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_7048516
_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
'C90.02 H84.06 Cu2 N2 O2 P4 S2, 2.04(B F4), 2(C4 H10 O)'
_chemical_formula_sum            'C98.02 H104.06 B2.04 Cu2 F8.16 N2 O4 P4 S2'
_chemical_formula_weight         1866.30
_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_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_audit_creation_date             2018-12-11
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_audit_update_record
;
2018-12-12 deposited with the CCDC.
2018-12-14 downloaded from the CCDC.
;
_cell_angle_alpha                72.305(4)
_cell_angle_beta                 71.948(4)
_cell_angle_gamma                66.698(4)
_cell_formula_units_Z            1
_cell_length_a                   12.6003(14)
_cell_length_b                   13.8878(15)
_cell_length_c                   15.3231(16)
_cell_measurement_reflns_used    9967
_cell_measurement_temperature    100.15
_cell_measurement_theta_max      28.32
_cell_measurement_theta_min      2.81
_cell_volume                     2290.4(4)
_computing_cell_refinement       'SAINT v8.37A (Bruker, 2015)'
_computing_data_collection       'Bruker APEX2'
_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 0.997
_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  0.0201
_diffrn_reflns_av_unetI/netI     0.0261
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.995
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            30305
_diffrn_reflns_point_group_measured_fraction_full 0.997
_diffrn_reflns_point_group_measured_fraction_max 0.995
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         28.348
_diffrn_reflns_theta_min         1.933
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.649
_exptl_absorpt_correction_T_max  0.7457
_exptl_absorpt_correction_T_min  0.6955
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
'SADABS-2014/5 (Bruker,2014/5) was used for absorption correction. wR2(int) was 0.0867 before and 0.0333 after correction. The Ratio of minimum to maximum transmission is 0.9327. The \l/2 correction factor is Not present.'
_exptl_crystal_colour            yellow
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    1.353
_exptl_crystal_description       prism
_exptl_crystal_F_000             972
_exptl_crystal_size_max          0.306
_exptl_crystal_size_mid          0.257
_exptl_crystal_size_min          0.234
_refine_diff_density_max         0.619
_refine_diff_density_min         -0.724
_refine_diff_density_rms         0.062
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.058
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     696
_refine_ls_number_reflns         11409
_refine_ls_number_restraints     794
_refine_ls_restrained_S_all      1.040
_refine_ls_R_factor_all          0.0463
_refine_ls_R_factor_gt           0.0388
_refine_ls_shift/su_max          0.003
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0586P)^2^+1.1968P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1049
_refine_ls_wR_factor_ref         0.1110
_reflns_Friedel_coverage         0.000
_reflns_number_gt                9784
_reflns_number_total             11409
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c8dt04588g2.cif
_cod_data_source_block           mw297_p
_cod_depositor_comments
'Adding full bibliography for 7048509--7048517.cif.'
_cod_database_code               7048516
_shelx_shelxl_version_number     2017/1
_olex2_refinement_description
;
1. Shared sites
{H7BC, H7AA}
2. Others
 Fixed Uiso: H2(0.057) H4A(0.043) H4B(0.043) H5A(0.046) H5B(0.046) H6A(0.053)
 H6B(0.053) H7BC(0.078) H7BD(0.078) H7AA(0.078) H7AB(0.078) H7CE(0.078)
 H7CF(0.078) H8AA(0.072) H8AB(0.072) H9AA(0.17) H9AB(0.17) H9AC(0.17)
 H11(0.039) H12(0.046) H13(0.047) H14(0.039) H17(0.03) H18(0.032) H19(0.031)
 H20(0.028) H23(0.033) H24(0.041) H25(0.044) H26(0.046) H27(0.039) H29(0.038)
 H30(0.046) H31(0.049) H32(0.045) H33(0.035) H35(0.037) H36(0.047) H37(0.048)
