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_4347673
_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         'C60 H93 B2 K2 N15 O2 S6, C2 H3 N'
_chemical_formula_sum            'C62 H96 B2 K2 N16 O2 S6'
_chemical_formula_weight         1389.72
_chemical_name_common
; catena-{tri-acetonitrile-di(mu2-aqua)-bis[mu2-hydrido-2,2',2''-boranetri-
yltris(6-tert-butylpyridazine-3(2H)-thione)]-di-potassium} acetonitrile
solvate (1:1)
;
_chemical_name_systematic
; catena-{tri-acetonitrile-di(mu2-aqua)-bis[mu2-hydrido-2,2',2''-boranetri-
yltris(6-tert-butylpyridazine-3(2H)-thione)]-di-potassium} acetonitrile
solvate (1:1)
;
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           'manual edited SHELXL-2014/6.cif file'
_cell_angle_alpha                73.3783(16)
_cell_angle_beta                 79.7478(14)
_cell_angle_gamma                74.8793(17)
_cell_formula_units_Z            2
_cell_length_a                   10.1685(5)
_cell_length_b                   19.1118(11)
_cell_length_c                   21.4271(11)
_cell_measurement_reflns_used    9722
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      30.63
_cell_measurement_theta_min      2.55
_cell_volume                     3827.8(4)
_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 0.999
_diffrn_measured_fraction_theta_max 0.999
_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  0.0537
_diffrn_reflns_av_unetI/netI     0.0464
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       23
_diffrn_reflns_limit_k_min       -23
_diffrn_reflns_limit_l_max       26
_diffrn_reflns_limit_l_min       -26
_diffrn_reflns_number            68243
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_theta_full        26.00
_diffrn_reflns_theta_max         26.00
_diffrn_reflns_theta_min         2.41
_exptl_absorpt_coefficient_mu    0.337
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.822
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
'Bruker (2001). SADABS. Bruker AXS Inc., Madison, Wisconsin, USA.'
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.206
_exptl_crystal_description       board
_exptl_crystal_F_000             1480
_exptl_crystal_size_max          0.360
_exptl_crystal_size_mid          0.280
_exptl_crystal_size_min          0.050
_refine_diff_density_max         0.712
_refine_diff_density_min         -0.323
_refine_diff_density_rms         0.056
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.032
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     893
_refine_ls_number_reflns         15041
_refine_ls_number_restraints     4
_refine_ls_restrained_S_all      1.032
_refine_ls_R_factor_all          0.0570
_refine_ls_R_factor_gt           0.0389
_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^)+(0.0440P)^2^+1.5864P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0909
_refine_ls_wR_factor_ref         0.0985
_reflns_Friedel_coverage         0.000
_reflns_number_gt                11791
_reflns_number_total             15041
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ic6b00464_si_002.cif
_cod_data_source_block           SHA7_KTn
_cod_database_code               4347673
_shelx_estimated_absorpt_t_min   0.888
_shelx_estimated_absorpt_t_max   0.983
_shelxl_version_number           2014/6
_shelx_res_checksum              28954
_shelx_hkl_checksum              64519