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_7127295
_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_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           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_symmetry_Int_Tables_number      2
_audit_creation_date             2020-04-11
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_audit_update_record
;
2020-07-04 deposited with the CCDC.	2020-09-18 downloaded from the CCDC.
;
_cell_angle_alpha                94.6542(9)
_cell_angle_beta                 108.3216(8)
_cell_angle_gamma                99.0418(9)
_cell_formula_units_Z            2
_cell_length_a                   11.5955(2)
_cell_length_b                   13.3944(2)
_cell_length_c                   13.4286(2)
_cell_measurement_reflns_used    747
_cell_measurement_temperature    100
_cell_measurement_theta_max      25.19
_cell_measurement_theta_min      2.61
_cell_volume                     1936.28(5)
_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      100
_diffrn_measured_fraction_theta_full 0.9973
_diffrn_measured_fraction_theta_max 0.9973
_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  0.0836
_diffrn_reflns_av_unetI/netI     0.0553
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            59394
_diffrn_reflns_theta_full        27.6305
_diffrn_reflns_theta_max         27.63
_diffrn_reflns_theta_min         1.89
_exptl_absorpt_coefficient_mu    0.609
_exptl_absorpt_correction_T_max  0.7456
_exptl_absorpt_correction_T_min  0.7037
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2014/5 (Bruker,2014/5) was used for absorption correction.
wR2(int) was 0.0693 before and 0.0636 after correction.
The Ratio of minimum to maximum transmission is 0.9438.
The \l/2 correction factor is 0.00150.
;
_exptl_crystal_density_diffrn    1.6823
_exptl_crystal_description       block
_exptl_crystal_F_000             994.6544
_exptl_crystal_size_max          0.204
_exptl_crystal_size_mid          0.146
_exptl_crystal_size_min          0.097
_refine_diff_density_max         0.8820
_refine_diff_density_min         -1.0069
_refine_diff_density_rms         0.1499
_refine_ls_d_res_high            0.7663
_refine_ls_d_res_low             10.8006
_refine_ls_goodness_of_fit_ref   1.0508
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_constraints    97
_refine_ls_number_parameters     559
_refine_ls_number_reflns         9001
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.0508
_refine_ls_R_factor_all          0.0651
_refine_ls_R_factor_gt           0.0391
_refine_ls_shift/su_max          0.0386
_refine_ls_shift/su_mean         0.0012
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0240P)^2^+2.0306P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0729
_refine_ls_wR_factor_ref         0.0840
_reflns_Friedel_coverage         0.0
_reflns_limit_h_max              14
_reflns_limit_h_min              -15
_reflns_limit_k_max              17
_reflns_limit_k_min              -17
_reflns_limit_l_max              17
_reflns_limit_l_min              0
_reflns_number_gt                6854
_reflns_number_total             9001
_reflns_threshold_expression     I>=2u(I)
_cod_data_source_file            d0cc04940a2.cif
_cod_data_source_block           distal
_cod_depositor_comments
'Adding full bibliography for 7127294--7127295.cif.'
