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_4132102
_publ_section_title
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 Electron Injection from Photoexcited Metal-Organic Framework Ligands to
 Ru<sub>2</sub> Secondary Building Units for Visible-Light-Driven Hydrogen
 Evolution.
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_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         'C51 H31 N5 O11 Ru3'
_chemical_formula_sum            'C51 H31 N5 O11 Ru3'
_chemical_formula_weight         1193.02
_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   geom
_atom_sites_solution_primary     direct
_audit_creation_date             2018-02-04
_audit_creation_method
;
Olex2 1.2
(compiled 2016.09.09 svn.r3337 for OlexSys, GUI svn.r5227)
;
_cell_angle_alpha                90.743(2)
_cell_angle_beta                 93.980(3)
_cell_angle_gamma                92.211(3)
_cell_formula_units_Z            2
_cell_length_a                   8.7321(11)
_cell_length_b                   21.947(3)
_cell_length_c                   22.807(3)
_cell_measurement_reflns_used    9879
_cell_measurement_temperature    273(2)
_cell_measurement_theta_max      11.42
_cell_measurement_theta_min      2.23
_cell_volume                     4356.5(10)
_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    'XS (Sheldrick, 2008)'
_diffrn_ambient_temperature      273.15
_diffrn_measured_fraction_theta_full 0.479
_diffrn_measured_fraction_theta_max 0.922
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_wavelength     0.41328
_diffrn_reflns_av_R_equivalents  0.1882
_diffrn_reflns_av_unetI/netI     0.0818
_diffrn_reflns_Laue_measured_fraction_full 0.479
_diffrn_reflns_Laue_measured_fraction_max 0.922
_diffrn_reflns_limit_h_max       8
_diffrn_reflns_limit_h_min       -8
_diffrn_reflns_limit_k_max       21
_diffrn_reflns_limit_k_min       -21
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            47931
_diffrn_reflns_point_group_measured_fraction_full 0.479
_diffrn_reflns_point_group_measured_fraction_max 0.922
_diffrn_reflns_theta_full        14.357
_diffrn_reflns_theta_max         11.500
_diffrn_reflns_theta_min         0.744
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.713
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            purple
_exptl_crystal_density_diffrn    0.909
_exptl_crystal_description       square
_exptl_crystal_F_000             1184
_exptl_crystal_size_max          0.02
_exptl_crystal_size_mid          0.02
_exptl_crystal_size_min          0.005
_refine_diff_density_max         1.832
_refine_diff_density_min         -1.370
_refine_diff_density_rms         0.218
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.864
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     543
_refine_ls_number_reflns         7561
_refine_ls_number_restraints     345
_refine_ls_restrained_S_all      1.937
_refine_ls_R_factor_all          0.1599
_refine_ls_R_factor_gt           0.1478
_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          0.4131
_refine_ls_wR_factor_ref         0.4295
_reflns_Friedel_coverage         0.000
_reflns_number_gt                6127
_reflns_number_total             7561
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ja8b01601_si_003.cif
_cod_data_source_block           rutbp
_cod_original_cell_volume        4356.6(9)
_cod_database_code               4132102
_shelxl_version_number           2013-3
_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
 Ru4-O11
 2.25 with sigma of 0.02
 Ru4-O17
 2.25 with sigma of 0.02
 C48-C0AA
 1.45 with sigma of 0.02
3. Rigid bond restraints
 N4, N7, N9, N10
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
4. Uiso/Uaniso restraints and constraints
N10 \\sim N4 \\sim N9 \\sim N7: within 2A with sigma of 0.04 and sigma for
terminal atoms of 0.08
Uanis(N4) \\sim Ueq, Uanis(N10) \\sim Ueq, Uanis(N7) \\sim Ueq, Uanis(N9) \\sim
Ueq: with sigma of 0.005 and sigma for terminal atoms of 0.01
Uanis(C23) \\sim Ueq, Uanis(C30) \\sim Ueq, Uanis(C32) \\sim Ueq, Uanis(C19)
\\sim Ueq, Uanis(C5) \\sim Ueq, Uanis(C38) \\sim Ueq, Uanis(C31) \\sim Ueq,
Uanis(C37) \\sim Ueq, Uanis(C22) \\sim Ueq, Uanis(C2) \\sim Ueq, Uanis(C33)
\\sim Ueq, Uanis(C49) \\sim Ueq, Uanis(C28) \\sim Ueq, Uanis(C26) \\sim Ueq,
Uanis(C3) \\sim Ueq, Uanis(C34) \\sim Ueq, Uanis(C14) \\sim Ueq, Uanis(C24)
\\sim Ueq, Uanis(C46) \\sim Ueq, Uanis(C18) \\sim Ueq: with sigma of 0.01 and
sigma for terminal atoms of 0.02
Uanis(O12) \\sim Ueq, Uanis(O8) \\sim Ueq: with sigma of 0.005 and sigma for
terminal atoms of 0.01
Uanis(O17) \\sim Ueq, Uanis(C52) \\sim Ueq, Uanis(C61) \\sim Ueq, Uanis(C64)
\\sim Ueq, Uanis(C6) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms
of 0.02
Uanis(O1AA) = Uanis(O7)
Uanis(C3) = Uanis(C21)
Uanis(C15) = Uanis(C5)
Uanis(C1AA) = Uanis(C35)
Uanis(C22) = Uanis(C2) = Uanis(C33) = Uanis(C39)
Uanis(C0AA) = Uanis(C48)
Uanis(O6) = Uanis(O5)
5. Rigid body (RIGU) restrains
 N7, C26, C3, C34, N9
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 C32, C18, C14
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 C60, C56, C29, C52, C47, C41, C45
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 C13, C16, C39, C42, C44, C48
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 C21, C40, C55, C61, C65, C70
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 O1AA, C6, O7
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.02
6.a Aromatic/amide H refined with riding coordinates:
 C13(H13), C16(H16), C42(H42), C44(H44), C40(H40), C55(H55), C65(H65),
 C70(H70), C23(H23), C24(H24), C28(H28), C29(H29), C41(H41), C52(H52), C56(H56),
  C30(H30), C31(H31), C37(H37), C46(H46), C49(H49), C51(H51), C58(H58),
 C64(H64), C76(H76), C7(H7)
6.b Fitted hexagon refined as free rotating group:
 C13(C16,C39,C42,C44,C48), C21(C40,C55,C61,C65,C70), C29(C41,C47,C52,C56,C60)
6.c Idealised Me refined as rotating group:
 C12(H12A,H12B,H12C), C20(H20A,H20B,H20C)
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_shelx_res_checksum              34888
_shelx_hkl_checksum              80169
_shelx_fab_checksum              96940
_olex2_submission_special_instructions 'No special instructions were received'