Variable oxidation state sulfur-bridged bithiazole ligands tune the electronic properties of ruthenium(ii) and copper(i) complexes.
Caron, Elise; Brown, Christopher M.; Hean, Duane; Wolf, Michael O.; Dalton transactions (Cambridge, England : 2003) 48 (2019) 1263–1274; doi:10.1039/c8dt04588g

data_7048514
_publ_section_title
;
 Variable oxidation state sulfur-bridged bithiazole ligands tune the
 electronic properties of ruthenium(ii) and copper(i) complexes.
;
_journal_issue                   4
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              1263
_journal_page_last               1274
_journal_paper_doi               10.1039/c8dt04588g
_journal_volume                  48
_journal_year                    2019
_chemical_formula_moiety         'C30 H20 N6 O2 Ru S3, 2.03(F6 P)'
_chemical_formula_sum            'C30 H20 F12.2 N6 O2 P2 Ru S3'
_chemical_formula_weight         987.46
_space_group_crystal_system      orthorhombic
_space_group_IT_number           61
_space_group_name_Hall           '-P 2ac 2ab'
_space_group_name_H-M_alt        'P b c a'
_symmetry_space_group_name_Hall  '-P 2ac 2ab'
_symmetry_space_group_name_H-M   'P b c a'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_audit_creation_date             2018-08-04
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_audit_update_record
;
2018-08-20 deposited with the CCDC.
2018-12-14 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   12.8317(8)
_cell_length_b                   15.2760(10)
_cell_length_c                   36.552(2)
_cell_measurement_reflns_used    9996
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      26.53
_cell_measurement_theta_min      2.66
_cell_volume                     7164.8(8)
_computing_cell_refinement       'SAINT V8.38A (?, 2016)'
_computing_data_reduction        'SAINT V8.38A (?, 2016)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_computing_structure_solution    'ShelXS (Sheldrick, 2008)'
_diffrn_ambient_temperature      100.15
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.995
_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  0.0390
_diffrn_reflns_av_unetI/netI     0.0413
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.995
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       41
_diffrn_reflns_limit_l_min       -45
_diffrn_reflns_number            31751
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.995
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         26.547
_diffrn_reflns_theta_min         1.939
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.807
_exptl_absorpt_correction_T_max  0.7454
_exptl_absorpt_correction_T_min  0.6581
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
'SADABS-2016/2 (Bruker,2016/2) was used for absorption correction. wR2(int) was 0.0745 before and 0.0534 after correction. The Ratio of minimum to maximum transmission is 0.8829. The \l/2 correction factor is Not present.'
_exptl_crystal_colour            orange
_exptl_crystal_colour_primary    orange
_exptl_crystal_density_diffrn    1.831
_exptl_crystal_description       plate
_exptl_crystal_F_000             3918
_exptl_crystal_size_max          0.123
_exptl_crystal_size_mid          0.101
_exptl_crystal_size_min          0.05
_refine_diff_density_max         1.118
_refine_diff_density_min         -0.499
_refine_diff_density_rms         0.107
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.122
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     569
_refine_ls_number_reflns         7421
_refine_ls_number_restraints     912
_refine_ls_restrained_S_all      1.065
_refine_ls_R_factor_all          0.0700
_refine_ls_R_factor_gt           0.0588
_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^)+(0.0379P)^2^+35.6317P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1358
_refine_ls_wR_factor_ref         0.1410
_reflns_Friedel_coverage         0.000
_reflns_number_gt                6240
_reflns_number_total             7421
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c8dt04588g2.cif
_cod_data_source_block           mw306_p_a
_cod_depositor_comments
'Adding full bibliography for 7048509--7048517.cif.'
_cod_original_cell_volume        7164.9(8)
_cod_original_formula_sum        'C30 H20 F12.20 N6 O2 P2 Ru S3'
_cod_database_code               7048514
_shelx_shelxl_version_number     2017/1
_shelx_estimated_absorpt_t_max   0.961
_shelx_estimated_absorpt_t_min   0.907
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
2. Restrained distances
 P2-F7 \\sim P2-F8 \\sim P2-F9 \\sim P2-F10 \\sim P2-F11 \\sim P2-F12
 with sigma of 0.01
 P2A-F8A \\sim P2A-F10A \\sim P2A-F11A \\sim P2A-F12A \\sim P2-F8
 with sigma of 0.01
 P2-F11 \\sim P2A-F11A \\sim P2A-F12A \\sim P2A-F10A \\sim P2-F10 \\sim P2A-F7A
\\sim P2-F9 \\sim P2A-F9A
 \\sim P2A-F8A \\sim P2-F8 \\sim P2-F7 \\sim P2-F12
 with sigma of 0.01
3. Uiso/Uaniso restraints and constraints
F7 \\sim P2 \\sim F9 \\sim F10 \\sim F8 \\sim F12 \\sim F11 \\sim P2A \\sim F8A
\\sim F9A \\sim F10A \\sim F11A \\sim F12A \\sim F7A: within 2A with sigma of
0.04 and sigma for terminal atoms of 0.08
4. Rigid body (RIGU) restrains
 All non-hydrogen atoms
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
5. Others
 Sof(P2A)=Sof(F10A)=Sof(F11A)=Sof(F12A)=Sof(F8A)=Sof(F7A)=Sof(F9A)=1-FVAR(1)
 Sof(P2)=Sof(F10)=Sof(F8)=Sof(F12)=Sof(F11)=FVAR(1)
 Fixed Sof: F7(0.75) F9(0.75)
6.a Aromatic/amide H refined with riding coordinates:
 C24(H24), C28(H28), C1(H1), C7(H7), C23(H23), C19(H19), C26(H26), C27(H27),
 C6(H6), C9(H9), C20(H20), C21(H21), C11(H11), C2(H2), C5(H5), C16(H16),
 C15(H15), C8(H8), C12(H12), C14(H14)
;
_olex2_submission_special_instructions 'No special instructions were received'