Chemical and photochemical water oxidation catalyzed by novel ruthenium complexes comprising a negatively charged NCNHCO ligand
Su, Wei; Younus, Hussein A.; Zhou, Kui; Khattak, Zafar A. K.; Chaemcheun, Somboon; Chen, Cheng; Verpoort, Francis; Catal. Sci. Technol. 7 (2017) 387–; doi:10.1039/C6CY02333A

data_1544776
_publ_section_title
;
 Chemical and photochemical water oxidation catalyzed by novel ruthenium
 complexes comprising a negatively charged NCNHCO ligand
;
_journal_issue                   2
_journal_name_full               'Catal. Sci. Technol.'
_journal_page_first              387
_journal_paper_doi               10.1039/C6CY02333A
_journal_volume                  7
_journal_year                    2017
_chemical_formula_moiety         '2(C19 H23 Cl N4 O3 Ru S), 3(C H2 Cl2)'
_chemical_formula_sum            'C41 H52 Cl8 N8 O6 Ru2 S2'
_chemical_formula_weight         1302.76
_chemical_name_common            RuCl(NCO)(DMSO)(Pic)
_chemical_name_systematic        'Ru WOCs'
_chemical_properties_physical
', Moisture-sensitive,Hygroscopic,Oxygen-sensitive'
_space_group_crystal_system      monoclinic
_space_group_IT_number           15
_space_group_name_Hall           '-C 2yc'
_space_group_name_H-M_alt        'C 1 2/c 1'
_symmetry_space_group_name_Hall  '-C 2yc'
_symmetry_space_group_name_H-M   'C 1 2/c 1'
_atom_sites_solution_hydrogens   geom
_audit_creation_date             2016-09-30
_audit_creation_method
;
Olex2 1.2
(compiled 2016.09.09 svn.r3337 for OlexSys, GUI svn.r5227)
;
_audit_update_record
;
2016-10-02 deposited with the CCDC.
2016-12-12 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 147.193(8)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   31.425(6)
_cell_length_b                   9.0156(18)
_cell_length_c                   34.410(5)
_cell_measurement_reflns_used    9898
_cell_measurement_temperature    297
_cell_measurement_theta_max      29.49
_cell_measurement_theta_min      2.35
_cell_volume                     5282(2)
_computing_cell_refinement       'Bruker SAINT'
_computing_data_collection       'Bruker APEX2'
_computing_data_reduction        'Bruker SAINT'
_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    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      297
_diffrn_measured_fraction_theta_full 0.990
_diffrn_measured_fraction_theta_max 0.991
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0270
_diffrn_reflns_av_unetI/netI     0.0263
_diffrn_reflns_Laue_measured_fraction_full 0.990
_diffrn_reflns_Laue_measured_fraction_max 0.991
_diffrn_reflns_limit_h_max       38
_diffrn_reflns_limit_h_min       -38
_diffrn_reflns_limit_k_max       10
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_l_max       42
_diffrn_reflns_limit_l_min       -42
_diffrn_reflns_number            19249
_diffrn_reflns_point_group_measured_fraction_full 0.990
_diffrn_reflns_point_group_measured_fraction_max 0.991
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         25.997
_diffrn_reflns_theta_min         1.308
_exptl_absorpt_coefficient_mu    1.107
_exptl_absorpt_correction_T_max  0.8974
_exptl_absorpt_correction_T_min  0.8787
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
'SADABS-2008/1 (Bruker,2008) was used for absorption correction.'
_exptl_crystal_colour            yellow
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    1.638
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             2632
_exptl_crystal_size_max          0.12
_exptl_crystal_size_mid          0.1
_exptl_crystal_size_min          0.1
_refine_diff_density_max         1.198
_refine_diff_density_min         -1.320
_refine_diff_density_rms         0.106
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.233
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     306
_refine_ls_number_reflns         5148
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.233
_refine_ls_R_factor_all          0.0683
_refine_ls_R_factor_gt           0.0636
_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^)+(0.0314P)^2^+55.0782P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1487
_refine_ls_wR_factor_ref         0.1517
_reflns_Friedel_coverage         0.000
_reflns_number_gt                4704
_reflns_number_total             5148
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c6cy02333a2.cif
_cod_data_source_block           mo_160912d_0m
_cod_depositor_comments          'Adding full bibliography for 1544776.cif.'
_cod_database_code               1544776
_shelx_estimated_absorpt_t_max   0.897
_shelx_estimated_absorpt_t_min   0.879
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Others
 Fixed Sof: H21A(0.5) H21B(0.5)
3.a Secondary CH2 refined with riding coordinates:
 C4(H4A,H4B), C10(H10A,H10B), C20(H20A,H20B), C21(H21A,H21B)
3.b Aromatic/amide H refined with riding coordinates:
 C2(H2), C3(H3), C6(H6), C7(H7), C8(H8), C9(H9), C14(H14), C15(H15), C17(H17),
 C18(H18)
3.c Idealised Me refined as rotating group:
 C12(H12A,H12B,H12C), C13(H13A,H13B,H13C), C19(H19A,H19B,H19C)
;
_shelx_res_checksum              91237
_shelx_hkl_checksum              3501
_shelx_shelxl_version_number     2014/7
_olex2_submission_special_instructions 'No special instructions were received'