A multi-stimuli responsive ruthenium complex for catalytic water oxidation.
Hirahara, Masanari; Goto, Hiroki; Yagi, Masayuki; Umemura, Yasushi; Chemical communications (Cambridge, England) 56 (2020) 12825–12828; doi:10.1039/d0cc04940a

data_7127294
_publ_section_title
;
 A multi-stimuli responsive ruthenium complex for catalytic water
 oxidation.
;
_journal_issue                   84
_journal_name_full               'Chemical communications (Cambridge, England)'
_journal_page_first              12825
_journal_page_last               12828
_journal_paper_doi               10.1039/d0cc04940a
_journal_volume                  56
_journal_year                    2020
_chemical_absolute_configuration unk
_chemical_formula_moiety         'C33 H31 N5 O3 Ru, 2(C F3 O3 S), 2(H2 O)'
_chemical_formula_sum            'C35 H35 F6 N5 O11 Ru S2'
_chemical_formula_weight         980.88
_space_group_crystal_system      triclinic
_space_group_IT_number           1
_space_group_name_Hall           'P 1'
_space_group_name_H-M_alt        'P 1'
_symmetry_Int_Tables_number      1
_audit_creation_date             2020-04-04
_audit_creation_method
;
Olex2 1.2
(compiled 2017.08.10 svn.r3458 for OlexSys, GUI svn.r5381)
;
_audit_update_record
;
2020-07-04 deposited with the CCDC.	2020-09-18 downloaded from the CCDC.
;
_cell_angle_alpha                66.564(5)
_cell_angle_beta                 72.663(5)
_cell_angle_gamma                78.969(5)
_cell_formula_units_Z            2
_cell_length_a                   10.011(4)
_cell_length_b                   13.646(5)
_cell_length_c                   16.369(6)
_cell_measurement_reflns_used    849
_cell_measurement_temperature    100
_cell_measurement_theta_max      23.75
_cell_measurement_theta_min      2.27
_cell_volume                     1951.7(13)
_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)'
_computing_structure_solution    'olex2.solve (Bourhis et al., 2015)'
_diffrn_ambient_temperature      100
_diffrn_measured_fraction_theta_full 0.9863
_diffrn_measured_fraction_theta_max 0.9423
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0510
_diffrn_reflns_av_unetI/netI     0.1562
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            23627
_diffrn_reflns_theta_full        25.0000
_diffrn_reflns_theta_max         27.97
_diffrn_reflns_theta_min         1.40
_exptl_absorpt_coefficient_mu    0.604
_exptl_absorpt_correction_T_max  0.7456
_exptl_absorpt_correction_T_min  0.6786
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2014/5 (Bruker,2014/5) was used for absorption correction.
wR2(int) was 0.0662 before and 0.0580 after correction.
The Ratio of minimum to maximum transmission is 0.9101.
The \l/2 correction factor is 0.00150.
;
_exptl_crystal_density_diffrn    1.6690
_exptl_crystal_description       block
_exptl_crystal_F_000             994.6544
_exptl_crystal_size_max          0.116
_exptl_crystal_size_mid          0.101
_exptl_crystal_size_min          0.056
_refine_diff_density_max         0.9599
_refine_diff_density_min         -1.0281
_refine_diff_density_rms         0.2086
_refine_ls_abs_structure_details
'Flack, H. D. (1983). Acta Cryst. A39, 876-881.'
_refine_ls_abs_structure_Flack   -0.03(2)
_refine_ls_d_res_high            0.7577
_refine_ls_d_res_low             14.5552
_refine_ls_goodness_of_fit_ref   1.0033
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_constraints    134
_refine_ls_number_parameters     954
_refine_ls_number_reflns         17686
_refine_ls_number_restraints     7
_refine_ls_restrained_S_all      1.0032
_refine_ls_R_factor_all          0.1096
_refine_ls_R_factor_gt           0.0647
_refine_ls_shift/su_max          0.0016
_refine_ls_shift/su_mean         0.0000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0078P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0868
_refine_ls_wR_factor_ref         0.1027
_reflns_Friedel_coverage         0.908
_reflns_limit_h_max              13
_reflns_limit_h_min              -13
_reflns_limit_k_max              17
_reflns_limit_k_min              -17
_reflns_limit_l_max              21
_reflns_limit_l_min              -21
_reflns_number_gt                12270
_reflns_number_total             17686
_reflns_threshold_expression     I>=2u(I)
_cod_data_source_file            d0cc04940a2.cif
_cod_data_source_block           proximal
_cod_depositor_comments
'Adding full bibliography for 7127294--7127295.cif.'
