#------------------------------------------------------------------------------
#$Date: 2016-03-23 02:19:42 +0100 (Wed, 23 Mar 2016) $
#$Revision: 179241 $
#$URL: svn://saulius.grazulis.lt/cod-secondary/cif/4/31/61/4316108.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_4316108
loop_
_publ_author_name
'Karl O. Christe'
'David A. Dixon'
'Daniel J. Grant'
'Ralf Haiges'
'Fook S. Tham'
'Ashwani Vij'
'Vandana Vij'
'Tsang-Hsiu Wang'
'William W. Wilson'
_publ_contact_author_address
;Loker Hydrocarbon Research Institute
University of Southern California
Los Angeles, CA 90089
;
_publ_contact_author_email       kchriste@usc.edu
_publ_contact_author_name        'Prof. Dr. Karl Christe'
_publ_section_title
;
 Dinitrogen Difluoride Chemistry. Improved Syntheses of cis- and
 trans-N2F2, Synthesis and Characterization of N2F+Sn2F9-, Ordered Crystal
 Structure of N2F+Sb2F11-, High-Level Electronic Structure Calculations of
 cis-N2F2, trans-N2F2, F2N=N, and N2F+, and Mechanism of the trans-cis
 Isomerization of N2F2
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              6823
_journal_page_last               6833
_journal_paper_doi               10.1021/ic100471s
_journal_volume                  49
_journal_year                    2010
_chemical_absolute_configuration unk
_chemical_compound_source        'From Cis-N2F2'
_chemical_formula_moiety         'F6 Sb, N2 F'
_chemical_formula_sum            'F7 N2 Sb'
_chemical_formula_weight         282.77
_chemical_name_common            'Fluorodiazonium antimonyhexafluoride'
_chemical_name_systematic        'Fluorodiazonium antimonyhexafluoride'
_chemical_properties_physical    'air-sensitive, moisture-sensitive'
_space_group_IT_number           65
_symmetry_cell_setting           orthorhombic
_symmetry_Int_Tables_number      65
_symmetry_space_group_name_Hall  '-C 2 2'
_symmetry_space_group_name_H-M   'C m m m'
_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            2
_cell_length_a                   6.8824(9)
_cell_length_b                   7.5308(9)
_cell_length_c                   5.5695(7)
_cell_measurement_reflns_used    936
_cell_measurement_temperature    203(2)
_cell_measurement_theta_max      25.33
_cell_measurement_theta_min      3.66
_cell_volume                     288.67(6)
_computing_cell_refinement       'BRUKER SMART'
_computing_data_collection       'Bruker SMART'
_computing_data_reduction        'BRUKER SAINT'
_computing_molecular_graphics    SHELXTL
_computing_publication_material  SHELXTL
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      203(2)
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 1.000
_diffrn_measurement_device_type  'Bruker APEX'
_diffrn_measurement_method       Omega
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0833
_diffrn_reflns_av_sigmaI/netI    0.0466
_diffrn_reflns_limit_h_max       8
_diffrn_reflns_limit_h_min       -7
_diffrn_reflns_limit_k_max       9
_diffrn_reflns_limit_k_min       -8
_diffrn_reflns_limit_l_max       6
_diffrn_reflns_limit_l_min       -6
_diffrn_reflns_number            936
_diffrn_reflns_theta_full        25.33
_diffrn_reflns_theta_max         25.33
_diffrn_reflns_theta_min         3.66
_diffrn_source                   'fine-focus sealed tube'
_diffrn_source_type              'Bruker APEX CCD'
_diffrn_standards_decay_%        0
_diffrn_standards_interval_count 30
_diffrn_standards_interval_time  360
_diffrn_standards_number         100
_exptl_absorpt_coefficient_mu    4.864
_exptl_absorpt_correction_T_max  0.4747
_exptl_absorpt_correction_T_min  0.1947
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_process_details   SADABS
_exptl_crystal_colour            Colorless
_exptl_crystal_density_diffrn    3.253
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       Prismatic
_exptl_crystal_F_000             256
_exptl_crystal_recrystallization_method 'Anhydrous HF'
_exptl_crystal_size_max          0.50
_exptl_crystal_size_mid          0.21
_exptl_crystal_size_min          0.18
_refine_diff_density_max         1.475
_refine_diff_density_min         -1.367
_refine_diff_density_rms         0.336
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.105
_refine_ls_matrix_type           full
_refine_ls_number_parameters     21
_refine_ls_number_reflns         172
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.105
_refine_ls_R_factor_all          0.0389
_refine_ls_R_factor_gt           0.0389
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0721P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0887
_refine_ls_wR_factor_ref         0.0887
_reflns_number_gt                172
_reflns_number_total             172
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic100471s_si_002.cif
_cod_data_source_block           cmmm
_cod_database_code               4316108
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, -y, z'
'-x, y, -z'
'x, -y, -z'
'x+1/2, y+1/2, z'
'-x+1/2, -y+1/2, z'
'-x+1/2, y+1/2, -z'
'x+1/2, -y+1/2, -z'
'-x, -y, -z'
'x, y, -z'
'x, -y, z'
'-x, y, z'
'-x+1/2, -y+1/2, -z'
'x+1/2, y+1/2, -z'
'x+1/2, -y+1/2, z'
'-x+1/2, y+1/2, z'
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
Sb1 Sb 0.0000 0.5000 0.0000 0.0160(5) Uani 1 8 d S . .