_cod_database_code               7127295
_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. Shared sites
{C32A, C32B}
3. Uiso/Uaniso restraints and constraints
Uanis(N1A) = Uanis(N2A) = Uanis(N3A) = Uanis(C1A) = Uanis(C2A) = Uanis(C3A) =
Uanis(C4A) = Uanis(C5A) = Uanis(C6A) = Uanis(C7A) = Uanis(C8A) = Uanis(C9A) =
Uanis(C10A) = Uanis(C11A) = Uanis(C12A) = Uanis(C13A) = Uanis(C14A) =
Uanis(C15A)
Uanis(N1B) = Uanis(N2B) = Uanis(N3B) = Uanis(C1B) = Uanis(C2B) = Uanis(C3B) =
Uanis(C4B) = Uanis(C5B) = Uanis(C6B) = Uanis(C7B) = Uanis(C8B) = Uanis(C9B) =
Uanis(C10B) = Uanis(C11B) = Uanis(C12B) = Uanis(C13B) = Uanis(C14B) =
Uanis(C15B)
Uanis(C16A) = Uanis(C17A) = Uanis(O2A)
Uanis(C16B) = Uanis(C17B) = Uanis(O2B)
Uanis(F4A) = Uanis(F5A) = Uanis(F6A) = Uanis(F4B) = Uanis(F5B) = Uanis(F6B)
Uanis(O11A) = Uanis(O11B)
Uanis(S2A) = Uanis(S2B)
Uanis(C32A) = Uanis(C32B)
Uanis(C33A) = Uanis(C33B)
4. Others
 Sof(N1B)=Sof(N2B)=Sof(N3B)=Sof(C1B)=Sof(H1B)=Sof(C2B)=Sof(H2B)=Sof(C3B)=
 Sof(H3B)=Sof(C4B)=Sof(H4B)=Sof(C5B)=Sof(C6B)=Sof(C7B)=Sof(H7B)=Sof(C8B)=
 Sof(C9B)=Sof(H9B)=Sof(C10B)=Sof(C11B)=Sof(C12B)=Sof(H12B)=Sof(C13B)=Sof(H13B)=
 Sof(C14B)=Sof(H14B)=Sof(C15B)=Sof(H15B)=Sof(C16B)=Sof(H16c)=Sof(H16d)=
 Sof(C17B)=Sof(H17d)=Sof(H17e)=Sof(H17f)=Sof(O2B)=Sof(S2B)=Sof(F4B)=Sof(F5B)=
 Sof(F6B)=Sof(O8B)=Sof(O9B)=Sof(O11B)=Sof(C33B)=Sof(H33a)=Sof(H33b)=Sof(H33c)=
 Sof(C35B)=Sof(Ru1B)=Sof(C32B)=Sof(H32c)=Sof(H32d)=1-FVAR(1)
 Sof(Ru1A)=Sof(N1A)=Sof(N2A)=Sof(N3A)=Sof(C1A)=Sof(H1A)=Sof(C2A)=Sof(H2A)=
 Sof(C3A)=Sof(H3A)=Sof(C4A)=Sof(H4A)=Sof(C5A)=Sof(C6A)=Sof(C7A)=Sof(H7A)=
 Sof(C8A)=Sof(C9A)=Sof(H9A)=Sof(C10A)=Sof(C11A)=Sof(C12A)=Sof(H12A)=Sof(C13A)=
 Sof(H13A)=Sof(C14A)=Sof(H14A)=Sof(C15A)=Sof(H15A)=Sof(C16A)=Sof(H16a)=
 Sof(H16b)=Sof(C17A)=Sof(H17a)=Sof(H17b)=Sof(H17c)=Sof(O2A)=Sof(S2A)=Sof(F4A)=
 Sof(F5A)=Sof(F6A)=Sof(O8A)=Sof(O9A)=Sof(O11A)=Sof(C32A)=Sof(H32a)=Sof(H32b)=
 Sof(C33A)=Sof(H33d)=Sof(H33e)=Sof(H33f)=FVAR(1)
5.a Secondary CH2 refined with riding coordinates:
 C16A(H16a,H16b), C16B(H16c,H16d), C32A(H32a,H32b), C32B(H32c,H32d)
5.b Aromatic/amide H refined with riding coordinates:
 C1A(H1A), C2A(H2A), C3A(H3A), C4A(H4A), C7A(H7A), C9A(H9A), C12A(H12A),
 C13A(H13A), C14A(H14A), C15A(H15A), C1B(H1B), C2B(H2B), C3B(H3B), C4B(H4B),
 C7B(H7B), C9B(H9B), C12B(H12B), C13B(H13B), C14B(H14B), C15B(H15B), C30(H30),
 C25(H25), C24(H24), C29(H29), C21(H21), C20(H20), C19(H19), C27(H27), C28(H28)
5.c Idealised Me refined as rotating group:
 C17A(H17a,H17b,H17c), C17B(H17d,H17e,H17f), C33B(H33a,H33b,H33c), C33A(H33d,
 H33e,H33f)
;
_olex2_submission_special_instructions 'No special instructions were received'