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_7048517
_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
'C42 H32 Cu N2 O P2 S3, B F4, 0.17(C H2 Cl2), 0.33(C4 H10 O1)'
_chemical_formula_sum            'C43.49 H35.63 B Cl0.34 Cu F4 N2 O1.33 P2 S3'
_chemical_formula_weight         928.05
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2yn'
_space_group_name_H-M_alt        'P 1 21/n 1'
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 1'
_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                 94.266(2)
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   13.0385(9)
_cell_length_b                   44.590(3)
_cell_length_c                   14.4382(8)
_cell_measurement_reflns_used    9809
_cell_measurement_temperature    100.15
_cell_measurement_theta_max      26.361
_cell_measurement_theta_min      2.406
_cell_volume                     8370.9(9)
_computing_cell_refinement       'SAINT v8.37A (Bruker, 2015)'
_computing_data_reduction        'SAINT v8.37A (Bruker, 2015)'
_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 0.995
_diffrn_measured_fraction_theta_max 0.993
_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  0.0315
_diffrn_reflns_av_unetI/netI     0.0320
_diffrn_reflns_Laue_measured_fraction_full 0.995
_diffrn_reflns_Laue_measured_fraction_max 0.993
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       55
_diffrn_reflns_limit_k_min       -47
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -11
_diffrn_reflns_number            68044
_diffrn_reflns_point_group_measured_fraction_full 0.995
_diffrn_reflns_point_group_measured_fraction_max 0.993
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         26.378
_diffrn_reflns_theta_min         0.913
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.826
_exptl_absorpt_correction_T_max  0.7454
_exptl_absorpt_correction_T_min  0.6499
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
'SADABS-2014/5 (Bruker,2014/5) was used for absorption correction. wR2(int) was 0.1183 before and 0.0450 after correction. The Ratio of minimum to maximum transmission is 0.8719. The \l/2 correction factor is Not present.'
_exptl_crystal_colour            yellow
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    1.473
_exptl_crystal_description       prism
_exptl_crystal_F_000             3800
_exptl_crystal_size_max          0.384
_exptl_crystal_size_mid          0.111
_exptl_crystal_size_min          0.02
_refine_diff_density_max         0.658
_refine_diff_density_min         -0.733
_refine_diff_density_rms         0.060
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.057
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1121
_refine_ls_number_reflns         17006
_refine_ls_number_restraints     3
_refine_ls_restrained_S_all      1.057
_refine_ls_R_factor_all          0.0442
_refine_ls_R_factor_gt           0.0352
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0402P)^2^+5.0842P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0847
_refine_ls_wR_factor_ref         0.0886
_reflns_Friedel_coverage         0.000
_reflns_number_gt                14185
_reflns_number_total             17006
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c8dt04588g2.cif
_cod_data_source_block           mw292_p
_cod_depositor_comments
'Adding full bibliography for 7048509--7048517.cif.'
_cod_database_code               7048517
_shelx_shelxl_version_number     2017/1
_shelx_estimated_absorpt_t_max   0.984
_shelx_estimated_absorpt_t_min   0.742
_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. Restrained distances
 Cl1-C6C \\sim Cl2-C6C
 with sigma of 0.01
 C1C-C2C \\sim C5C-C4C
 with sigma of 0.01
 O1C-C4C \\sim O1C-C2C
 with sigma of 0.01
3. Others
 Sof(O1C)=Sof(C1C)=Sof(H1CA)=Sof(H1CB)=Sof(H1CC)=Sof(C2C)=Sof(H2CA)=Sof(H2CB)=
 Sof(C4C)=Sof(H4CA)=Sof(H4CB)=Sof(C5C)=Sof(H5CA)=Sof(H5CB)=Sof(H5CC)=1-FVAR(1)
 Sof(Cl1)=Sof(Cl2)=Sof(C6C)=Sof(H6CA)=Sof(H6CB)=FVAR(1)
 Sof(F1BB)=Sof(F2BB)=Sof(F3BB)=Sof(F4BB)=1-FVAR(2)
 Sof(F1B)=Sof(F2B)=Sof(F3B)=Sof(F4B)=FVAR(2)
4.a Secondary CH2 refined with riding coordinates:
 C6C(H6CA,H6CB), C2C(H2CA,H2CB), C4C(H4CA,H4CB)
4.b Aromatic/amide H refined with riding coordinates:
 C1A(H1A), C2A(H2A), C5A(H5A), C6A(H6A), C8A(H8A), C9A(H9A), C10A(H10A),
 C11A(H11A), C14A(H14A), C15A(H15A), C16A(H16A), C17A(H17A), C20A(H20A),
 C21A(H21A), C22A(H22A), C23A(H23A), C24A(H24A), C26A(H26A), C27A(H27A),
 C28A(H28A), C29A(H29A), C30A(H30A), C32A(H32A), C33A(H33A), C34A(H34A),
 C35A(H35A), C36A(H36A), C38A(H38A), C39A(H39A), C40A(H40A), C41A(H41A),
 C42A(H42A), C1B(H1B), C2B(H2B), C5B(H5B), C6B(H6B), C8B(H8B), C9B(H9B),
 C10B(H10B), C11B(H11B), C14B(H14B), C15B(H15B), C16B(H16B), C17B(H17B),
 C20B(H20B), C21B(H21B), C22B(H22B), C23B(H23B), C24B(H24B), C26B(H26B),
 C27B(H27B), C28B(H28B), C29B(H29B), C30B(H30B), C32B(H32B), C33B(H33B),
 C34B(H34B), C35B(H35B), C36B(H36B), C38B(H38B), C39B(H39B), C40B(H40B),
 C41B(H41B), C42B(H42B)
4.c Idealised Me refined as rotating group:
 C1C(H1CA,H1CB,H1CC), C5C(H5CA,H5CB,H5CC)
;
_olex2_submission_special_instructions 'No special instructions were received'