#------------------------------------------------------------------------------
#$Date: 2016-02-20 18:35:30 +0200 (Sat, 20 Feb 2016) $
#$Revision: 176787 $
#$URL: svn://www.crystallography.net/cod/cif/2/21/29/2212943.cif $
#------------------------------------------------------------------------------
#
# This file is available in the Crystallography Open Database (COD),
# http://www.crystallography.net/. The original data for this entry
# were provided by IUCr Journals, http://journals.iucr.org/.
#
# The file may be used within the scientific community so long as
# proper attribution is given to the journal article from which the
# data were obtained.
#
data_2212943
loop_
_publ_author_name
'Marielle Nicole C. Balili'
'Tomislav Pintauer'
_publ_section_title
(Acetonitrile){hydridotris[3,5-bis(trifluoromethyl)-1-pyrazolyl]borato}copper(I)
_journal_coeditor_code           KP2089
_journal_issue                   4
_journal_name_full               'Acta Crystallographica Section E'
_journal_page_first              m988
_journal_page_last               m990
_journal_paper_doi               10.1107/S1600536807009762
_journal_volume                  63
_journal_year                    2007
_chemical_formula_iupac          '[Cu (C15 H4 B F18 N6) (C2 H3 N1)]'
_chemical_formula_moiety         'C17 H6.97 B Cu F18 N7'
_chemical_formula_sum            'C17 H6.97 B Cu F18 N7'
_chemical_formula_weight         725.65
_chemical_name_systematic
;
(Acetonitrile){hydridotris[3,5-bis(trifluoromethyl)-1-
pyrazolyl]borato}copper(I)
;
_space_group_IT_number           161
_symmetry_cell_setting           trigonal
_symmetry_space_group_name_Hall  'R 3 -2"c'
_symmetry_space_group_name_H-M   'R 3 c :H'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                120.00
_cell_formula_units_Z            6
_cell_length_a                   13.0510(14)
_cell_length_b                   13.0510(14)
_cell_length_c                   25.047(5)
_cell_measurement_reflns_used    7594
_cell_measurement_temperature    150
_cell_measurement_theta_max      31.989
_cell_measurement_theta_min      2.4245
_cell_volume                     3694.7(9)
_computing_cell_refinement       'SAINT (Bruker, 1998)'
_computing_data_collection       'SMART (Bruker, 1998)'
_computing_data_reduction        SAINT
_computing_molecular_graphics    'SHELXTL (Sheldrick, 2000)'
_computing_publication_material  'ORTEP-3 for Windows (Faruggia, 1997)'
_computing_structure_refinement  'SHELXL97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS97 (Sheldrick, 1997)'
_diffrn_ambient_temperature      296(2)
_diffrn_measured_fraction_theta_full 0.985
_diffrn_measured_fraction_theta_max 0.985
_diffrn_measurement_device_type  'Bruker SMART APEXII'
_diffrn_measurement_method       'φ and ω'
_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  0.0440
_diffrn_reflns_av_sigmaI/netI    0.0253
_diffrn_reflns_limit_h_max       19
_diffrn_reflns_limit_h_min       -19
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       37
_diffrn_reflns_limit_l_min       -37
_diffrn_reflns_number            14977
_diffrn_reflns_theta_full        32.62
_diffrn_reflns_theta_max         32.62
_diffrn_reflns_theta_min         2.43
_diffrn_standards_interval_count 0
_diffrn_standards_interval_time  0
_diffrn_standards_number         2907
_exptl_absorpt_coefficient_mu    1.048
_exptl_absorpt_correction_T_max  0.735
_exptl_absorpt_correction_T_min  0.664
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   '(SADABS; Sheldrick, 2002)'
