Efficient molecular ruthenium catalysts containing anionic ligands for water oxidation.
Lu, Zhongkai; Gao, Yan; Chen, Hong; Liu, Zhao; Chen, Lifang; Sun, Licheng; Dalton transactions (Cambridge, England : 2003) 45 (2016) 18459–18464; doi:10.1039/c6dt02056a

data_7039892
_publ_section_title
;
 Efficient molecular ruthenium catalysts containing anionic ligands for
 water oxidation.
;
_journal_issue                   46
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              18459
_journal_page_last               18464
_journal_paper_doi               10.1039/c6dt02056a
_journal_volume                  45
_journal_year                    2016
_chemical_formula_moiety         'C31 H28 N6 O2 Ru, 7(H2 O)'
_chemical_formula_sum            'C31 H42 N6 O9 Ru'
_chemical_formula_weight         743.77
_space_group_crystal_system      monoclinic
_space_group_IT_number           9
_space_group_name_Hall           'C -2yc'
_space_group_name_H-M_alt        'C 1 c 1'
_symmetry_space_group_name_Hall  'C -2yc'
_symmetry_space_group_name_H-M   'C 1 c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_audit_creation_date             2016-07-07
_audit_creation_method
;
Olex2 1.2
(compiled 2016.02.19 svn.r3266 for OlexSys, GUI svn.r5155)
;
_audit_update_record
;
2016-07-08 deposited with the CCDC.
2016-07-11 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 99.017(2)
_cell_angle_gamma                90
_cell_formula_units_Z            12
_cell_length_a                   14.819(2)
_cell_length_b                   25.424(3)
_cell_length_c                   29.317(5)
_cell_measurement_reflns_used    6890
_cell_measurement_temperature    296(2)
_cell_measurement_theta_max      24.41
_cell_measurement_theta_min      3.23
_cell_volume                     10909(3)
_computing_cell_refinement       'CrysAlisPro 1.171.38.41 (Rigaku OD, 2015)'
_computing_data_collection       'CrysAlisPro 1.171.38.41 (Rigaku OD, 2015)'
_computing_data_reduction        'CrysAlisPro 1.171.38.41 (Rigaku OD, 2015)'
_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      296.15
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measurement_device_type  'Saxi goniometer imported SAXI images'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0572
_diffrn_reflns_av_unetI/netI     0.1045
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.997
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       26
_diffrn_reflns_limit_k_min       -30
_diffrn_reflns_limit_l_max       34
_diffrn_reflns_limit_l_min       -34
_diffrn_reflns_number            23177
_diffrn_reflns_point_group_measured_fraction_full 0.997
_diffrn_reflns_point_group_measured_fraction_max 0.997
_diffrn_reflns_theta_full        25.027
_diffrn_reflns_theta_max         25.027
_diffrn_reflns_theta_min         1.602
_diffrn_source                   'Enhance (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    0.488
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.62080
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.35 (release 13-08-2014 CrysAlis171 .NET)
(compiled Aug 13 2014,18:06:01)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            red
_exptl_crystal_colour_primary    red
_exptl_crystal_density_diffrn    1.359
_exptl_crystal_description       plate
_exptl_crystal_F_000             4632
_exptl_crystal_size_max          0.12
_exptl_crystal_size_mid          0.12
_exptl_crystal_size_min          0.08
_refine_diff_density_max         0.584
_refine_diff_density_min         -0.532
_refine_diff_density_rms         0.060
_refine_ls_abs_structure_details
;
 Refined as an inversion twin.
;
_refine_ls_abs_structure_Flack   0.34(5)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.930
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1163
_refine_ls_number_reflns         15693
_refine_ls_number_restraints     1127
_refine_ls_restrained_S_all      0.915
_refine_ls_R_factor_all          0.1035
_refine_ls_R_factor_gt           0.0592
_refine_ls_shift/su_max          0.019
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0610P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1316
_refine_ls_wR_factor_ref         0.1506
_reflns_Friedel_coverage         0.998
_reflns_Friedel_fraction_full    0.997
_reflns_Friedel_fraction_max     0.997
_reflns_number_gt                9189
_reflns_number_total             15693
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c6dt02056a2.cif
_cod_data_source_block           afinal
_cod_depositor_comments          'Adding full bibliography for 7039892.cif.'
_cod_database_code               7039892
_shelx_estimated_absorpt_t_max   0.962
_shelx_estimated_absorpt_t_min   0.944
_olex2_refinement_description
;
1. Twinned data refinement
 Scales: 0.2 0.8
2. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
 At 1.5 times of:
  All C(H,H,H) groups
3. Rigid body (RIGU) restrains
 All non-hydrogen atoms
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
4.a Me refined with riding coordinates:
 C17(H17A,H17B,H17C), C23(H23A,H23B,H23C), C29(H29A,H29B,H29C), C48(H48A,H48B,
 H48C), C54(H54A,H54B,H54C), C60(H60A,H60B,H60C), C79(H79A,H79B,H79C), C85(H85A,
 H85B,H85C), C91(H91A,H91B,H91C)
4.b Aromatic/amide H refined with riding coordinates:
 C3(H3), C4(H4), C5(H5), C9(H9), C10(H10), C11(H11), C12(H12), C14(H14),
 C15(H15), C18(H18), C19(H19), C20(H20), C21(H21), C24(H24), C25(H25), C26(H26),
  C27(H27), C30(H30), C31(H31), C34(H34), C35(H35), C36(H36), C40(H40),
 C41(H41), C42(H42), C43(H43), C45(H45), C46(H46), C49(H49), C50(H50), C51(H51),
  C52(H52), C55(H55), C56(H56), C57(H57), C58(H58), C61(H61), C62(H62),
 C65(H65), C66(H66), C67(H67), C71(H71), C72(H72), C73(H73), C74(H74), C76(H76),
  C77(H77), C80(H80), C81(H81), C82(H82), C83(H83), C86(H86), C87(H87),
 C88(H88), C89(H89), C92(H92), C93(H93)
;
_shelx_res_checksum              11053
_shelx_fab_checksum              75672
_shelx_shelxl_version_number     2014/7
_olex2_submission_special_instructions 'No special instructions were received'
_platon_squeeze_void_probe_radius 1.20