#------------------------------------------------------------------------------
#$Date: 2019-03-05 10:52:05 +0200 (Tue, 05 Mar 2019) $
#$Revision: 213973 $
#$URL: file:///home/coder/svn-repositories/cod/cif/7/20/45/7204519.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_7204519
loop_
_publ_author_name
'Pringle, Jennifer M.'
'Golding, Jake'
'Forsyth, Craig M.'
'Deacon, Glen B.'
'Forsyth, Maria'
'MacFarlane, Douglas R.'
_publ_section_title
;
 Physical trends and structural features in organic salts of the
 thiocyanate anion
;
_journal_issue                   12
_journal_name_full               'Journal of Materials Chemistry'
_journal_page_first              3475
_journal_paper_doi               10.1039/b208372h
_journal_volume                  12
_journal_year                    2002
_chemical_formula_sum            'C7 H14 N2 S'
_chemical_formula_weight         158.26
_chemical_name_systematic
; 
N,N-dimethylpyrrolidinium thiocyanate 
;
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/c 1'
_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                 104.763(1)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   8.4101(2)
_cell_length_b                   7.8090(2)
_cell_length_c                   13.6228(5)
_cell_measurement_temperature    123(2)
_cell_volume                     865.14(4)
_computing_cell_refinement       'DENZO-SMN (Otwinoski and Minor, 1993)'
_computing_data_collection       'COLLECT (Nonius BV, 1994)'
_computing_data_reduction        'DENZO-SMN (Otwinoski and Minor, 1993)'
_computing_molecular_graphics    'POVRAY 3.0'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      123(2)
_diffrn_measured_fraction_theta_full 0.990
_diffrn_measured_fraction_theta_max 0.990
_diffrn_measurement_device_type  'Enraf Nonius Kappa CCD'
_diffrn_measurement_method       '1 deg frames in phi and omega'
_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  0.0482
_diffrn_reflns_av_sigmaI/netI    0.0467
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       10
_diffrn_reflns_limit_k_min       -10
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            12646
_diffrn_reflns_theta_full        28.30
_diffrn_reflns_theta_max         28.30
_diffrn_reflns_theta_min         2.50
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.305
_exptl_absorpt_process_details   none
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.215
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       irregular
_exptl_crystal_F_000             344
_exptl_crystal_size_max          0.13
_exptl_crystal_size_mid          0.13
_exptl_crystal_size_min          0.06
_refine_diff_density_max         0.274
_refine_diff_density_min         -0.234
_refine_diff_density_rms         0.047
_refine_ls_extinction_coef       0.014(3)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4^
_refine_ls_extinction_method     SHELXL
_refine_ls_goodness_of_fit_ref   0.993
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     148
_refine_ls_number_reflns         2133
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.993
_refine_ls_R_factor_all          0.0641
_refine_ls_R_factor_gt           0.0355
_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)+(0.0556P)²+0.0000P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0854
_refine_ls_wR_factor_ref         0.0967
_reflns_number_gt                1486
_reflns_number_total             2133
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            b208372h.txt
_cod_data_source_block           1
_cod_original_cell_volume        865.1(3)
_cod_original_sg_symbol_H-M      P2(1)/c
_cod_database_code               7204519
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, y+1/2, -z+1/2'
'-x, -y, -z'
'x, -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
S1 S 0.31602(4) 0.19217(5) 0.01073(3) 0.03392(16) Uani 1 1 d . . .
N1 N 0.15283(16) 0.28083(15) 0.15958(10) 0.0326(3) Uani 1 1 d . . .
C1 C 0.21958(16) 0.24513(18) 0.09725(10) 0.0249(3) Uani 1 1 d . . .
N2 N -0.24499(13) 0.19243(13) -0.26414(8) 0.0219(3) Uani 1 1 d . . .
C2 C -0.38851(17) 0.18117(19) -0.21667(11) 0.0253(3) Uani 1 1 d . . .
C3 C -0.33569(18) 0.2884(2) -0.12011(11) 0.0295(3) Uani 1 1 d . . .
C4 C -0.14646(18) 0.2759(2) -0.08871(11) 0.0291(3) Uani 1 1 d . . .
C5 C -0.09865(17) 0.17590(19) -0.17250(11) 0.0253(3) Uani 1 1 d . . .
