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_4327121
_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_formula_moiety         'C33 H49 B Cu N6 P S3, 3 (C H2 Cl2)'
_chemical_formula_sum            'C36 H55 B Cl6 Cu N6 P S3'
_chemical_formula_weight         986.06
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_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
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                75.682(5)
_cell_angle_beta                 74.773(4)
_cell_angle_gamma                78.656(4)
_cell_formula_units_Z            2
_cell_length_a                   11.2357(14)
_cell_length_b                   12.9285(17)
_cell_length_c                   16.999(2)
_cell_measurement_reflns_used    9986
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      29.00
_cell_measurement_theta_min      2.72
_cell_volume                     2285.6(5)
_computing_cell_refinement       'Bruker SAINT'
_computing_data_collection       'Bruker APEX2'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_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 0.981
_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  0.0479
_diffrn_reflns_av_sigmaI/netI    0.0277
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_number            107332
_diffrn_reflns_theta_full        27.50
_diffrn_reflns_theta_max         29.10
_diffrn_reflns_theta_min         1.27
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    1.035
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.3591
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   SADABS
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.433
_exptl_crystal_description       block
_exptl_crystal_F_000             1024
_exptl_crystal_size_max          0.57
_exptl_crystal_size_mid          0.49
_exptl_crystal_size_min          0.37
_refine_diff_density_max         1.780
_refine_diff_density_min         -1.120
_refine_diff_density_rms         0.117
_refine_ls_extinction_coef       0.0124(6)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     SHELXL
_refine_ls_goodness_of_fit_ref   1.085
_refine_ls_hydrogen_treatment    riding
_refine_ls_matrix_type           full
_refine_ls_number_parameters     514
_refine_ls_number_reflns         12055
_refine_ls_number_restraints     4
_refine_ls_restrained_S_all      1.090
_refine_ls_R_factor_all          0.0432
_refine_ls_R_factor_gt           0.0372
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0547P)^2^+2.2589P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0990
_refine_ls_wR_factor_ref         0.1084
_reflns_number_gt                10832
_reflns_number_total             12055
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic201666w_si_001_1.cif
_cod_data_source_block           GN166_cuspcy
_cod_original_cell_volume        2285.5(5)
_cod_database_code               4327121