#------------------------------------------------------------------------------
#$Date: 2016-02-21 02:03:34 +0200 (Sun, 21 Feb 2016) $
#$Revision: 176798 $
#$URL: svn://www.crystallography.net/cod/cif/2/23/96/2239657.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_2239657
loop_
_publ_author_name
'Soury, Raoudha'
'Belkhiria, Mohamed Salah'
'Giorgi, Michel'
'Nasri, Habib'
_publ_section_title
;
 Dichlorido(5,10,15,20-tetraphenylporphyrinato-κ⁴N)antimony(V)
 hexachloridoantimonate(V)
;
_journal_issue                   7
_journal_name_full               'Acta Crystallographica Section E'
_journal_page_first              m256
_journal_page_last               m257
_journal_paper_doi               10.1107/S1600536814012653
_journal_volume                  70
_journal_year                    2014
_chemical_formula_iupac          '[Sb (C44 H28 N4) Cl2] [Sb Cl6]'
_chemical_formula_moiety         'C44 H28 Cl2 N4 Sb +, Cl6 Sb -'
_chemical_formula_sum            'C44 H28 Cl8 N4 Sb2'
_chemical_formula_weight         1139.80
_chemical_name_systematic
;
Dichlorido(5,10,15,20-tetraphenylporphyrinato-κ⁴N)antimony(V)
hexachloridoantimonate(V)
;
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                70.685(2)
_cell_angle_beta                 83.398(2)
_cell_angle_gamma                63.050(3)
_cell_formula_units_Z            1
_cell_length_a                   10.2044(4)
_cell_length_b                   11.1242(4)
_cell_length_c                   11.3901(4)
_cell_measurement_reflns_used    22201
_cell_measurement_temperature    223(2)
_cell_measurement_theta_max      30.081
_cell_measurement_theta_min      1.896
_cell_volume                     1086.73(8)
_computing_cell_refinement       'DENZO/SCALEPACK (Otwinowski & Minor, 1997)'
_computing_data_collection       'COLLECT (Nonius, 2002)'
_computing_data_reduction        'DENZO/SCALEPACK (Otwinowski & Minor, 1997)'
_computing_molecular_graphics    'ORTEP-3 for Windows (Farrugia, 2012)'
_computing_publication_material  'SHELXL97 (Sheldrick, 2008)'
_computing_structure_refinement  'SHELXL97 (Sheldrick, 2008)'
_computing_structure_solution    'SIR2004 (Burla et al., 2005)'
_diffrn_ambient_temperature      223(2)
_diffrn_measured_fraction_theta_full 0.990
_diffrn_measured_fraction_theta_max 0.990
_diffrn_measurement_device_type  'Bruker--Nonius KappaCCD'
_diffrn_measurement_method       'φ & 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  0.1243
_diffrn_reflns_av_sigmaI/netI    0.0716
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       14
_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_number            19871
_diffrn_reflns_theta_full        26.73
_diffrn_reflns_theta_max         27.10
_diffrn_reflns_theta_min         1.90
_exptl_absorpt_coefficient_mu    1.773
_exptl_absorpt_correction_T_max  0.773
_exptl_absorpt_correction_T_min  0.723
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
(SORTAV; Blessing, 1995)
;
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    1.742
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             558
_exptl_crystal_size_max          0.2
_exptl_crystal_size_mid          0.16
_exptl_crystal_size_min          0.12
_refine_diff_density_max         2.550
_refine_diff_density_min         -1.452
_refine_ls_extinction_coef       0.042(4)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4^
