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_7048515
_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 O3 P2 S3, B F4, C H2 Cl2'
_chemical_formula_sum            'C43 H34 B Cl2 Cu F4 N2 O3 P2 S3'
_chemical_formula_weight         1006.09
_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             2018-12-12
_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                90
_cell_angle_beta                 93.727(2)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   13.2844(6)
_cell_length_b                   12.9331(6)
_cell_length_c                   25.3545(11)
_cell_measurement_reflns_used    9945
_cell_measurement_temperature    100.15
_cell_measurement_theta_max      30.412
_cell_measurement_theta_min      2.377
_cell_volume                     4346.9(3)
_computing_cell_refinement       'SAINT V8.38A (?, 2016)'
_computing_data_collection       'Bruker APEX2'
_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 0.993
_diffrn_measured_fraction_theta_max 0.954
_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  0.0215
_diffrn_reflns_av_unetI/netI     0.0212
_diffrn_reflns_Laue_measured_fraction_full 0.993
_diffrn_reflns_Laue_measured_fraction_max 0.954
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       33
_diffrn_reflns_limit_l_min       -27
_diffrn_reflns_number            30265
_diffrn_reflns_point_group_measured_fraction_full 0.993
_diffrn_reflns_point_group_measured_fraction_max 0.954
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.999
_diffrn_reflns_theta_min         1.610
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.903
_exptl_absorpt_correction_T_max  0.7461
_exptl_absorpt_correction_T_min  0.6750
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
'SADABS-2016/2 (Bruker,2016/2) was used for absorption correction. wR2(int) was 0.0565 before and 0.0314 after correction. The Ratio of minimum to maximum transmission is 0.9047. The \l/2 correction factor is Not present.'
_exptl_crystal_colour            yellow
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    1.537
_exptl_crystal_description       prism
_exptl_crystal_F_000             2048
_exptl_crystal_size_max          0.409
_exptl_crystal_size_mid          0.208
_exptl_crystal_size_min          0.105
_refine_diff_density_max         0.655
_refine_diff_density_min         -0.501
_refine_diff_density_rms         0.057
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.046
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     560
_refine_ls_number_reflns         10029
_refine_ls_number_restraints     52
_refine_ls_restrained_S_all      1.052
_refine_ls_R_factor_all          0.0306
_refine_ls_R_factor_gt           0.0278
_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^)+(0.0315P)^2^+3.3427P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0701
_refine_ls_wR_factor_ref         0.0716
_reflns_Friedel_coverage         0.000
_reflns_number_gt                9211
_reflns_number_total             10029
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c8dt04588g2.cif
_cod_data_source_block           mw288_p
_cod_depositor_comments
'Adding full bibliography for 7048509--7048517.cif.'
_cod_database_code               7048515
_shelx_shelxl_version_number     2017/1
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
2. Restrained distances
 Cl1-C43 \\sim Cl2-C43
 with sigma of 0.01
 F1-B1 \\sim F2A-B1 \\sim F2-B1 \\sim F3A-B1 \\sim F3-B1 \\sim F4A-B1 \\sim
F4-B1
 with sigma of 0.01
3. Uiso/Uaniso restraints and constraints
F4 \\sim F4A \\sim F3 \\sim F3A \\sim F2 \\sim F2A \\sim F1: within 2A with
sigma of 0.04 and sigma for terminal atoms of 0.08
Uanis(F4A) = Uanis(F4)
Uanis(F2A) = Uanis(F2)
Uanis(F3A) = Uanis(F3)
4. Rigid body (RIGU) restrains
 F3A, F3, F4A, F4, F1, F2A, F2
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
5. Others
 Sof(F2A)=Sof(F4A)=Sof(F3A)=1-FVAR(1)
 Sof(F4)=Sof(F3)=Sof(F2)=FVAR(1)
6.a Secondary CH2 refined with riding coordinates:
 C43(H43A,H43B)
6.b Aromatic/amide H refined with riding coordinates:
 C26(H26), C27(H27), C28(H28), C29(H29), C30(H30), C20(H20), C24(H24),
 C23(H23), C22(H22), C21(H21), C17(H17), C16(H16), C15(H15), C14(H14), C11(H11),
  C10(H10), C9(H9), C8(H8), C42(H42), C41(H41), C40(H40), C39(H39), C38(H38),
 C36(H36), C35(H35), C34(H34), C33(H33), C32(H32), C5(H5), C6(H6), C2(H2),
 C1(H1)
;
_olex2_submission_special_instructions 'No special instructions were received'