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.957
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prisms
_exptl_crystal_F_000             2123.8
_exptl_crystal_size_max          0.40
_exptl_crystal_size_mid          0.37
_exptl_crystal_size_min          0.30
_refine_diff_density_max         0.477
_refine_diff_density_min         -0.230
_refine_ls_abs_structure_details 'Flack (1983)'
_refine_ls_abs_structure_Flack   0.007(10)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.012
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     136
_refine_ls_number_reflns         2907
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.012
_refine_ls_R_factor_all          0.0305
_refine_ls_R_factor_gt           0.0265
_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)+(0.0473P)²] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0702
_refine_ls_wR_factor_ref         0.0718
_reflns_number_gt                2601
_reflns_number_total             2907
_reflns_threshold_expression     I>2σ(I)
_cod_data_source_file            kp2089.cif
_cod_data_source_block           I
_cod_original_sg_symbol_H-M      'R 3 c'
_cod_database_code               2212943
_cod_database_fobs_code          2212943
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-y, x-y, z'
'-x+y, -x, z'
'-y, -x, z+1/2'
'-x+y, y, z+1/2'
'x, x-y, z+1/2'
'x+2/3, y+1/3, z+1/3'
'-y+2/3, x-y+1/3, z+1/3'
'-x+y+2/3, -x+1/3, z+1/3'
'-y+2/3, -x+1/3, z+5/6'
'-x+y+2/3, y+1/3, z+5/6'
'x+2/3, x-y+1/3, z+5/6'
'x+1/3, y+2/3, z+2/3'
'-y+1/3, x-y+2/3, z+2/3'
'-x+y+1/3, -x+2/3, z+2/3'
'-y+1/3, -x+2/3, z+7/6'
'-x+y+1/3, y+2/3, z+7/6'
'x+1/3, x-y+2/3, z+7/6'
loop_
_atom_site_type_symbol
_atom_site_label
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_occupancy
Cu Cu1 0.6667 0.3333 0.893096(15) 0.02801(8) Uani d S 1
C C1 0.6667 0.3333 0.77220(15) 0.0316(7) Uani d S 1
N N2 0.77043(10) 0.28976(11) 0.94166(4) 0.0234(2) Uani d . 1
F F4 0.87543(12) 0.37598(11) 1.10185(5) 0.0506(3) Uani d . 1
C C6 0.82907(12) 0.26897(13) 1.02169(5) 0.0260(2) Uani d . 1
N N3 0.75603(10) 0.29702(10) 0.99484(4) 0.02097(19) Uani d . 1
C C5 0.89239(14) 0.24298(15) 0.98566(6) 0.0324(3) Uani d . 1
H H5 0.9488 0.2211 0.9926 0.039 Uiso calc R 1
F F5 0.73799(12) 0.19505(13) 1.10518(5) 0.0484(3) Uani d . 1
C C7 0.83937(15) 0.26972(16) 1.08104(6) 0.0338(3) Uani d . 1
F F6 0.91834(13) 0.23762(14) 1.09492(4) 0.0508(3) Uani d . 1
F F3 1.00119(10) 0.26550(16) 0.88275(5) 0.0650(4) Uani d . 1
C C4 0.85182(12) 0.25732(13) 0.93638(6) 0.0276(3) Uani d . 1
F F2 0.82784(13) 0.12369(13) 0.86898(6) 0.0626(4) Uani d . 1
N N1 0.6667 0.3333 0.81771(10) 0.0336(5) Uani d S 1
C C3 0.88876(14) 0.23692(16) 0.88271(6) 0.0350(3) Uani d . 1
C C2 0.6667 0.3333 0.71351(12) 0.0396(7) Uani d S 1
H H2A 0.5883 0.2798 0.7007 0.059 Uiso calc PR 0.33
H H2B 0.7202 0.3085 0.7007 0.059 Uiso calc PR 0.33
H H2C 0.6915 0.4117 0.7007 0.059 Uiso calc PR 0.33
F F1 0.8724(2) 0.2952(2) 0.84425(6) 0.0871(6) Uani d . 1
B B1 0.6667 0.3333 1.01603(12) 0.0189(5) Uani d S 1
H H1 0.6667 0.3333 1.0580(15) 0.017(8) Uiso d S 1
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'
Cu Cu 0.3201 1.2651 '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_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle
_geom_angle_publ_flag
N1 Cu1 N2 . 2_655 125.41(3) yes
N1 Cu1 N2 . 3_665 125.41(3) yes
N2 Cu1 N2 2_655 3_665 89.80(5) yes
N1 Cu1 N2 . . 125.41(3) yes
N2 Cu1 N2 2_655 . 89.79(5) yes
N2 Cu1 N2 3_665 . 89.79(5) yes
N1 C1 C2 . . 180.000(2) yes
C4 N2 N3 . . 106.26(11) ?