F2 F 0.1901(9) 0.5000 0.2410(11) 0.0426(14) Uani 1 2 d S . .
F1 F 0.0000 0.2535(12) 0.0000 0.046(2) Uani 1 4 d S . .
N2 N 0.5000 0.5000 0.5000 0.032(4) Uani 1 8 d S . .
N1 N 0.5000 0.6553(12) 0.5000 0.039(2) Uani 0.50 4 d SP . .
F3 F 0.5000 0.6553(12) 0.5000 0.039(2) Uani 0.50 4 d SP . .
loop_
_atom_site_aniso_label
_atom_site_aniso_U_11
_atom_site_aniso_U_22
_atom_site_aniso_U_33
_atom_site_aniso_U_23
_atom_site_aniso_U_13
_atom_site_aniso_U_12
Sb1 0.0084(7) 0.0339(7) 0.0057(6) 0.000 0.000 0.000
F2 0.023(3) 0.078(4) 0.026(3) 0.000 -0.012(3) 0.000
F1 0.044(6) 0.032(4) 0.062(6) 0.000 0.000 0.000
N2 0.018(9) 0.064(14) 0.014(8) 0.000 0.000 0.000
N1 0.045(7) 0.036(6) 0.036(6) 0.000 0.000 0.000
F3 0.045(7) 0.036(6) 0.036(6) 0.000 0.000 0.000
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
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'
Sb Sb -0.5866 1.5461 '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
F1 Sb1 F1 180.0 9_565 . ?
F1 Sb1 F2 90.0 9_565 9_565 ?
F1 Sb1 F2 90.0 . 9_565 ?
F1 Sb1 F2 90.000(1) 9_565 10 ?
F1 Sb1 F2 90.0 . 10 ?
F2 Sb1 F2 88.5(4) 9_565 10 ?
F1 Sb1 F2 90.000(1) 9_565 2_565 ?
F1 Sb1 F2 90.0 . 2_565 ?
F2 Sb1 F2 91.5(4) 9_565 2_565 ?
F2 Sb1 F2 180.000(1) 10 2_565 ?
F1 Sb1 F2 90.0 9_565 . ?
F1 Sb1 F2 90.0 . . ?
F2 Sb1 F2 180.0(3) 9_565 . ?
F2 Sb1 F2 91.5(4) 10 . ?
F2 Sb1 F2 88.5(4) 2_565 . ?
F3 N2 N1 0.000(1) 9_666 9_666 ?
F3 N2 N1 180.000(2) 9_666 . ?
N1 N2 N1 180.000(2) 9_666 . ?
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
Sb1 F1 1.856(9) 9_565 ?
Sb1 F1 1.856(9) . ?
Sb1 F2 1.874(6) 9_565 ?
Sb1 F2 1.874(6) 10 ?
Sb1 F2 1.874(6) 2_565 ?
Sb1 F2 1.874(6) . ?
N2 F3 1.170(9) 9_666 ?
N2 N1 1.170(9) 9_666 ?
N2 N1 1.170(9) . ?