_cod_original_cell_volume        1951.7(12)
_cod_original_sg_symbol_Hall     ' P 1'
_cod_database_code               7127294
_olex2_refinement_description
;
1. Twinned data refinement
 Scales: 1.03(2)
 -0.03(2)
2. 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
3. Restrained distances
 O15-H21b
 2 with sigma of 0.02
 H21b-O21
 0.85 with sigma of 0.02
 H4b-H63
 2.5 with sigma of 0.02
 O4-H4a
 0.85 with sigma of 0.02
4. Uiso/Uaniso restraints and constraints
Uanis(N7) = Uanis(C39) = Uanis(C40) = Uanis(C41) = Uanis(C42) = Uanis(C43)
Uanis(N3) = Uanis(C15) = Uanis(C14) = Uanis(C13) = Uanis(C12) = Uanis(C11)
Uanis(N2) = Uanis(C10) = Uanis(C9) = Uanis(C8) = Uanis(C7) = Uanis(C6)
Uanis(N8) = Uanis(C44) = Uanis(C45) = Uanis(C46) = Uanis(C47) = Uanis(C48)
Uanis(N4) = Uanis(C18) = Uanis(C19) = Uanis(C20) = Uanis(C21) = Uanis(C22)
Uanis(C65B) = Uanis(C66B) = Uanis(C65A) = Uanis(C66A)
5. Others
 Sof(C66B)=Sof(C65B)=Sof(H32c)=Sof(H32d)=Sof(H33d)=Sof(H33e)=Sof(H33f)=
 Sof(H65c)=Sof(H65d)=Sof(H66d)=Sof(H66e)=Sof(H66f)=1-FVAR(1)
 Sof(C65A)=Sof(C66A)=Sof(H32a)=Sof(H32b)=Sof(H33a)=Sof(H33b)=Sof(H33c)=
 Sof(H65a)=Sof(H65b)=Sof(H66a)=Sof(H66b)=Sof(H66c)=FVAR(1)
 Fixed Sof: O23(0.25)
6.a Free rotating group:
 O22(H22a,H22b), O19(H19a,H19b), O20(H20a,H20b), O21(H21a,H21b)
6.b Rotating group:
 O1(H1a,H1b), O4(H4a,H4b)
6.c Secondary CH2 refined with riding coordinates:
 C49(H49a,H49b), C32(H32a,H32b), C16(H16a,H16b), C65B(H65c,H65d), C65A(H65a,
 H65b)
6.d Aromatic/amide H refined with riding coordinates:
 C58(H58), C47(H47), C25(H25), C19(H19), C20(H20), C3(H3), C2(H2), C29(H29),
 C42(H42), C27(H27), C21(H21), C24(H24), C15(H15), C13(H13), C54(H54), C28(H28),
  C4(H4), C57(H57), C35(H35), C48(H48), C12(H12), C62(H62), C63(H63), C1(H1),
 C61(H61), C9(H9), C14(H14), C45(H45), C34(H34), C7(H7), C36(H36), C46(H46),
 C30(H30), C40(H40), C37(H37), C60(H60), C53(H53), C52(H52)
6.e Idealised Me refined as rotating group:
 C17(H17a,H17b,H17c), C33(H33a,H33b,H33c), C50(H50a,H50b,H50c), C66A(H66a,H66b,
 H66c), C66B(H66d,H66e,H66f)
;
_olex2_submission_special_instructions 'No special instructions were received'