Direct Synthesis of a Bis(pyrazolyl)boratocopper(I) Complex: Synthesis and Characterization of [H2B(3,5-(CF3)2Pz)2]Cu(PPh3)2 Displaying an Unusual Coordination Mode for a Poly(pyrazolyl)borate Ligand
H. V. Rasika Dias; Hui-Ling Lu; Inorganic Chemistry 39 (2000) 2246–2248; doi:10.1021/ic991385t

data_4320960
_publ_section_title
;
 Direct Synthesis of a Bis(pyrazolyl)boratocopper(I) Complex: Synthesis
 and Characterization of [H2B(3,5-(CF3)2Pz)2]Cu(PPh3)2 Displaying an
 Unusual Coordination Mode for a Poly(pyrazolyl)borate Ligand
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              2246
_journal_page_last               2248
_journal_paper_doi               10.1021/ic991385t
_journal_volume                  39
_journal_year                    2000
_chemical_formula_sum            'C49 H41 B Cu F12 N4 P2'
_chemical_formula_weight         1050.15
_chemical_name_common            '[(CF3)2Bp]Cu(PPh3)2.0.5(hexane)'
_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                80.288(8)
_cell_angle_beta                 82.151(9)
_cell_angle_gamma                75.677(8)
_cell_formula_units_Z            2
_cell_length_a                   13.4865(19)
_cell_length_b                   13.6724(12)
_cell_length_c                   13.9087(14)
_cell_measurement_reflns_used    39
_cell_measurement_temperature    183(2)
_cell_measurement_theta_max      12.52
_cell_measurement_theta_min      4.65
_cell_volume                     2437.2(5)
_computing_cell_refinement       'Bruker XSCANS'
_computing_data_collection       'Bruker XSCANS'
_computing_data_reduction        'Bruker SHELXTL'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      183(2)
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device_type  'Bruker P4'
_diffrn_measurement_method       '\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  0.0193
_diffrn_reflns_av_sigmaI/netI    0.0326
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -1
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       14
_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_number            7326
_diffrn_reflns_theta_full        22.50
_diffrn_reflns_theta_max         22.50
_diffrn_reflns_theta_min         1.94
_diffrn_standards_decay_%        12.49
_diffrn_standards_interval_count 97
_diffrn_standards_number         3
_exptl_absorpt_coefficient_mu    0.598
_exptl_absorpt_correction_T_max  1.0000
_exptl_absorpt_correction_T_min  0.8709
_exptl_absorpt_correction_type   empirical
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.431
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       Parallelpipeds
_exptl_crystal_F_000             1070
_exptl_crystal_size_max          0.51
_exptl_crystal_size_mid          0.43
_exptl_crystal_size_min          0.34
_refine_diff_density_max         0.383
_refine_diff_density_min         -0.359
_refine_diff_density_rms         0.045
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.053
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     687
_refine_ls_number_reflns         6352
_refine_ls_number_restraints     558
_refine_ls_restrained_S_all      1.035
_refine_ls_R_factor_all          0.0423
_refine_ls_R_factor_gt           0.0342
_refine_ls_shift/su_max          0.014
_refine_ls_shift/su_mean         0.001
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0398P)^2^+1.4505P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0840
_refine_ls_wR_factor_ref         0.0884
_reflns_number_gt                5501
_reflns_number_total             6352
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic991385t.cif
_cod_data_source_block           rd134
_cod_depositor_comments
;
The following automatic conversions were performed:

'_symmetry_cell_setting' value 'Triclinic' changed to 'triclinic'
according to the built-in table from CIF Core dictionary named
'cif_core.dic' version 2.4.1 from 2010-06-29.

Automatic conversion script
Id: cif_fix_values 1646 2011-03-28 12:23:43Z adriana 
;
_cod_database_code               4320960