_refine_ls_extinction_method     'SHELXL97 (Sheldrick, 2008)'
_refine_ls_goodness_of_fit_ref   1.132
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     266
_refine_ls_number_reflns         4749
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.132
_refine_ls_R_factor_all          0.0692
_refine_ls_R_factor_gt           0.0651
_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)+(0.0507P)²+7.0167P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1693
_refine_ls_wR_factor_ref         0.1726
_reflns_number_gt                4433
_reflns_number_total             4749
_reflns_threshold_expression     I>2σ(I)
_cod_data_source_file            is5356sup1.cf
_cod_data_source_block           I
_cod_original_cell_volume        1086.73(7)
_cod_database_code               2239657
_cod_database_fobs_code          2239657
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, -y, -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
Sb Sb1 0.5000 0.0000 0.5000 0.0226(2) Uani d S 1 2
N N1 0.4725(5) 0.1913(5) 0.3693(4) 0.0259(9) Uani d . 1 1
N N2 0.3841(5) 0.1056(5) 0.6238(4) 0.0261(9) Uani d . 1 1
Cl Cl1 0.28107(16) 0.02557(17) 0.42325(15) 0.0368(4) Uani d . 1 1
C C1 0.5256(6) 0.2093(6) 0.2499(5) 0.0278(11) Uani d . 1 1
C C2 0.4834(7) 0.3574(7) 0.1912(6) 0.0358(13) Uani d . 1 1
H H2 0.5047 0.3994 0.1098 0.043 Uiso calc R 1 1
C C3 0.4073(7) 0.4267(6) 0.2732(5) 0.0317(12) Uani d . 1 1
H H3 0.3669 0.5251 0.2589 0.038 Uiso calc R 1 1
C C4 0.3993(6) 0.3234(6) 0.3857(5) 0.0270(11) Uani d . 1 1
C C5 0.3287(6) 0.3531(5) 0.4932(5) 0.0265(11) Uani d . 1 1
C C6 0.3224(6) 0.2509(6) 0.6023(5) 0.0273(11) Uani d . 1 1
C C7 0.2497(6) 0.2797(6) 0.7118(6) 0.0312(12) Uani d . 1 1
H H7 0.1987 0.3696 0.7229 0.037 Uiso calc R 1 1
C C8 0.2678(7) 0.1537(7) 0.7969(6) 0.0341(13) Uani d . 1 1
H H8 0.2310 0.1416 0.8774 0.041 Uiso calc R 1 1
C C9 0.3518(7) 0.0429(6) 0.7440(5) 0.0292(11) Uani d . 1 1
C C10 0.3941(6) -0.1013(6) 0.8037(5) 0.0286(11) Uani d . 1 1
C C11 0.2526(6) 0.5050(6) 0.4938(5) 0.0287(11) Uani d . 1 1
C C12 0.1165(7) 0.5944(6) 0.4362(6) 0.0322(12) Uani d . 1 1
H H12 0.0745 0.5636 0.3899 0.039 Uiso calc R 1 1
C C13 0.0393(7) 0.7315(7) 0.4458(7) 0.0396(14) Uani d . 1 1
H H13 -0.0549 0.7946 0.4082 0.047 Uiso calc R 1 1
C C14 0.1080(8) 0.7667(9) 0.5117(6) 0.0467(17) Uani d . 1 1
H H14 0.0566 0.8583 0.5192 0.056 Uiso calc R 1 1
C C15 0.2426(8) 0.6865(7) 0.5688(8) 0.0437(16) Uani d . 1 1
H H15 0.2841 0.7212 0.6114 0.052 Uiso calc R 1 1
C C16 0.3165(8) 0.5489(7) 0.5611(7) 0.0427(15) Uani d . 1 1
H H16 0.4093 0.4865 0.6015 0.051 Uiso calc R 1 1
C C17 0.3501(6) -0.1422(6) 0.9394(6) 0.0314(12) Uani d . 1 1
C C18 0.2256(10) -0.1633(11) 0.9654(7) 0.059(2) Uani d . 1 1
H H18 0.1746 -0.1651 0.9028 0.070 Uiso calc R 1 1
C C19 0.1769(11) -0.1821(12) 1.0868(8) 0.070(3) Uani d . 1 1
H H19 0.0911 -0.1949 1.1067 0.084 Uiso calc R 1 1
C C20 0.2564(10) -0.1816(8) 1.1781(7) 0.054(2) Uani d . 1 1
H H20 0.2231 -0.1922 1.2596 0.064 Uiso calc R 1 1
C C21 0.3802(12) -0.1662(12) 1.1503(7) 0.068(3) Uani d . 1 1
H H21 0.4348 -0.1698 1.2136 0.081 Uiso calc R 1 1
C C22 0.4296(10) -0.1447(11) 1.0289(7) 0.054(2) Uani d . 1 1
H H22 0.5156 -0.1323 1.0096 0.065 Uiso calc R 1 1
Sb Sb2 0.0000 0.5000 1.0000 0.0698(4) Uani d S 1 2
Cl Cl2 -0.2299(3) 0.5140(4) 1.0805(3) 0.0961(11) Uani d . 1 1
