Thiopyridazine-Based Copper Boratrane Complexes Demonstrating the Z-type Nature of the Ligand.
Holler, Stefan; Tüchler, Michael; Belaj, Ferdinand; Veiros, Luis F.; Kirchner, Karl; Mösch-Zanetti, Nadia C; Inorganic chemistry 55 (2016) 4980–4991; doi:10.1021/acs.inorgchem.6b00464

data_4347678
_publ_section_title
;
 Thiopyridazine-Based Copper Boratrane Complexes Demonstrating the Z-type
 Nature of the Ligand.
;
_journal_issue                   10
_journal_name_full               'Inorganic chemistry'
_journal_page_first              4980
_journal_page_last               4991
_journal_paper_doi               10.1021/acs.inorgchem.6b00464
_journal_volume                  55
_journal_year                    2016
_chemical_compound_source        'synthetical product'
_chemical_formula_moiety         '2(C27 H39 B Cu N9 S3), C H2 Cl2'
_chemical_formula_sum            'C55 H80 B2 Cl2 Cu2 N18 S6'
_chemical_formula_weight         1405.33
_chemical_name_common
; azido-(2,2',2"-boranetriyl-tris(6-tert-butylpyridazine-3(2H)-thione))-cop-
per(I) dichloromethane solvate (2:1)
;
_chemical_name_systematic
; azido-(2,2',2"-boranetriyl-tris(6-tert-butylpyridazine-3(2H)-thione))-cop-
per(I) dichloromethane solvate (2:1)
;
_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     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           'manual edited SHELXL-2014/6.cif file'
_cell_angle_alpha                90
_cell_angle_beta                 92.2761(14)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   9.8606(4)
_cell_length_b                   19.8005(10)
_cell_length_c                   18.3543(8)
_cell_measurement_reflns_used    7475
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      26.99
_cell_measurement_theta_min      2.53
_cell_volume                     3580.8(3)
_computing_cell_refinement       'Bruker SAINT'
_computing_data_collection       'Bruker APEX2'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    'modified ORTEP (Johnson, 1965)'
_computing_publication_material  'SHELXL-2014/6 (Sheldrick, 2014)'
_computing_structure_refinement  'SHELXL-2014/6 (Sheldrick, 2014)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 0.994
_diffrn_measured_fraction_theta_max 0.994
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_monochromator  'multilayer monochromator'
_diffrn_radiation_source         'Incoatec microfocus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0505
_diffrn_reflns_av_unetI/netI     0.0688
_diffrn_reflns_Laue_measured_fraction_full 0.994
_diffrn_reflns_Laue_measured_fraction_max 0.994
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       -23
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            17400
_diffrn_reflns_point_group_measured_fraction_full 0.994
_diffrn_reflns_point_group_measured_fraction_max 0.994
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         25.00
_diffrn_reflns_theta_min         2.31
_exptl_absorpt_coefficient_mu    0.891
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.694
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
'Bruker (2001). SADABS. Bruker AXS Inc., Madison, Wisconsin, USA.'
_exptl_crystal_colour            orange
_exptl_crystal_density_diffrn    1.303
_exptl_crystal_description       needle
_exptl_crystal_F_000             1468
_exptl_crystal_size_max          0.350
_exptl_crystal_size_mid          0.110
_exptl_crystal_size_min          0.070
_refine_diff_density_max         1.366
_refine_diff_density_min         -0.698
_refine_diff_density_rms         0.094
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.087
_refine_ls_hydrogen_treatment    refU
_refine_ls_matrix_type           full
_refine_ls_number_parameters     420
_refine_ls_number_reflns         6278
_refine_ls_number_restraints     4
_refine_ls_restrained_S_all      1.086
_refine_ls_R_factor_all          0.0844
_refine_ls_R_factor_gt           0.0566
_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^)+(0.0632P)^2^+3.8210P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1330
_refine_ls_wR_factor_ref         0.1429
_reflns_Friedel_coverage         0.000
_reflns_number_gt                4580
_reflns_number_total             6278
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ic6b00464_si_002.cif
_cod_data_source_block           SH180B_6
_cod_original_sg_symbol_H-M      'P 21/c'
_cod_database_code               4347678
_shelx_estimated_absorpt_t_min   0.746
_shelx_estimated_absorpt_t_max   0.940
_shelxl_version_number           2014/6
_shelx_res_checksum              4776
_shelx_hkl_checksum              86295