#------------------------------------------------------------------------------
#$Date: 2019-11-23 10:28:03 +0200 (Sat, 23 Nov 2019) $
#$Revision: 232875 $
#$URL: file:///home/coder/svn-repositories/cod/cif/4/34/83/4348319.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_4348319
loop_
_publ_author_name
'Goettel, James T.'
'Kostiuk, Nathan'
'Gerken, Michael'
_publ_section_title
;
 Interactions between SF4 and Fluoride: A Crystallographic Study of
 Solvolysis Products of SF4·Nitrogen-Base Adducts by HF.
;
_journal_issue                   14
_journal_name_full               'Inorganic chemistry'
_journal_page_first              7126
_journal_page_last               7134
_journal_paper_doi               10.1021/acs.inorgchem.6b01112
_journal_volume                  55
_journal_year                    2016
_chemical_formula_sum            'C6 H9 F2 N'
_chemical_formula_weight         133.14
_space_group_IT_number           62
_space_group_name_Hall           '-P 2ac 2n'
_space_group_name_H-M_alt        'P n m a'
_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_H-M   'P n m a'
_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                   19.22(4)
_cell_length_b                   7.741(16)
_cell_length_c                   4.740(10)
_cell_measurement_temperature    153(2)
_cell_volume                     705(3)
_computing_cell_refinement       'APEX2 (Bruker, 2006)'
_computing_data_collection       'APEX2 (Bruker, 2006)'
_computing_data_reduction        'SAINT-Plus (Bruker, 2006)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      153(2)
_diffrn_measured_fraction_theta_full 0.986
_diffrn_measured_fraction_theta_max 0.986
_diffrn_measurement_device_type  'Bruker Smart Apex II'
_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  0.0401
_diffrn_reflns_av_sigmaI/netI    0.0244
_diffrn_reflns_limit_h_max       24
_diffrn_reflns_limit_h_min       -25
_diffrn_reflns_limit_k_max       10
_diffrn_reflns_limit_k_min       -9
_diffrn_reflns_limit_l_max       6
_diffrn_reflns_limit_l_min       -6
_diffrn_reflns_number            7416
_diffrn_reflns_theta_full        27.69
_diffrn_reflns_theta_max         27.69
_diffrn_reflns_theta_min         2.12
_exptl_absorpt_coefficient_mu    0.112
_exptl_absorpt_correction_T_max  0.7456
_exptl_absorpt_correction_T_min  0.6606
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
; 
SADABS (Sheldrick, 2004)
;
_exptl_crystal_density_diffrn    1.254
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       needle
_exptl_crystal_F_000             280
_exptl_crystal_size_max          0.35
_exptl_crystal_size_mid          0.16
_exptl_crystal_size_min          0.09
_refine_diff_density_max         0.197
_refine_diff_density_min         -0.140
_refine_diff_density_rms         0.033
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.019
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     53
_refine_ls_number_reflns         869
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.019
_refine_ls_R_factor_all          0.0541
_refine_ls_R_factor_gt           0.0366
_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/[σ²(Fo²)+(0.0524P)²+0.1984P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1016
_refine_ls_wR_factor_ref         0.1148
_reflns_number_gt                638
_reflns_number_total             869
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic6b01112_si_002.cif
_cod_data_source_block           mg12078_0ma
_cod_original_cell_volume        705(2)
_cod_original_sg_symbol_H-M      Pnma
_cod_database_code               4348319
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x+1/2, -y, z+1/2'
'-x, y+1/2, -z'
'x+1/2, -y+1/2, -z+1/2'
'-x, -y, -z'
'x-1/2, y, -z-1/2'
'x, -y-1/2, z'
'-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
N1 N 0.05582(8) 0.2500 0.7051(3) 0.0395(4) Uani 1 2 d S
H1 H 0.0233 0.2500 0.8359 0.047 Uiso 1 2 calc SR
C4 C 0.08000(7) 0.40037(18) 0.6079(3) 0.0438(4) Uani 1 1 d .
H4 H 0.0617 0.5058 0.6790 0.053 Uiso 1 1 calc R
C3 C 0.13110(7) 0.4034(2) 0.4057(3) 0.0484(4) Uani 1 1 d .
H3 H 0.1480 0.5108 0.3373 0.058 Uiso 1 1 calc R
C2 C 0.15812(10) 0.2500 0.3008(4) 0.0483(6) Uani 1 2 d S
C1 C 0.21543(12) 0.2500 0.0872(5) 0.0891(11) Uani 1 2 d S
H1A H 0.2599 0.2720 0.1817 0.134 Uiso 0.50 1 calc PR
H1B H 0.2068 0.3406 -0.0529 0.134 Uiso 0.50 1 calc PR
H1C H 0.2172 0.1374 -0.0070 0.134 Uiso 0.50 1 calc PR
F1 F -0.03696(6) 0.2500 1.0846(3) 0.0507(4) Uani 1 2 d S
H5 H -0.0996(17) 0.2500 1.011(7) 0.121(13) Uiso 1 2 d S
F2 F -0.15439(7) 0.2500 0.9686(3) 0.0569(4) Uani 1 2 d S
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
N1 0.0346(8) 0.0473(10) 0.0365(8) 0.000 -0.0020(7) 0.000
C4 0.0454(8) 0.0356(8) 0.0504(8) -0.0034(7) -0.0127(6) 0.0033(6)
C3 0.0445(8) 0.0527(9) 0.0480(8) 0.0162(7) -0.0143(6) -0.0130(7)
C2 0.0335(10) 0.0804(16) 0.0311(9) 0.000 -0.0098(8) 0.000
C1 0.0374(12) 0.191(4) 0.0386(12) 0.000 -0.0009(10) 0.000
F1 0.0479(7) 0.0506(8) 0.0536(8) 0.000 0.0092(5) 0.000
F2 0.0506(8) 0.0530(8) 0.0672(9) 0.000 0.0094(6) 0.000
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'
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'
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
C4 N1 C4 121.3(2) 7_565 .
N1 C4 C3 120.33(15) . .
C4 C3 C2 120.21(16) . .
C3 C2 C3 117.6(2) . 7_565
C3 C2 C1 121.18(11) . .
C3 C2 C1 121.18(11) 7_565 .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
N1 C4 1.335(3) 7_565
N1 C4 1.335(3) .
C4 C3 1.372(3) .
C3 C2 1.388(3) .
C2 C3 1.388(3) 7_565
C2 C1 1.496(4) .
loop_
_geom_hbond_atom_site_label_D
_geom_hbond_atom_site_label_H
_geom_hbond_atom_site_label_A
_geom_hbond_distance_DH
_geom_hbond_distance_HA
_geom_hbond_distance_DA
_geom_hbond_angle_DHA
N1 H1 F1 0.88 1.65 2.533(4) 179.3
