#------------------------------------------------------------------------------
#$Date: 2016-03-23 02:51:16 +0200 (Wed, 23 Mar 2016) $
#$Revision: 179211 $
#$URL: svn://www.crystallography.net/cod/cif/4/31/41/4314114.cif $
#------------------------------------------------------------------------------
#
# This file is available in the Crystallography Open Database (COD),
# http://www.crystallography.net/
#
# All data on this site have been placed in the public domain by the
# contributors.
#
data_4314114
loop_
_publ_author_name
'H. V. Rasika Dias'
'Wiechang Jin'
_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       'ω 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+0.001xFc²λ³/sin(2θ)]^-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/[σ²(Fo²)+(0.0669P)²+2.8686P] where P=(Fo²+2Fc²)/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
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, -y, z'
'-x+1/2, y+1/2, -z+1/2'
'x+1/2, -y+1/2, -z+1/2'
'-x, -y, -z'
'x, y, -z'
'x-1/2, -y-1/2, z-1/2'
'-x-1/2, y-1/2, z-1/2'
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
Zn Zn 0.71240(3) -0.07053(7) 1.0000 0.0341(3) Uani 1 2 d S . .
N11 N 0.7908(2) -0.3603(5) 1.0000 0.0241(10) Uani 1 2 d S . .
N12 N 0.7240(2) -0.3040(5) 1.0000 0.0281(10) Uani 1 2 d S . .
N21 N 0.84935(14) -0.1533(3) 0.9128(2) 0.0271(7) Uani 1 1 d . . .
N22 N 0.79276(15) -0.0647(3) 0.8989(2) 0.0280(8) Uani 1 1 d . . .
C13 C 0.6819(3) -0.4211(6) 1.0000 0.0291(13) Uani 1 2 d S . .
C14 C 0.7185(3) -0.5520(6) 1.0000 0.0315(13) Uani 1 2 d S . .
H14 H 0.7007 -0.6477 1.0000 0.038 Uiso 1 2 calc SR . .
C15 C 0.7874(3) -0.5100(6) 1.0000 0.0312(13) Uani 1 2 d S . .
C16 C 0.6044(3) -0.4043(7) 1.0000 0.0418(15) Uani 1 2 d S . .
C17 C 0.8499(3) -0.6072(6) 1.0000 0.0409(15) Uani 1 2 d S . .
C23 C 0.8038(2) 0.0037(5) 0.8194(3) 0.0340(9) Uani 1 1 d . . .
C24 C 0.8665(2) -0.0376(5) 0.7804(3) 0.0395(10) Uani 1 1 d . . .
H24 H 0.8858 -0.0048 0.7252 0.047 Uiso 1 1 calc R . .
C25 C 0.8937(2) -0.1372(4) 0.8410(3) 0.0334(10) Uani 1 1 d . . .
C26 C 0.7519(3) 0.1097(5) 0.7807(3) 0.0495(12) Uani 1 1 d . . .
C27 C 0.9620(2) -0.2156(5) 0.8338(3) 0.0466(12) Uani 1 1 d . . .
F16A F 0.5748(2) -0.5322(5) 1.0000 0.147(3) Uani 1 2 d S . .
F16B F 0.58130(13) -0.3314(5) 1.0714(2) 0.0866(12) Uani 1 1 d . . .
F17A F 0.88949(15) -0.5876(3) 1.0733(3) 0.0797(10) Uani 1 1 d . . .
F17B F 0.83042(18) -0.7496(4) 1.0000 0.0524(10) Uani 1 2 d S . .
F26A F 0.7772(2) 0.1787(5) 0.7088(3) 0.1173(17) Uani 1 1 d . . .
F26B F 0.73175(18) 0.2112(3) 0.83906(19) 0.0743(10) Uani 1 1 d . . .
F26C F 0.6955(2) 0.0455(4) 0.7511(4) 0.127(2) Uani 1 1 d . . .
F27A F 0.99271(15) -0.1780(4) 0.7535(2) 0.0741(10) Uani 1 1 d . . .
F27B F 1.00591(13) -0.1764(3) 0.9010(2) 0.0650(8) Uani 1 1 d . . .
F27C F 0.95600(13) -0.3605(3) 0.8346(2) 0.0644(8) Uani 1 1 d . . .
B B 0.8539(3) -0.2530(7) 1.0000 0.0277(14) Uani 1 2 d S . .
H H 0.902(3) -0.326(7) 1.0000 0.050 Uiso 1 2 d S . .
C1 C 0.6242(3) 0.0394(7) 1.0000 0.0507(18) Uani 1 2 d S . .
C2 C 0.5792(6) 0.0475(19) 0.9205(10) 0.111(6) Uani 0.50 1 d P . .
H2A H 0.5339 0.0823 0.9390 0.166 Uiso 0.50 1 calc PR . .
H2B H 0.5748 -0.0490 0.8934 0.166 Uiso 0.50 1 calc PR . .
