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_4314115
_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 H10 Al B F18 N6'
_chemical_formula_weight         678.10
_chemical_name_common            '[HB(3,5-(CF3)2Pz)3]AlMe2'
_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
_cell_angle_alpha                76.055(10)
_cell_angle_beta                 69.300(12)
_cell_angle_gamma                85.176(13)
_cell_formula_units_Z            2
_cell_length_a                   9.284(2)
_cell_length_b                   11.788(2)
_cell_length_c                   12.604(1)
_cell_measurement_reflns_used    25
_cell_measurement_temperature    183(2)
_cell_measurement_theta_max      12.45
_cell_measurement_theta_min      4.91
_cell_volume                     1252.3(4)
_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-93 (Sheldrick, 1993)'
_computing_structure_solution    'SHELXS-86 (Sheldrick, 1990)'
_diffrn_ambient_temperature      183(2)
_diffrn_measurement_device       'Siemens 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  0.0186
_diffrn_reflns_av_sigmaI/netI    0.0416
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_h_min       -1
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       13
_diffrn_reflns_limit_l_min       -13
_diffrn_reflns_number            3997
_diffrn_reflns_theta_max         22.49
_diffrn_reflns_theta_min         1.77
_diffrn_standards_decay_%        8.26
_diffrn_standards_interval_count 97
_diffrn_standards_number         3
_exptl_absorpt_coefficient_mu    0.237
_exptl_absorpt_correction_T_max  0.9348
_exptl_absorpt_correction_T_min  0.9042
_exptl_absorpt_correction_type   empirical
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.798
_exptl_crystal_description       paralellpipeds
_exptl_crystal_F_000             668
_exptl_crystal_size_max          0.39
_exptl_crystal_size_mid          0.24
_exptl_crystal_size_min          0.14
_refine_diff_density_max         0.413
_refine_diff_density_min         -0.279
_refine_diff_density_rms         0.048
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_all   1.047
_refine_ls_goodness_of_fit_obs   1.083
_refine_ls_matrix_type           full
_refine_ls_number_parameters     394
_refine_ls_number_reflns         3262
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.048
_refine_ls_restrained_S_obs      1.083
_refine_ls_R_factor_all          0.0642
_refine_ls_R_factor_obs          0.0450
_refine_ls_shift/esd_max         0.018
_refine_ls_shift/esd_mean        0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0372P)^2^+1.5083P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.1123
_refine_ls_wR_factor_obs         0.1002
_reflns_number_observed          2525
_reflns_number_total             3263
_reflns_observed_criterion       >2sigma(I)
_cod_data_source_file            ic0345875si20030603_115209_2.cif
_cod_data_source_block           rd132
_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 

The following automatic conversions were performed:

'_refine_ls_weighting_scheme' value 'calc
w=1/[\s^2^(Fo^2^)+(0.0372P)^2^+1.5083P] where P=(Fo^2^+2Fc^2^)/3' was
changed to 'calc'. New tag '_refine_ls_weighting_details' was
created. The value of the new tag was set to
'w=1/[\s^2^(Fo^2^)+(0.0372P)^2^+1.5083P] where P=(Fo^2^+2Fc^2^)/3'.

Automatic conversion script
Id: cif_fix_values 3143 2015-03-26 13:38:13Z robertas 
;
_cod_original_cell_volume        1252.4(3)
_cod_database_code               4314115