Structural evolution of the Ru-bms complex to the real water oxidation catalyst of Ru-bda: the bite angle matters.
Yang, Jing; Liu, Bin; Duan, Lele; Dalton transactions (Cambridge, England : 2003) 49 (2020) 4369–4375; doi:10.1039/c9dt04693c

data_7703624
_publ_section_title
;
 Structural evolution of the Ru-bms complex to the real water oxidation
 catalyst of Ru-bda: the bite angle matters.
;
_journal_issue                   14
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              4369
_journal_page_last               4375
_journal_paper_doi               10.1039/c9dt04693c
_journal_volume                  49
_journal_year                    2020
_chemical_formula_moiety         'C24 H24 N4 O6 Ru S2, 2.5(H2 O)'
_chemical_formula_sum            'C24 H29 N4 O8.5 Ru S2'
_chemical_formula_weight         674.70
_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   mixed
_audit_creation_date             2020-02-25
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_audit_update_record
;
2020-02-25 deposited with the CCDC.	2020-02-26 downloaded from the CCDC.
;
_cell_angle_alpha                109.863(4)
_cell_angle_beta                 110.609(4)
_cell_angle_gamma                100.390(4)
_cell_formula_units_Z            4
_cell_length_a                   14.085(4)
_cell_length_b                   15.200(5)
_cell_length_c                   15.861(5)
_cell_measurement_reflns_used    4818
_cell_measurement_temperature    296(2)
_cell_measurement_theta_max      26.164
_cell_measurement_theta_min      2.180
_cell_volume                     2810.4(15)
_computing_cell_refinement       'SAINT V8.32B (?, 2016)'
_computing_data_collection       'Bruker apex3'
_computing_data_reduction        'SAINT V8.32B (?, 2016)'
_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    'ShelXT (Sheldrick, 2015)'
_diffrn_ambient_temperature      296.15
_diffrn_detector_area_resol_mean 7.9
_diffrn_detector_type            'CMOS area detector'
_diffrn_measured_fraction_theta_full 0.995
_diffrn_measured_fraction_theta_max 0.977
_diffrn_measurement_device       'three-circle diffractometer'
_diffrn_measurement_device_type  'Bruker CMOS area detector'
_diffrn_measurement_method       '\w and \f scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0602
_diffrn_reflns_av_unetI/netI     0.0984
_diffrn_reflns_Laue_measured_fraction_full 0.995
_diffrn_reflns_Laue_measured_fraction_max 0.977
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_h_min       -18
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            25294
_diffrn_reflns_point_group_measured_fraction_full 0.995
_diffrn_reflns_point_group_measured_fraction_max 0.977
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.520
_diffrn_reflns_theta_min         1.612
_exptl_absorpt_coefficient_mu    0.762
_exptl_absorpt_correction_T_max  0.7455
_exptl_absorpt_correction_T_min  0.5668
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
'SADABS-2012/1 (Bruker,2012) was used for absorption correction. wR2(int) was 0.0941 before and 0.0506 after correction. The Ratio of minimum to maximum transmission is 0.7603. The \l/2 correction factor is 0.0015.'
_exptl_crystal_colour            'dull dark black'
_exptl_crystal_colour_lustre     dull
_exptl_crystal_colour_modifier   dark
_exptl_crystal_colour_primary    black
_exptl_crystal_density_diffrn    1.595
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             1380
_exptl_crystal_size_max          0.14
_exptl_crystal_size_mid          0.12
_exptl_crystal_size_min          0.1
_refine_diff_density_max         0.904
_refine_diff_density_min         -1.279
_refine_diff_density_rms         0.124
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.964
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     728
_refine_ls_number_reflns         12640
_refine_ls_number_restraints     13
_refine_ls_restrained_S_all      0.966
_refine_ls_R_factor_all          0.0892
_refine_ls_R_factor_gt           0.0506
_refine_ls_shift/su_max          0.007
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0536P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1072
_refine_ls_wR_factor_ref         0.1214
_reflns_Friedel_coverage         0.000
_reflns_number_gt                8296
_reflns_number_total             12640
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c9dt04693c2.cif
_cod_data_source_block           a
_cod_depositor_comments          'Adding full bibliography for 7703624.cif.'
_cod_original_cell_volume        2810.3(15)
_cod_original_formula_sum        'C24 H29 N4 O8.50 Ru S2'
_cod_database_code               7703624
_shelx_shelxl_version_number     2014/7
_shelx_estimated_absorpt_t_max   0.928
_shelx_estimated_absorpt_t_min   0.901
_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, All O(H,H) groups
2. Uiso/Uaniso restraints and constraints
Uanis(O14) \\sim Ueq, Uanis(O16) \\sim Ueq: with sigma of 0.01 and sigma for
terminal atoms of 0.02
3.a Everything fixed:
 H13A, H13B
3.b Free rotating group:
 O14(H14A,H14B), O15(H15A,H15B), O16(H16A,H16B), O17(H17A,H17B)
3.c Secondary CH2 refined with riding coordinates:
 C65(H65A,H65B), C872(H87A,H87B), C19(H19A,H19B), C20(H20A,H20B)
3.d Aromatic/amide H refined with riding coordinates:
 C62(H62), C63(H63), C64(H64), C66(H66), C67(H67), C69(H69), C70(H70),
 C76(H76), C78(H78), C79(H79), C83(H83), C90(H90), C91(H91), C95(H95), C1(H1),
 C5(H5), C6(H6), C7(H7), C8(H8), C10(H10), C11(H11), C12(H12), C13(H13),
 C14(H14), C16(H16), C17(H17), C21(H21), C40(H40)
3.e Idealised Me refined as rotating group:
 C110(H11A,H11B,H11C), C111(H11D,H11E,H11F), C3(H3A,H3B,H3C), C4(H4A,H4B,H4C)
;
_shelx_res_checksum              4918
_olex2_submission_special_instructions 'No special instructions were received'