 H38(0.044) H39(0.035) H41(0.053) H42(0.064) H43(0.066) H44(0.06) H45(0.046)
 H8A(0.072) H8B(0.072) H8BA(0.09) H8BB(0.09) H9A(0.134) H9B(0.134) H9C(0.134)
 H9BA(0.105) H9BB(0.105) H9BC(0.105) H48A(0.049) H48B(0.049) H47A(0.065)
 H47B(0.065) H46A(0.089) H46B(0.089) H46C(0.089) H49A(0.135) H49B(0.135)
 H49C(0.135) H48C(0.049) H48D(0.049) H46D(0.089) H46E(0.089) H46F(0.089)
 H47C(0.065) H47D(0.065) H49D(0.135) H49E(0.135) H49F(0.135)
 Fixed X: H2(0.838036) H4A(1.064415) H4B(1.014487) H5A(0.822254) H5B(0.880787)
 H6A(0.947165) H6B(0.998035) H7BC(0.761269) H7BD(0.803803) H7AA(0.756143)
 H7AB(0.812002) H7CE(0.753963) H7CF(0.832392) H8AA(0.932047) H8AB(0.792461)
 H9AA(0.880733) H9AB(0.89985) H9AC(0.768771) H11(1.469712) H12(1.488205)
 H13(1.377437) H14(1.250301) H17(1.379849) H18(1.436049) H19(1.338703)
 H20(1.185885) H23(1.011284) H24(0.838825) H25(0.670241) H26(0.672843)
 H27(0.845884) H29(1.194333) H30(1.161623) H31(0.998172) H32(0.868386)
 H33(0.901233) H35(1.536117) H36(1.664537) H37(1.645578) H38(1.499143)
 H39(1.368395) H41(1.222535) H42(1.256001) H43(1.418169) H44(1.547678)
 H45(1.518441) H8A(0.89965) H8B(0.94366) H8BA(0.738526) H8BB(0.833979)
 H9A(0.791161) H9B(0.701683) H9C(0.748656) H9BA(0.906999) H9BB(0.901103)
 H9BC(0.992117) H48A(1.40051) H48B(1.425805) H47A(1.32592) H47B(1.291843)
 H46A(1.090991) H46B(1.122869) H46C(1.149555) H49A(1.429688) H49B(1.324552)
 H49C(1.296164) H48C(1.254624) H48D(1.37965) H46D(1.149794) H46E(1.141893)
 H46F(1.134384) H47C(1.329568) H47D(1.328738) H49D(1.47409) H49E(1.345559)
 H49F(1.397909)
 Fixed Y: H2(0.276323) H4A(0.165983) H4B(0.255354) H5A(0.239226) H5B(0.141939)
 H6A(0.138991) H6B(0.040868) H7BC(0.122781) H7BD(0.032284) H7AA(0.120838)
 H7AB(0.018159) H7CE(0.119508) H7CF(0.002657) H8AA(-0.081744) H8AB(-0.06165)
 H9AA(-0.024283) H9AB(0.075503) H9AC(0.073504) H11(0.085484) H12(-0.089471)
 H13(-0.122635) H14(0.020779) H17(0.126612) H18(0.203492) H19(0.382605)
 H20(0.487693) H23(0.324168) H24(0.285234) H25(0.358989) H26(0.471218)
 H27(0.507642) H29(0.599079) H30(0.778626) H31(0.875227) H32(0.791695)
 H33(0.611287) H35(0.181156) H36(0.236049) H37(0.415946) H38(0.543775)
 H39(0.490794) H41(0.261003) H42(0.270149) H43(0.313653) H44(0.346782)
 H45(0.33301) H8A(0.031044) H8B(-0.073697) H8BA(0.012766) H8BB(0.064176) H9A(-
 0.085399) H9B(0.02205) H9C(-0.084736) H9BA(-0.130577) H9BB(-0.137582) H9BC(-
 0.088176) H48A(-0.077031) H48B(0.009375) H47A(-0.044448) H47B(-0.127143) H46A(-
 0.030298) H46B(0.055774) H46C(-0.064071) H49A(0.061371) H49B(0.148537)
 H49C(0.063623) H48C(0.012151) H48D(-0.083357) H46D(0.037253) H46E(0.051645)
 H46F(-0.055927) H47C(-0.048313) H47D(-0.125257) H49D(0.051165) H49E(0.137763)
 H49F(0.043041)
 Fixed Z: H2(0.605576) H4A(0.453433) H4B(0.368062) H5A(0.441668) H5B(0.519262)
 H6A(0.323677) H6B(0.403845) H7BC(0.38148) H7BD(0.468478) H7AA(0.388872)
 H7AB(0.464937) H7CE(0.415264) H7CF(0.457555) H8AA(0.351811) H8AB(0.374288)
 H9AA(0.206144) H9AB(0.222811) H9AC(0.239899) H11(0.426158) H12(0.431803)
 H13(0.354167) H14(0.267067) H17(0.115449) H18(-0.0428) H19(-0.102146) H20(-
 0.002723) H23(0.116145) H24(0.140114) H25(0.247958) H26(0.333055)
 H27(0.312095) H29(0.164388) H30(0.090781) H31(0.022434) H32(0.025739)
 H33(0.098319) H35(0.212614) H36(0.075919) H37(0.021374) H38(0.103841)
 H39(0.238302) H41(0.530734) H42(0.669251) H43(0.664179) H44(0.522556)
 H45(0.383487) H8A(0.263875) H8B(0.342811) H8BA(0.335024) H8BB(0.260409)
 H9A(0.285787) H9B(0.320524) H9C(0.395509) H9BA(0.283596) H9BB(0.391101)
 H9BC(0.309531) H48A(-0.072702) H48B(-0.039306) H47A(0.111194) H47B(0.079875)
 H46A(0.12193) H46B(0.149513) H46C(0.210381) H49A(-0.202647) H49B(-0.148847)
 H49C(-0.181122) H48C(-0.075029) H48D(-0.080427) H46D(0.039046) H46E(0.140854)
 H46F(0.129009) H47C(0.140388) H47D(0.080806) H49D(-0.155548) H49E(-0.161443)
 H49F(-0.21776)
;
_olex2_submission_special_instructions 'No special instructions were received'