2014'
_refine_ls_goodness_of_fit_ref   1.106
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     224
_refine_ls_number_reflns         3848
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.106
_refine_ls_R_factor_all          0.0280
_refine_ls_R_factor_gt           0.0279
_refine_ls_shift/su_max          0.004
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0432P)^2^+1.4090P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0743
_refine_ls_wR_factor_ref         0.0744
_reflns_Friedel_coverage         0.000
_reflns_number_gt                3806
_reflns_number_total             3848
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ja8b01601_si_002.cif
_cod_data_source_block           Ru-PD
_cod_database_code               4132101
_shelx_shelxl_version_number     2014/7
_shelx_estimated_absorpt_t_max   0.5047
_shelx_estimated_absorpt_t_min   0.4487
_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.a Aromatic/amide H refined with riding coordinates:
 C9(H9)
2.b Idealised Me refined as rotating group:
 C2(H2A,H2B,H2C), C4(H4A,H4B,H4C), C6(H6A,H6B,H6C), C8(H8A,H8B,H8C), C10(H10A,
 H10B,H10C), C11(H11A,H11B,H11C)
;
_shelx_res_checksum              42204
_shelx_hkl_checksum              67112
_olex2_submission_special_instructions 'No special instructions were received'