Syntheses of Aluminum and Zinc Alkyl Complexes of a Highly Fluorinated Tris(pyrazolyl)borate Using [HB(3,5-(CF3)2Pz)3]Ag(THF) as the Ligand Transfer Agent
H. V. Rasika Dias; Wiechang Jin; Inorganic Chemistry 42 (2003) 5034–5036; doi:10.1021/ic0345875

data_4314114
_publ_contact_author_address
;Dept. of Chemistry and Biochemistry
The University of Texas at Arlington
Arlington
Texas 76019-0065
USA
;
_publ_contact_author_email       dias@uta.edu
_publ_contact_author_fax         817-272-3808
_publ_contact_author_name        'Dr. Rasika Dias'
_publ_contact_author_phone       817-272-3813
_publ_section_title
;
 Syntheses of Aluminum and Zinc Alkyl Complexes of a Highly Fluorinated
 Tris(pyrazolyl)borate Using [HB(3,5-(CF3)2Pz)3]Ag(THF) as the Ligand
 Transfer Agent
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              5034
_journal_page_last               5036
_journal_paper_doi               10.1021/ic0345875
_journal_volume                  42
_journal_year                    2003
_chemical_formula_sum            'C17 H9 B F18 N6 Zn'
_chemical_formula_weight         715.48
_chemical_name_common            '[HB(3,5-(CF3)2Pz)3]ZnEt'
_chemical_name_systematic
;
  ?
;
_space_group_IT_number           58
_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_Hall  '-P 2 2n'
_symmetry_space_group_name_H-M   'P n n m'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   19.156(2)
_cell_length_b                   9.0308(9)
_cell_length_c                   14.4970(19)
_cell_measurement_reflns_used    41
_cell_measurement_temperature    183(2)
_cell_measurement_theta_max      12.51
_cell_measurement_theta_min      5.01
_cell_volume                     2507.9(5)
_computing_cell_refinement       'Siemens XSCANS'
_computing_data_collection       'Siemens XSCANS'
_computing_data_reduction        'Siemens SHELXTL'
_computing_molecular_graphics    'Siemens SHELXTL'
_computing_publication_material  'Siemens 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 0.999
_diffrn_measured_fraction_theta_max 0.999
_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  0.0272
_diffrn_reflns_av_sigmaI/netI    0.0325
_diffrn_reflns_limit_h_max       20
_diffrn_reflns_limit_h_min       -1
_diffrn_reflns_limit_k_max       9
_diffrn_reflns_limit_k_min       -1
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_limit_l_min       -1
_diffrn_reflns_number            2308
_diffrn_reflns_theta_full        22.49
_diffrn_reflns_theta_max         22.49
_diffrn_reflns_theta_min         2.13
_diffrn_standards_interval_count 97
_diffrn_standards_number         3
_exptl_absorpt_coefficient_mu    1.134
_exptl_absorpt_correction_T_max  0.9806
_exptl_absorpt_correction_T_min  0.8216
_exptl_absorpt_correction_type   empirical
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.895
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       blocks
_exptl_crystal_F_000             1400
_exptl_crystal_size_max          0.72
_exptl_crystal_size_mid          0.40
_exptl_crystal_size_min          0.11
_refine_diff_density_max         0.458
_refine_diff_density_min         -0.338
_refine_diff_density_rms         0.073
_refine_ls_extinction_coef       0.0007(5)
_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   1.039
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     221
_refine_ls_number_reflns         1723
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.039
_refine_ls_R_factor_all          0.0523
_refine_ls_R_factor_gt           0.0414
_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^)+(0.0669P)^2^+2.8686P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1075
_refine_ls_wR_factor_ref         0.1147
_reflns_number_gt                1436
_reflns_number_total             1723
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic0345875si20030603_115209_1.cif
_cod_data_source_block           rd130a
_cod_depositor_comments
;
The following automatic conversions were performed:

'_symmetry_cell_setting' value 'Orthorhombic' changed to
'orthorhombic' 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               4314114