#------------------------------------------------------------------------------
#$Date: 2016-02-21 02:03:34 +0200 (Sun, 21 Feb 2016) $
#$Revision: 176798 $
#$URL: svn://www.crystallography.net/cod/cif/2/23/45/2234570.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_2234570
loop_
_publ_author_name
'Xu, Qian'
_publ_section_title
;
 Bis(2-methylpiperidinium) pentachloridoantimonate(III)
;
_journal_coeditor_code           CV5279
_journal_issue                   5
_journal_name_full               'Acta Crystallographica Section E'
_journal_page_first              m671
_journal_paper_doi               10.1107/S1600536812017163
_journal_volume                  68
_journal_year                    2012
_chemical_formula_iupac          '(C6 H14 N)2 [Sb Cl5]'
_chemical_formula_moiety         '2(C6 H14 N +), Cl5 Sb 2-'
_chemical_formula_sum            'C12 H28 Cl5 N2 Sb'
_chemical_formula_weight         499.36
_chemical_name_systematic
;
Bis(2-methylpiperidinium) pentachloridoantimonate(III)
;
_space_group_IT_number           62
_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_Hall  '-P 2ac 2n'
_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                   7.5995(15)
_cell_length_b                   23.165(5)
_cell_length_c                   11.453(2)
_cell_measurement_reflns_used    2361
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      27.480
_cell_measurement_theta_min      2.2
_cell_volume                     2016.2(7)
_computing_cell_refinement
'SCXmini Benchtop Crystallography System Software (Rigaku, 2006)'
_computing_data_collection
'SCXmini Benchtop Crystallography System Software (Rigaku, 2006)'
_computing_data_reduction
'SCXmini Benchtop Crystallography System Software (Rigaku, 2006)'
_computing_molecular_graphics    'DIAMOND (Brandenburg & Putz, 2005)'
_computing_publication_material  'SHELXL97 (Sheldrick, 2008)'
_computing_structure_refinement  'SHELXL97 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device_type  'Rigaku Mercury70 CCD'
_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  0.0609
_diffrn_reflns_av_sigmaI/netI    0.0316
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_k_max       30
_diffrn_reflns_limit_k_min       -30
_diffrn_reflns_limit_l_max       14
_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_number            19754
_diffrn_reflns_theta_full        27.47
_diffrn_reflns_theta_max         27.47
_diffrn_reflns_theta_min         3.18
_exptl_absorpt_coefficient_mu    2.025
_exptl_absorpt_correction_T_max  0.558
_exptl_absorpt_correction_T_min  0.421
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   '(CrystalClear; Rigaku, 2005)'
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.645
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             1000
_exptl_crystal_size_max          0.2800
_exptl_crystal_size_mid          0.2500
_exptl_crystal_size_min          0.2100
_refine_diff_density_max         0.577
_refine_diff_density_min         -0.519
_refine_ls_extinction_coef       0
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.075
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     98
_refine_ls_number_reflns         2361
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.075
_refine_ls_R_factor_all          0.0459
_refine_ls_R_factor_gt           0.0331
_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)+(0.0181P)²+1.8699P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0615
_refine_ls_wR_factor_ref         0.0652
_reflns_number_gt                1938
_reflns_number_total             2361
_reflns_threshold_expression     I>2sigma(I)
_cod_data_source_file            cv5279.cif
_cod_data_source_block           I
_cod_database_code               2234570
_cod_database_fobs_code          2234570
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x+1/2, -y, z+1/2'
'x+1/2, -y+1/2, -z+1/2'
'-x, y+1/2, -z'
'-x, -y, -z'
'x-1/2, y, -z-1/2'
'-x-1/2, y-1/2, z-1/2'
'x, -y-1/2, z'
