Catalytic water oxidation by an <i>in situ</i> generated ruthenium nitrosyl complex bearing a bipyridine-bis(alkoxide) ligand.
Liu, Yingying; Ng, Siu-Mui; Yiu, Shek-Man; Lau, Tai-Chu; Dalton transactions (Cambridge, England : 2003) 50 (2021) 12316–12323; doi:10.1039/d1dt01918j

data_7708063
_publ_section_title
;
 Catalytic water oxidation by an <i>in situ</i> generated ruthenium
 nitrosyl complex bearing a bipyridine-bis(alkoxide) ligand.
;
_journal_issue                   35
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              12316
_journal_page_last               12323
_journal_paper_doi               10.1039/d1dt01918j
_journal_volume                  50
_journal_year                    2021
_chemical_formula_moiety
'C28 H32 N4 O2 Ru, Ce N6 O18, 2(C2 H3 N), 1[CH3CN]'
_chemical_formula_sum            'C34 H41 Ce N13 O20 Ru'
_chemical_formula_weight         1192.99
_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
_audit_creation_date             2021-07-15
_audit_creation_method
;
Olex2 1.3
(compiled 2020.11.12 svn.r5f609507 for OlexSys, GUI svn.r6272)
;
_audit_update_record
;
2021-07-16 deposited with the CCDC.	2021-07-30 downloaded from the CCDC.
;
_cell_angle_alpha                88.005(2)
_cell_angle_beta                 89.737(3)
_cell_angle_gamma                71.800(3)
_cell_formula_units_Z            2
_cell_length_a                   11.4188(4)
_cell_length_b                   12.6730(4)
_cell_length_c                   16.9821(5)
_cell_measurement_reflns_used    9735
_cell_measurement_temperature    173(2)
_cell_measurement_theta_max      71.6790
_cell_measurement_theta_min      6.8390
_cell_volume                     2333.08(14)
_computing_cell_refinement       'CrysAlisPro, Agilent Technologies'
_computing_data_collection       'CrysAlisPro, Agilent Technologies'
_computing_data_reduction        'CrysAlisPro, Agilent Technologies'
_computing_molecular_graphics    'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL-2016/6 (Sheldrick, 2016)'
_computing_structure_solution    'SHELXT-2014/5 (Sheldrick, 2014)'
_diffrn_ambient_temperature      173.00(14)
_diffrn_detector_area_resol_mean 16.1270
_diffrn_measured_fraction_theta_full 0.993
_diffrn_measured_fraction_theta_max 0.993
_diffrn_measurement_device_type  'Xcalibur, Sapphire3, Gemini ultra'
_diffrn_measurement_method       '\w scans'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54178
_diffrn_reflns_av_R_equivalents  0.0379
_diffrn_reflns_av_unetI/netI     0.0411
_diffrn_reflns_Laue_measured_fraction_full 0.993
_diffrn_reflns_Laue_measured_fraction_max 0.993
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -13
_diffrn_reflns_number            16452
_diffrn_reflns_point_group_measured_fraction_full 0.993
_diffrn_reflns_point_group_measured_fraction_max 0.993
_diffrn_reflns_theta_full        67.679
_diffrn_reflns_theta_max         68.225
_diffrn_reflns_theta_min         3.674
_diffrn_source                   'Enhance Ultra (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    10.854
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.10693
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.35h (release 09-02-2015 CrysAlis171 .NET)
(compiled Feb  9 2015,16:26:32)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            green
_exptl_crystal_density_diffrn    1.698
_exptl_crystal_description       block
_exptl_crystal_F_000             1196
_exptl_crystal_size_max          0.34
_exptl_crystal_size_mid          0.17
_exptl_crystal_size_min          0.02
_refine_diff_density_max         1.659
_refine_diff_density_min         -0.898
_refine_diff_density_rms         0.132
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.075
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     603
_refine_ls_number_reflns         8489
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.075
_refine_ls_R_factor_all          0.0387
_refine_ls_R_factor_gt           0.0378
_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^)+(0.0699P)^2^+1.0580P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1041
_refine_ls_wR_factor_ref         0.1051
_reflns_Friedel_coverage         0.000
_reflns_number_gt                8246
_reflns_number_total             8489
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d1dt01918j2.cif
_cod_data_source_block           051717a_ying
_cod_depositor_comments
'Adding full bibliography for 7708063--7708064.cif.'
_cod_database_code               7708063
_shelx_shelxl_version_number     2016/6
_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:
 C2(H2), C3(H3), C4(H4), C7(H7), C8(H8), C9(H9), C17(H17), C18(H18), C20(H20),
 C21(H21), C23(H23), C24(H24), C26(H26), C27(H27)
2.b Idealised Me refined as rotating group:
 C11(H11A,H11B,H11C), C13(H13A,H13B,H13C), C14(H14A,H14B,H14C), C16(H16A,H16B,
 H16C), C22(H22A,H22B,H22C), C28(H28A,H28B,H28C), C30(H30A,H30B,H30C), C32(H32A,
 H32B,H32C)
;
_smtbx_masks_special_details
;
A solvent mask was calculated and 38 electrons were 
found in a volume of 175\%A^3^ in 2 voids per unit cell. 
This is consistent with the presence of 
1[CH3CN] per Asymmetric Unit 
which account for 44 electrons 
per unit cell.
;
_smtbx_masks_void_probe_radius   1.2
_smtbx_masks_void_truncation_radius 1.2
_shelx_res_checksum              51271
_shelx_fab_checksum              15375
_olex2_submission_special_instructions 'No special instructions were received'