H2C H 0.5988 0.1147 0.8762 0.166 Uiso 0.50 1 calc PR . .
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
B B 0.0013 0.0007 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
F F 0.0171 0.0103 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Zn Zn 0.2839 1.4301 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
C1 Zn N12 126.5(2) . . ?
C1 Zn N22 127.69(13) . 6_557 ?
N12 Zn N22 87.06(11) . 6_557 ?
C1 Zn N22 127.69(13) . . ?
N12 Zn N22 87.06(11) . . ?
N22 Zn N22 87.18(16) 6_557 . ?
C15 N11 N12 108.9(4) . . ?
C15 N11 B 131.5(4) . . ?
N12 N11 B 119.6(4) . . ?
C13 N12 N11 105.7(4) . . ?
C13 N12 Zn 136.6(3) . . ?
N11 N12 Zn 117.7(3) . . ?
C25 N21 N22 108.8(3) . . ?
C25 N21 B 130.8(3) . . ?
N22 N21 B 120.4(3) . . ?
C23 N22 N21 106.0(3) . . ?
C23 N22 Zn 136.7(3) . . ?
N21 N22 Zn 117.3(2) . . ?
N12 C13 C14 111.9(4) . . ?
N12 C13 C16 121.5(5) . . ?
C14 C13 C16 126.6(5) . . ?
C15 C14 C13 104.7(5) . . ?
N11 C15 C14 108.8(5) . . ?
N11 C15 C17 123.5(5) . . ?
C14 C15 C17 127.7(5) . . ?
F16A C16 F16B 107.6(4) . 6_557 ?
F16A C16 F16B 107.6(4) . . ?
F16B C16 F16B 105.0(5) 6_557 . ?
F16A C16 C13 110.3(5) . . ?
F16B C16 C13 112.9(3) 6_557 . ?
F16B C16 C13 112.9(3) . . ?
F17A C17 F17A 107.6(5) . 6_557 ?
F17A C17 F17B 106.8(3) . . ?
F17A C17 F17B 106.8(3) 6_557 . ?
F17A C17 C15 112.6(3) . . ?
F17A C17 C15 112.6(3) 6_557 . ?
F17B C17 C15 110.0(5) . . ?
N22 C23 C24 111.7(4) . . ?
N22 C23 C26 121.4(4) . . ?
C24 C23 C26 126.9(4) . . ?
C25 C24 C23 104.3(4) . . ?
N21 C25 C24 109.1(3) . . ?
N21 C25 C27 123.7(4) . . ?
C24 C25 C27 127.2(4) . . ?
F26C C26 F26B 106.4(5) . . ?
F26C C26 F26A 104.9(4) . . ?
F26B C26 F26A 106.9(4) . . ?
F26C C26 C23 113.1(4) . . ?
F26B C26 C23 113.8(4) . . ?
F26A C26 C23 111.1(4) . . ?
F27C C27 F27B 108.2(4) . . ?
F27C C27 F27A 107.3(4) . . ?
F27B C27 F27A 106.7(3) . . ?
F27C C27 C25 113.3(4) . . ?
F27B C27 C25 112.1(4) . . ?
F27A C27 C25 108.9(4) . . ?
N11 B N21 108.6(3) . 6_557 ?
N11 B N21 108.6(3) . . ?
N21 B N21 108.8(4) 6_557 . ?
C2 C1 C2 106.1(11) 6_557 . ?
C2 C1 Zn 122.8(6) 6_557 . ?
C2 C1 Zn 122.8(6) . . ?
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Zn C1 1.959(6) . ?
Zn N12 2.121(4) . ?
Zn N22 2.127(3) 6_557 ?
Zn N22 2.127(3) . ?
N11 C15 1.353(7) . ?
N11 N12 1.377(6) . ?
N11 B 1.549(7) . ?
N12 C13 1.330(7) . ?
N21 C25 1.351(5) . ?
N21 N22 1.363(4) . ?
N21 B 1.555(5) . ?
N22 C23 1.324(5) . ?
C13 C14 1.374(8) . ?
C13 C16 1.491(8) . ?
C14 C15 1.373(8) . ?
C15 C17 1.485(8) . ?
C16 F16A 1.287(8) . ?
C16 F16B 1.304(5) 6_557 ?
C16 F16B 1.304(5) . ?
C17 F17A 1.318(4) . ?
C17 F17A 1.318(4) 6_557 ?
C17 F17B 1.340(7) . ?
C23 C24 1.379(6) . ?
C23 C26 1.490(6) . ?
C24 C25 1.362(6) . ?
C25 C27 1.491(6) . ?
C26 F26C 1.298(6) . ?
C26 F26B 1.307(5) . ?
C26 F26A 1.307(6) . ?
C27 F27C 1.313(5) . ?
C27 F27B 1.336(6) . ?
C27 F27A 1.348(5) . ?
B N21 1.555(5) 6_557 ?
C1 C2 1.442(14) 6_557 ?
C1 C2 1.442(14) . ?
