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_1569448
_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 H27.844 N4 O1.974 Ru S1.974, 2(C24 H20 B), 0.751(C2 H3 N), 0.026(O S)'
_chemical_formula_sum            'C73.5 H70.1 B2 N4.75 O2 Ru S2'
_chemical_formula_weight         1238.78
_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                 119.2530(10)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   22.0415(9)
_cell_length_b                   14.2574(6)
_cell_length_c                   22.4105(9)
_cell_measurement_reflns_used    9892
_cell_measurement_temperature    90
_cell_measurement_theta_max      24.49
_cell_measurement_theta_min      2.31
_cell_volume                     6144.5(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 1.000
_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  0.0571
_diffrn_reflns_av_unetI/netI     0.0345
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 1.000
_diffrn_reflns_limit_h_max       29
_diffrn_reflns_limit_h_min       -29
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       29
_diffrn_reflns_limit_l_min       -29
_diffrn_reflns_number            120670
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 1.000
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         28.102
_diffrn_reflns_theta_min         1.059
_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  0.7457
_exptl_absorpt_correction_T_min  0.6966
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2016/2 (Bruker,2016/2) was used for absorption correction.
wR2(int) was 0.0957 before and 0.0514 after correction.
The Ratio of minimum to maximum transmission is 0.9342.
The \l/2 correction factor is Not present.
;
_exptl_crystal_colour            'light orange'
_exptl_crystal_colour_modifier   light
_exptl_crystal_colour_primary    orange
_exptl_crystal_density_diffrn    1.339
_exptl_crystal_description       plate
_exptl_crystal_F_000             2585
_exptl_crystal_size_max          0.14
_exptl_crystal_size_mid          0.14
_exptl_crystal_size_min          0.02
_refine_diff_density_max         1.168
_refine_diff_density_min         -0.666
_refine_diff_density_rms         0.076
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.051
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     800
_refine_ls_number_reflns         14979
_refine_ls_number_restraints     103
_refine_ls_restrained_S_all      1.059
_refine_ls_R_factor_all          0.0566
_refine_ls_R_factor_gt           0.0413
_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^)+(0.0397P)^2^+7.9467P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0975
_refine_ls_wR_factor_ref         0.1046
_reflns_Friedel_coverage         0.000
_reflns_number_gt                12119
_reflns_number_total             14979
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d3sc01526b2.cif
_cod_data_source_block           p21_c_CCDC2
_cod_original_formula_sum        'C73.50 H70.10 B2 N4.75 O2 Ru S2'
_cod_database_code               1569448
_shelx_shelxl_version_number     2018/3
_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
 O3-S3
 1.5 with sigma of 0.02
3. Uiso/Uaniso restraints and constraints
S1 \\sim O1 \\sim C1 \\sim H1A \\sim H1B \\sim H1C \\sim C2 \\sim H2A \\sim H2B
\\sim H2C \\sim O3 \\sim S3: within 2A with sigma of 0.005 and sigma for
terminal atoms of 0.01 within 2A
4. Others
 Sof(O3)=Sof(S3)=1-FVAR(1)
 Sof(S1)=Sof(O1)=Sof(H1A)=Sof(H1B)=Sof(H1C)=Sof(H2A)=Sof(H2B)=Sof(H2C)=FVAR(1)
 Sof(C26)=Sof(N5)=Sof(C25)=Sof(H25A)=Sof(H25B)=Sof(H25C)=FVAR(2)
5.a Aromatic/amide H refined with riding coordinates:
 C00C(H00C), C00E(H00E), C00G(H00G), C00H(H00H), C13(H13), C00N(H00N),
 C00O(H00O), C00Q(H00Q), C00R(H00R), C00S(H00S), C00T(H00T), C00U(H00U),
 C00V(H00V), C00W(H00W), C00X(H00X), C00Y(H00Y), C00Z(H00Z), C010(H010), C8(H8),
  C012(H012), C013(H013), C015(H015), C016(H016), C018(H018), C019(H019),
 C01A(H01A), C01B(H01B), C01C(H01C), C24(H24), C5(H5), C01G(H01G), C7(H7),
 C23(H23), C01J(H01J), C01K(H01K), C01L(H01L), C01M(H01M), C14(H14), C15(H15),
 C12(H12), C01Q(H01Q), C11(H11), C01S(H01S), C01T(H01T), C01U(H01U), C01W(H01W),
  C01X(H01X), C22(H22), C01Z(H01Z), C6(H6), C21(H21), C024(H024), C026(H026),
 C18(H18), C17(H17), C16(H16)
5.b Idealised Me refined as rotating group:
 C4(H4A,H4B,H4C), C1(H1A,H1B,H1C), C3(H3A,H3B,H3C), C2(H2A,H2B,H2C), C25(H25A,
 H25B,H25C)
;
_shelx_res_checksum              10569
_shelx_hkl_checksum              15264
_olex2_submission_special_instructions 'No special instructions were received'