C6 C -0.24947(19) 0.0529(2) -0.33997(12) 0.0296(3) Uani 1 1 d . . .
C7 C -0.24204(19) 0.3624(2) -0.31481(12) 0.0269(3) Uani 1 1 d . . .
H2A H -0.4790(19) 0.2202(18) -0.2645(11) 0.024(4) Uiso 1 1 d . . .
H3A H -0.3753(19) 0.416(2) -0.1356(12) 0.047(5) Uiso 1 1 d . . .
H4A H -0.0993(17) 0.392(2) -0.0818(11) 0.032(4) Uiso 1 1 d . . .
H5A H -0.004(2) 0.217(2) -0.1911(12) 0.036(4) Uiso 1 1 d . . .
H6A H -0.1556(17) 0.0659(19) -0.3646(10) 0.027(4) Uiso 1 1 d . . .
H7A H -0.1475(17) 0.3630(18) -0.3437(11) 0.025(4) Uiso 1 1 d . . .
H2B H -0.3948(16) 0.059(2) -0.2028(11) 0.027(4) Uiso 1 1 d . . .
H3B H -0.386(2) 0.241(2) -0.0696(14) 0.041(4) Uiso 1 1 d . . .
H4B H -0.108(2) 0.215(2) -0.0243(14) 0.038(4) Uiso 1 1 d . . .
H5B H -0.0888(15) 0.0555(19) -0.1582(10) 0.022(3) Uiso 1 1 d . . .
H6B H -0.2533(15) -0.054(2) -0.3070(10) 0.022(4) Uiso 1 1 d . . .
H7B H -0.2337(15) 0.449(2) -0.2663(11) 0.028(4) Uiso 1 1 d . . .
H6C H -0.3491(18) 0.070(2) -0.3941(12) 0.036(4) Uiso 1 1 d . . .
H7C H -0.3387(18) 0.3727(19) -0.3660(12) 0.029(4) Uiso 1 1 d . . .
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
S1 0.0312(2) 0.0437(3) 0.0281(2) -0.00118(16) 0.00983(16) 0.00292(16)
N1 0.0330(7) 0.0342(8) 0.0316(7) -0.0009(6) 0.0101(6) -0.0023(5)
C1 0.0231(7) 0.0230(7) 0.0260(8) 0.0028(6) 0.0013(6) -0.0031(6)
N2 0.0232(6) 0.0218(6) 0.0209(6) 0.0008(4) 0.0057(5) -0.0012(4)
C2 0.0192(7) 0.0314(8) 0.0260(8) 0.0020(6) 0.0068(6) -0.0007(6)
C3 0.0268(8) 0.0370(9) 0.0261(8) -0.0007(6) 0.0094(6) 0.0006(6)
C4 0.0272(8) 0.0348(9) 0.0242(8) 0.0002(6) 0.0045(6) 0.0004(6)
C5 0.0211(7) 0.0283(8) 0.0251(8) 0.0019(6) 0.0032(6) 0.0014(6)
C6 0.0339(8) 0.0272(8) 0.0289(8) -0.0043(7) 0.0101(7) -0.0023(7)
C7 0.0309(8) 0.0248(8) 0.0251(8) 0.0033(6) 0.0072(7) -0.0016(6)
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'
S S 0.1246 0.1234 '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
N1 C1 S1 178.92(13) . . ?
C6 N2 C7 109.10(11) . . ?
C6 N2 C2 111.79(11) . . ?
C7 N2 C2 110.95(11) . . ?
C6 N2 C5 112.24(10) . . ?
C7 N2 C5 110.41(10) . . ?
C2 N2 C5 102.23(10) . . ?
N2 C2 C3 104.37(11) . . ?
C2 C3 C4 104.90(12) . . ?
C5 C4 C3 106.03(12) . . ?
N2 C5 C4 105.05(11) . . ?
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
S1 C1 1.6448(15) . ?
N1 C1 1.1649(18) . ?
N2 C6 1.4952(18) . ?
N2 C7 1.4989(18) . ?
N2 C2 1.5101(18) . ?
N2 C5 1.5187(17) . ?
C2 C3 1.527(2) . ?
C3 C4 1.542(2) . ?
C4 C5 1.519(2) . ?
loop_
_cod_related_entry_id
_cod_related_entry_database
_cod_related_entry_code
1 ChemSpider 26945271
