Photocrystallography of [Ru(bpy)2(dmso)2]2+ reveals an O-bonded metastable state
Marr, Zoe Y.; Thapa Magar, Rajani; Fournier, Bertrand; Benedict, Jason B.; Rack, Jeffrey J.; Chemical Science 14 (2023) 7279–7284; doi:10.1039/D3SC01526B

data_1569447
_publ_section_title
;
 Photocrystallography of [Ru(bpy)2(dmso)2]2+ reveals an O-bonded
 metastable state
;
_journal_issue                   26
_journal_name_full               'Chemical Science'
_journal_page_first              7279
_journal_page_last               7284
_journal_paper_doi               10.1039/D3SC01526B
_journal_volume                  14
_journal_year                    2023
_chemical_formula_moiety
'C24 H28 N4 O2 Ru S2, 2(C24 H20 B), 0.758(C2 H3 N)'
_chemical_formula_sum            'C73.51 H70.28 B2 N4.76 O2 Ru S2'
_chemical_formula_weight         1239.21
_chemical_properties_physical    Light-sensitive
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2ybc'
_space_group_name_H-M_alt        'P 1 21/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_audit_creation_date             2022-12-12
_audit_creation_method
;
Olex2 1.5
(compiled 2022.04.07 svn.rca3783a0 for OlexSys, GUI svn.r6498)
;
_audit_update_record
;
2022-12-13 deposited with the CCDC.	2023-06-08 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 119.1730(10)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   22.0479(8)
_cell_length_b                   14.2689(6)
_cell_length_c                   22.3824(9)
_cell_measurement_reflns_used    9896
_cell_measurement_temperature    90
_cell_measurement_theta_max      23.93
_cell_measurement_theta_min      2.31
_cell_volume                     6148.3(4)
_computing_cell_refinement       'SAINT V8.40B (?, 2016)'
_computing_data_reduction        'SAINT V8.40B (?, 2016)'
_computing_molecular_graphics    'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_structure_refinement  'XL  (Sheldrick, 2008)'
_computing_structure_solution    'SHELXT 2018/2 (Sheldrick, 2018)'
_diffrn_ambient_temperature      90
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0602
_diffrn_reflns_av_unetI/netI     0.0386
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_limit_h_max       27
_diffrn_reflns_limit_h_min       -27
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       28
_diffrn_reflns_limit_l_min       -28
_diffrn_reflns_number            108163
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         26.765
_diffrn_reflns_theta_min         1.767
_diffrn_source_current           24.0
_diffrn_source_power             1.2
_diffrn_source_voltage           50.0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.375
_exptl_absorpt_correction_T_max  0.7454
_exptl_absorpt_correction_T_min  0.6765
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2016/2 (Bruker,2016/2) was used for absorption correction.
wR2(int) was 0.1025 before and 0.0581 after correction.
The Ratio of minimum to maximum transmission is 0.9076.
The \l/2 correction factor is Not present.
;
_exptl_crystal_colour            'dark red'
_exptl_crystal_colour_modifier   dark
_exptl_crystal_colour_primary    red
_exptl_crystal_density_diffrn    1.339
_exptl_crystal_description       plate
_exptl_crystal_F_000             2587
_exptl_crystal_size_max          0.14
_exptl_crystal_size_mid          0.14
_exptl_crystal_size_min          0.02
_refine_diff_density_max         0.921
_refine_diff_density_min         -0.539
_refine_diff_density_rms         0.068
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.027
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     868
_refine_ls_number_reflns         13089
_refine_ls_number_restraints     163
_refine_ls_restrained_S_all      1.027
_refine_ls_R_factor_all          0.0583
_refine_ls_R_factor_gt           0.0410
_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^)+(0.0472P)^2^+6.3829P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1018
_refine_ls_wR_factor_ref         0.1091
_reflns_Friedel_coverage         0.000
_reflns_number_gt                10265
_reflns_number_total             13089
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d3sc01526b2.cif
_cod_data_source_block           p21_c_CCDC1
_cod_database_code               1569447
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   0.993
_shelx_estimated_absorpt_t_min   0.949
_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. Restrained distances
 O1A-S1A
 1.5 with sigma of 0.02
3. Uiso/Uaniso restraints and constraints
S2A \\sim O2A \\sim C3 \\sim S2 \\sim O2 \\sim C4A \\sim C4 \\sim C3A: within
2A with sigma of 0.005 and sigma for terminal atoms of 0.01 within 2A
O1A \\sim S1 \\sim O1 \\sim S1A \\sim C1 \\sim C1A \\sim C2 \\sim C2A: within
2A with sigma of 0.01 and sigma for terminal atoms of 0.02 within 2A
4. Others
 Sof(O2A)=Sof(S2A)=Sof(C3A)=Sof(H3AA)=Sof(H3AB)=Sof(H3AC)=Sof(C4A)=Sof(H4AA)=
 Sof(H4AB)=Sof(H4AC)=1-FVAR(1)
 Sof(S2)=Sof(O2)=Sof(C4)=Sof(H4A)=Sof(H4B)=Sof(H4C)=Sof(C3)=Sof(H3A)=Sof(H3B)=
 Sof(H3C)=FVAR(1)
 Sof(O1A)=Sof(S1A)=Sof(C1A)=Sof(H1AA)=Sof(H1AB)=Sof(H1AC)=Sof(C2A)=Sof(H2AA)=
 Sof(H2AB)=Sof(H2AC)=1-FVAR(2)
 Sof(S1)=Sof(O1)=Sof(C2)=Sof(H2A)=Sof(H2B)=Sof(H2C)=Sof(C1)=Sof(H1A)=Sof(H1B)=
 Sof(H1C)=FVAR(2)
 Sof(Ru2)=1-FVAR(3)
 Sof(Ru1)=Sof(C73)=Sof(N5)=Sof(C74)=Sof(H74A)=Sof(H74B)=Sof(H74C)=FVAR(3)
5.a Aromatic/amide H refined with riding coordinates:
 C44(H44), C42(H42), C68(H68), C72(H72), C32(H32), C45(H45), C56(H56),
 C38(H38), C50(H50), C48(H48), C47(H47), C60(H60), C30(H30), C33(H33), C46(H46),
  C51(H51), C57(H57), C13(H13), C39(H39), C40(H40), C66(H66), C63(H63),
 C41(H41), C8(H8), C62(H62), C71(H71), C26(H26), C65(H65), C58(H58), C14(H14),
 C70(H70), C7(H7), C54(H54), C23(H23), C69(H69), C64(H64), C12(H12), C15(H15),
 C52(H52), C11(H11), C59(H59), C5(H5), C53(H53), C29(H29), C22(H22), C24(H24),
 C36(H36), C6(H6), C28(H28), C21(H21), C35(H35), C34(H34), C27(H27), C18(H18),
 C16(H16), C17(H17)
5.b Idealised Me refined as rotating group:
 C4(H4A,H4B,H4C), C2(H2A,H2B,H2C), C1(H1A,H1B,H1C), C3(H3A,H3B,H3C), C74(H74A,
 H74B,H74C), C1A(H1AA,H1AB,H1AC), C2A(H2AA,H2AB,H2AC), C3A(H3AA,H3AB,H3AC),
 C4A(H4AA,H4AB,H4AC)
;
_shelx_res_checksum              90424
_shelx_hkl_checksum              95487
_olex2_submission_special_instructions 'No special instructions were received'