Catalytic water oxidation by a single site [Ru(Fc-tpy)(bpy)OH2]2+ complex and it’s mechanistic study
Vatsa, Aditi; Padhi, Sumanta Kumar; Inorganica Chimica Acta 504 (2020) 119444–; doi:10.1016/j.ica.2020.119444

data_1565262
_publ_section_title
;
 Catalytic water oxidation by a single site [Ru(Fc-tpy)(bpy)OH2]2+ complex
 and it&#x2019;s mechanistic study
;
_journal_name_full               'Inorganica Chimica Acta'
_journal_page_first              119444
_journal_paper_doi               10.1016/j.ica.2020.119444
_journal_volume                  504
_journal_year                    2020
_chemical_formula_moiety         'C35 H27 Cl Fe N5 Ru, F6 P'
_chemical_formula_sum            'C35 H27 Cl F6 Fe N5 P Ru'
_chemical_formula_weight         854.96
_chemical_name_systematic        '[Ru(Fc-tpy)(bpy)Cl](PF6)'
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_symmetry_Int_Tables_number      2
_cell_angle_alpha                76.772(5)
_cell_angle_beta                 85.757(5)
_cell_angle_gamma                77.233(6)
_cell_formula_units_Z            2
_cell_length_a                   10.3905(7)
_cell_length_b                   13.6630(9)
_cell_length_c                   14.4405(8)
_cell_measurement_reflns_used    262
_cell_measurement_temperature    298
_cell_measurement_theta_max      16.9860
_cell_measurement_theta_min      2.8950
_cell_volume                     1945.7(2)
_computing_cell_refinement
;
'CrysAlisPro 1.171.39.29c (Rigaku OD, 2017)'
;
_computing_data_collection
;
'CrysAlisPro 1.171.39.29c (Rigaku OD, 2017)'
;
_computing_data_reduction
;
'CrysAlisPro 1.171.39.29c (Rigaku OD, 2017)'
;
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'olex2.refine (Bourhis et al., 2015)'
_diffrn_ambient_temperature      298.0
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 16.0606
_diffrn_detector_type            EosS2
_diffrn_measured_fraction_theta_full 0.9915
_diffrn_measured_fraction_theta_max 0.9915
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type
'SuperNova, Single source at offset/far, EosS2'
_diffrn_measurement_method       \w-scans
_diffrn_measurement_specimen_support 'Mitegen 50um'
_diffrn_radiation_collimation    0.3
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0000
_diffrn_reflns_av_unetI/netI     0.0819
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_number            6413
_diffrn_reflns_theta_full        26.0000
_diffrn_reflns_theta_max         24.50
_diffrn_reflns_theta_min         2.27
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_current           24.0
_diffrn_source_power             1.2
_diffrn_source_target            Mo
_diffrn_source_type              'SuperNova (Mo) X-ray Source'
_diffrn_source_voltage           50.0
_exptl_absorpt_coefficient_mu    0.930
_exptl_absorpt_correction_T_max  0.862
_exptl_absorpt_correction_T_min  0.830
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.39.29c (Rigaku Oxford Diffraction, 2017)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            'clear dark pink'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   dark
_exptl_crystal_colour_primary    pink
_exptl_crystal_density_diffrn    1.4592
_exptl_crystal_description       block
_exptl_crystal_F_000             855.1271
_exptl_crystal_size_max          0.2
_exptl_crystal_size_mid          0.18
_exptl_crystal_size_min          0.16
_refine_diff_density_max         0.9266
_refine_diff_density_min         -0.6828
_refine_diff_density_rms         0.1369
_refine_ls_d_res_high            0.8570
_refine_ls_d_res_low             8.9562
_refine_ls_goodness_of_fit_ref   0.9278
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_constraints    54
_refine_ls_number_parameters     451
_refine_ls_number_reflns         6413
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.9278
_refine_ls_R_factor_all          0.0984
_refine_ls_R_factor_gt           0.0649
_refine_ls_shift/su_max          0.0000
_refine_ls_shift/su_mean         0.0000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.1095P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1637
_refine_ls_wR_factor_ref         0.1794
_reflns_Friedel_coverage         0.0
_reflns_limit_h_max              12
_reflns_limit_h_min              -12
_reflns_limit_k_max              15
_reflns_limit_k_min              -15
_reflns_limit_l_max              16
_reflns_limit_l_min              0
_reflns_number_gt                4035
_reflns_number_total             6413
_reflns_threshold_expression     I>=2u(I)
_cod_data_source_file            ICA-2020-504-119444.cif
_cod_data_source_block           Rfctpy_2
_cod_database_code               1565262
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
2. Restrained planarity
 F2, F4, F5, F6
 with sigma of 0.1
 F6, F1, F4, F3
 with sigma of 0.1
 F6, F5, F4, F2
 with sigma of 0.1
3.a Aromatic/amide H refined with riding coordinates:
 C12(H12), C9(H9), C13(H13), C14(H14), C27(H27), C7(H7), C15(H15), C30(H30),
 C1(H1), C16(H16), C25(H25), C24(H24), C4(H4), C2(H2), C23(H23), C22(H22),
 C3(H3), C17(H17), C28(H28), C29(H29), C19(H19), C18(H18), C33(H33), C31(H31),
 C35(H35), C34(H34), C32(H32)
;
_olex2_submission_original_sample_id '[Ru(Fc-tpy)(bpy)Cl](PF6)'
_olex2_submission_special_instructions 'No special instructions were received'