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
_atom_site_symmetry_multiplicity
C C1 0.8199(5) 0.1245(2) -0.1957(3) 0.0703(12) Uani d . 1 1
H H1A 0.7817 0.1631 -0.2129 0.105 Uiso calc R 1 1
H H1B 0.7841 0.0991 -0.2575 0.105 Uiso calc R 1 1
H H1C 0.9457 0.1238 -0.1887 0.105 Uiso calc R 1 1
C C2 0.7387(5) 0.10494(17) -0.0830(3) 0.0554(10) Uani d . 1 1
H H2 0.6106 0.1081 -0.0900 0.066 Uiso calc R 1 1
C C3 0.7834(6) 0.04338(18) -0.0511(4) 0.0750(13) Uani d . 1 1
H H3A 0.7347 0.0177 -0.1098 0.090 Uiso calc R 1 1
H H3B 0.9103 0.0388 -0.0519 0.090 Uiso calc R 1 1
C C4 0.7143(7) 0.0260(2) 0.0672(4) 0.0866(15) Uani d . 1 1
H H4A 0.7536 -0.0128 0.0855 0.104 Uiso calc R 1 1
H H4B 0.5866 0.0259 0.0659 0.104 Uiso calc R 1 1
C C5 0.7785(6) 0.06724(18) 0.1599(4) 0.0707(12) Uani d . 1 1
H H5A 0.7284 0.0566 0.2348 0.085 Uiso calc R 1 1
H H5B 0.9055 0.0647 0.1661 0.085 Uiso calc R 1 1
C C6 0.7275(5) 0.12723(16) 0.1310(3) 0.0552(10) Uani d . 1 1
H H6A 0.7741 0.1534 0.1895 0.066 Uiso calc R 1 1
H H6B 0.6002 0.1306 0.1314 0.066 Uiso calc R 1 1
N N1 0.7977(4) 0.14369(12) 0.0122(3) 0.0499(7) Uani d . 1 1
H H1D 0.7632 0.1799 -0.0044 0.060 Uiso calc R 1 1
H H1E 0.9160 0.1435 0.0147 0.060 Uiso calc R 1 1
Cl Cl1 0.73805(11) 0.13613(4) 0.45405(8) 0.0508(2) Uani d . 1 1
Cl Cl2 0.58634(15) 0.2500 0.61136(10) 0.0463(3) Uani d S 1 2
Cl Cl3 1.05345(15) 0.2500 0.57047(11) 0.0489(3) Uani d S 1 2
Cl Cl4 0.48085(16) 0.2500 0.31467(11) 0.0529(3) Uani d S 1 2
Sb Sb1 0.76256(3) 0.2500 0.44041(2) 0.03097(9) Uani d S 1 2
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'
Cl Cl 0.1484 0.1585 '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'
O O 0.0106 0.0060 '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_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle
C2 C1 H1A . . 109.5
C2 C1 H1B . . 109.5
H1A C1 H1B . . 109.5
C2 C1 H1C . . 109.5
H1A C1 H1C . . 109.5
H1B C1 H1C . . 109.5
N1 C2 C1 . . 109.0(3)
N1 C2 C3 . . 109.0(3)
C1 C2 C3 . . 113.6(3)
N1 C2 H2 . . 108.4
C1 C2 H2 . . 108.4
C3 C2 H2 . . 108.4
C4 C3 C2 . . 113.0(4)
C4 C3 H3A . . 109.0
C2 C3 H3A . . 109.0
C4 C3 H3B . . 109.0
C2 C3 H3B . . 109.0
H3A C3 H3B . . 107.8
C3 C4 C5 . . 110.5(4)
C3 C4 H4A . . 109.6
C5 C4 H4A . . 109.6
C3 C4 H4B . . 109.6
C5 C4 H4B . . 109.6
H4A C4 H4B . . 108.1
C6 C5 C4 . . 110.6(4)
C6 C5 H5A . . 109.5
C4 C5 H5A . . 109.5
C6 C5 H5B . . 109.5
C4 C5 H5B . . 109.5
H5A C5 H5B . . 108.1
C5 C6 N1 . . 110.3(3)
C5 C6 H6A . . 109.6
N1 C6 H6A . . 109.6
C5 C6 H6B . . 109.6
N1 C6 H6B . . 109.6
H6A C6 H6B . . 108.1
C2 N1 C6 . . 113.8(3)
C2 N1 H1D . . 108.8
C6 N1 H1D . . 108.8
C2 N1 H1E . . 108.8
C6 N1 H1E . . 108.8
H1D N1 H1E . . 107.7
Cl2 Sb1 Cl4 . . 89.56(5)
Cl2 Sb1 Cl1 . . 84.93(2)
Cl4 Sb1 Cl1 . . 88.54(2)
Cl2 Sb1 Cl1 . 8_565 84.93(2)
Cl4 Sb1 Cl1 . 8_565 88.542(19)
Cl1 Sb1 Cl1 . 8_565 169.47(4)
Cl2 Sb1 Cl3 . . 90.40(4)
Cl4 Sb1 Cl3 . . 179.96(4)
Cl1 Sb1 Cl3 . . 91.454(19)
Cl1 Sb1 Cl3 8_565 . 91.454(19)
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_site_symmetry_2
_geom_bond_distance
C1 C2 . 1.500(5)
C1 H1A . 0.9600
C1 H1B . 0.9600
C1 H1C . 0.9600
C2 N1 . 1.481(4)
C2 C3 . 1.511(6)
C2 H2 . 0.9800
C3 C4 . 1.509(6)
C3 H3A . 0.9700
C3 H3B . 0.9700
C4 C5 . 1.510(6)
C4 H4A . 0.9700
C4 H4B . 0.9700
C5 C6 . 1.480(5)
C5 H5A . 0.9700
C5 H5B . 0.9700
C6 N1 . 1.511(5)
C6 H6A . 0.9700
C6 H6B . 0.9700
N1 H1D . 0.9000
N1 H1E . 0.9000
Cl1 Sb1 . 2.6491(10)
Cl2 Sb1 . 2.3721(11)
Cl3 Sb1 . 2.6656(12)
Cl4 Sb1 . 2.5802(12)
Sb1 Cl1 8_565 2.6491(10)
loop_
_geom_hbond_atom_site_label_D
_geom_hbond_atom_site_label_H
_geom_hbond_atom_site_label_A
_geom_hbond_site_symmetry_A
_geom_hbond_distance_DH
_geom_hbond_distance_HA
_geom_hbond_distance_DA
_geom_hbond_angle_DHA
N1 H1D Cl3 6_556 0.90 2.40 3.226(3) 153.1
N1 H1E Cl1 6_656 0.90 2.48 3.373(3) 172.6
loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
N1 C2 C3 C4 53.2(5)
C1 C2 C3 C4 175.0(4)
C2 C3 C4 C5 -55.2(6)
C3 C4 C5 C6 56.5(5)
C4 C5 C6 N1 -56.7(5)
C1 C2 N1 C6 -178.6(3)
C3 C2 N1 C6 -54.0(4)
C5 C6 N1 C2 57.2(4)