C4 N2 Cu1 . . 138.90(10) ?
N3 N2 Cu1 . . 114.82(8) ?
N3 C6 C5 . . 109.32(12) ?
N3 C6 C7 . . 124.38(12) ?
C5 C6 C7 . . 126.29(12) ?
N2 N3 C6 . . 109.11(10) ?
N2 N3 B1 . . 120.52(14) ?
C6 N3 B1 . . 130.37(14) ?
C6 C5 C4 . . 103.46(12) ?
C6 C5 H5 . . 128.3 ?
C4 C5 H5 . . 128.3 ?
F4 C7 F5 . . 106.83(14) ?
F4 C7 F6 . . 107.38(13) ?
F5 C7 F6 . . 106.96(14) ?
F4 C7 C6 . . 112.43(14) ?
F5 C7 C6 . . 113.19(13) ?
F6 C7 C6 . . 109.74(12) ?
N2 C4 C5 . . 111.85(12) ?
N2 C4 C3 . . 121.64(13) ?
C5 C4 C3 . . 126.49(13) ?
C1 N1 Cu1 . . 180.0000(10) yes
F1 C3 F3 . . 108.51(17) ?
F1 C3 F2 . . 105.98(17) ?
F3 C3 F2 . . 106.09(15) ?
F1 C3 C4 . . 113.40(14) ?
F3 C3 C4 . . 111.12(13) ?
F2 C3 C4 . . 111.36(14) ?
C1 C2 H2A . . 109.5 ?
C1 C2 H2B . . 109.5 ?
H2A C2 H2B . . 109.5 ?
C1 C2 H2C . . 109.5 ?
H2A C2 H2C . . 109.5 ?
H2B C2 H2C . . 109.5 ?
N3 B1 N3 . 3_665 108.99(12) ?
N3 B1 N3 . 2_655 108.99(12) ?
N3 B1 N3 3_665 2_655 108.99(12) ?
N3 B1 H1 . . 109.94(11) ?
N3 B1 H1 3_665 . 109.95(12) ?
N3 B1 H1 2_655 . 109.95(12) ?
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_site_symmetry_2
_geom_bond_distance
_geom_bond_publ_flag
Cu1 N1 . 1.888(3) yes
Cu1 N2 2_655 2.0992(12) yes
Cu1 N2 3_665 2.0992(12) yes
Cu1 N2 . 2.0992(12) yes
C1 N1 . 1.140(5) yes
C1 C2 . 1.470(5) ?
N2 C4 . 1.3322(18) ?
N2 N3 . 1.3553(15) ?
F4 C7 . 1.328(2) ?
C6 N3 . 1.3578(17) ?
C6 C5 . 1.3758(18) ?
C6 C7 . 1.492(2) ?
N3 B1 . 1.5554(15) ?
C5 C4 . 1.392(2) ?
C5 H5 . 0.9300 ?
F5 C7 . 1.333(2) ?
C7 F6 . 1.3381(18) ?
F3 C3 . 1.321(2) ?
C4 C3 . 1.496(2) ?
F2 C3 . 1.326(2) ?
C3 F1 . 1.309(2) ?
C2 H2A . 0.9600 ?
C2 H2B . 0.9600 ?
C2 H2C . 0.9600 ?
B1 N3 3_665 1.5554(15) ?
B1 N3 2_655 1.5554(15) ?
B1 H1 . 1.05(4) ?
