Pyridazine Based Scorpionate Ligand in a Copper Boratrane Compound
Gernot Nuss; Gerald Saischek; Bastian N. Harum; Manuel Volpe; Ferdinand Belaj; Nadia C. Mösch-Zanetti; Inorganic Chemistry 50 (2011) 12632–12640; doi:10.1021/ic201666w

data_4327124
_publ_contact_author_address
; Institute of Chemistry,
  Karl-Franzens University Graz,
  Schubertstr. 1,
  A-8010 Graz,
  Austria
;
_publ_contact_author_email       ferdinand.belaj@uni-graz.at
_publ_contact_author_fax         43(316)3809835
_publ_contact_author_name        'Ferdinand Belaj'
_publ_contact_author_phone       43(316)3805288
_publ_section_title
;
 Pyridazine Based Scorpionate Ligand in a Copper Boratrane Compound
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              12632
_journal_page_last               12640
_journal_paper_doi               10.1021/ic201666w
_journal_volume                  50
_journal_year                    2011
_chemical_compound_source        'synthetical product'
_chemical_formula_moiety         'C48 H68 B2 Cu2 N12 S6, 3(C H2 Cl2)'
_chemical_formula_sum            'C51 H74 B2 Cl6 Cu2 N12 S6'
_chemical_formula_weight         1408.98
_chemical_name_systematic
; bis(mu2-hydrogen-tris(3-mercapto-6-tert-butyl-pyridazin-2-yl)borato-S,S',
S'')-di-copper(I) dichloromethane solvate (1:3)
;
_space_group_IT_number           15
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-C 2yc'
_symmetry_space_group_name_H-M   'C 1 2/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           'manual edited SHELXL-97 .cif file'
_cell_angle_alpha                90.00
_cell_angle_beta                 107.4795(9)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   16.5494(6)
_cell_length_b                   17.6573(7)
_cell_length_c                   24.1261(9)
_cell_measurement_reflns_used    9018
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      30.65
_cell_measurement_theta_min      2.18
_cell_volume                     6724.5(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-97 (Sheldrick, 2008)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0179
_diffrn_reflns_av_sigmaI/netI    0.0187
_diffrn_reflns_limit_h_max       23
_diffrn_reflns_limit_h_min       -21
_diffrn_reflns_limit_k_max       24
_diffrn_reflns_limit_k_min       -24
_diffrn_reflns_limit_l_max       33
_diffrn_reflns_limit_l_min       -33
_diffrn_reflns_number            32372
_diffrn_reflns_theta_full        30.00
_diffrn_reflns_theta_max         30.00
_diffrn_reflns_theta_min         2.18
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    1.101
_exptl_absorpt_correction_T_max  0.7461
_exptl_absorpt_correction_T_min  0.6434
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'Bruker SADABS'
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    1.392
_exptl_crystal_description       block
_exptl_crystal_F_000             2920
_exptl_crystal_size_max          0.36
_exptl_crystal_size_mid          0.34
_exptl_crystal_size_min          0.30
_refine_diff_density_max         0.693
_refine_diff_density_min         -0.885
_refine_diff_density_rms         0.064
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.023
_refine_ls_hydrogen_treatment    refU
_refine_ls_matrix_type           full
_refine_ls_number_parameters     399
_refine_ls_number_reflns         9765
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.023
_refine_ls_R_factor_all          0.0373
_refine_ls_R_factor_gt           0.0298
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0376P)^2^+10.1785P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0762
_refine_ls_wR_factor_ref         0.0811
_reflns_number_gt                8486
_reflns_number_total             9765
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic201666w_si_001_4.cif
_cod_data_source_block           GN234
_cod_original_sg_symbol_H-M      'C 2/c'
_cod_database_code               4327124