Cl Cl3 0.0724(3) 0.4837(5) 1.1918(3) 0.1218(17) Uani d . 1 1
Cl Cl4 0.0999(5) 0.2463(5) 1.0692(4) 0.1156(13) Uani d . 1 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'
N N 0.0061 0.0033 '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'
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
N2 Sb1 N2 2_656 . 180.00(16)
N2 Sb1 N1 2_656 . 90.19(18)
N2 Sb1 N1 . . 89.81(18)
N2 Sb1 N1 2_656 2_656 89.81(18)
N2 Sb1 N1 . 2_656 90.19(18)
N1 Sb1 N1 . 2_656 180.0(2)
N2 Sb1 Cl1 2_656 2_656 90.57(14)
N2 Sb1 Cl1 . 2_656 89.43(14)
N1 Sb1 Cl1 . 2_656 89.98(14)
N1 Sb1 Cl1 2_656 2_656 90.02(14)
N2 Sb1 Cl1 2_656 . 89.43(14)
N2 Sb1 Cl1 . . 90.57(14)
N1 Sb1 Cl1 . . 90.02(14)
N1 Sb1 Cl1 2_656 . 89.98(14)
Cl1 Sb1 Cl1 2_656 . 180.0
C4 N1 C1 . . 108.0(4)
C4 N1 Sb1 . . 126.0(4)
C1 N1 Sb1 . . 126.0(4)
C6 N2 C9 . . 108.0(4)
C6 N2 Sb1 . . 126.3(4)
C9 N2 Sb1 . . 125.6(4)
N1 C1 C10 . 2_656 126.1(5)
N1 C1 C2 . . 107.9(5)
C10 C1 C2 2_656 . 126.0(5)
C3 C2 C1 . . 108.1(5)
C3 C2 H2 . . 125.9
C1 C2 H2 . . 125.9
C2 C3 C4 . . 107.9(5)
C2 C3 H3 . . 126.0
C4 C3 H3 . . 126.0
N1 C4 C5 . . 126.6(5)
N1 C4 C3 . . 108.1(5)
C5 C4 C3 . . 125.4(5)
C6 C5 C4 . . 124.6(5)
C6 C5 C11 . . 116.2(5)
C4 C5 C11 . . 119.2(5)
N2 C6 C5 . . 126.6(5)
N2 C6 C7 . . 108.1(5)
C5 C6 C7 . . 125.3(5)
C8 C7 C6 . . 107.7(5)
C8 C7 H7 . . 126.2
C6 C7 H7 . . 126.2
C7 C8 C9 . . 108.7(5)
C7 C8 H8 . . 125.7
C9 C8 H8 . . 125.7
C10 C9 N2 . . 127.0(5)
C10 C9 C8 . . 125.5(5)
N2 C9 C8 . . 107.5(5)
C9 C10 C1 . 2_656 125.1(5)
C9 C10 C17 . . 116.2(5)
C1 C10 C17 2_656 . 118.7(5)
C12 C11 C16 . . 120.6(6)
C12 C11 C5 . . 120.1(5)
C16 C11 C5 . . 119.1(5)
C11 C12 C13 . . 120.5(6)
C11 C12 H12 . . 119.8
C13 C12 H12 . . 119.8
C14 C13 C12 . . 115.6(7)
C14 C13 H13 . . 122.2
C12 C13 H13 . . 122.2
C13 C14 C15 . . 127.7(8)
C13 C14 H14 . . 116.2
C15 C14 H14 . . 116.2
C14 C15 C16 . . 116.0(7)
C14 C15 H15 . . 122.0
C16 C15 H15 . . 122.0
C11 C16 C15 . . 119.6(6)
C11 C16 H16 . . 120.2
C15 C16 H16 . . 120.2
C22 C17 C18 . . 122.1(6)
C22 C17 C10 . . 118.2(6)
C18 C17 C10 . . 119.5(6)
C17 C18 C19 . . 118.5(8)
C17 C18 H18 . . 120.7
C19 C18 H18 . . 120.7
C20 C19 C18 . . 119.4(8)
C20 C19 H19 . . 120.3
C18 C19 H19 . . 120.3
C21 C20 C19 . . 120.4(7)
C21 C20 H20 . . 119.8
C19 C20 H20 . . 119.8
C20 C21 C22 . . 121.1(8)
C20 C21 H21 . . 119.4
C22 C21 H21 . . 119.4
C17 C22 C21 . . 118.4(7)
C17 C22 H22 . . 120.8
C21 C22 H22 . . 120.8
Cl3 Sb2 Cl3 . 2_567 180.0000(10)
Cl3 Sb2 Cl2 . 2_567 90.36(11)
Cl3 Sb2 Cl2 2_567 2_567 89.64(11)
Cl3 Sb2 Cl2 . . 89.64(11)
Cl3 Sb2 Cl2 2_567 . 90.36(11)
Cl2 Sb2 Cl2 2_567 . 180.0
Cl3 Sb2 Cl4 . . 87.99(16)
Cl3 Sb2 Cl4 2_567 . 92.01(16)
Cl2 Sb2 Cl4 2_567 . 90.45(14)
Cl2 Sb2 Cl4 . . 89.55(14)
Cl3 Sb2 Cl4 . 2_567 92.01(16)
Cl3 Sb2 Cl4 2_567 2_567 87.99(16)
Cl2 Sb2 Cl4 2_567 2_567 89.55(14)
Cl2 Sb2 Cl4 . 2_567 90.45(14)
Cl4 Sb2 Cl4 . 2_567 180.0000(10)
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_site_symmetry_2
_geom_bond_distance
Sb1 N2 2_656 2.054(4)
Sb1 N2 . 2.054(4)
Sb1 N1 . 2.070(4)
Sb1 N1 2_656 2.070(4)
Sb1 Cl1 2_656 2.3547(14)
Sb1 Cl1 . 2.3547(14)
N1 C4 . 1.380(7)
N1 C1 . 1.390(7)
N2 C6 . 1.386(7)
N2 C9 . 1.394(7)
C1 C10 2_656 1.402(8)
C1 C2 . 1.429(8)
C2 C3 . 1.356(9)
C2 H2 . 0.9400
C3 C4 . 1.434(8)
C3 H3 . 0.9400
C4 C5 . 1.406(8)
C5 C6 . 1.398(8)
C5 C11 . 1.508(7)
C6 C7 . 1.430(8)
C7 C8 . 1.359(9)
C7 H7 . 0.9400
C8 C9 . 1.426(8)
C8 H8 . 0.9400
C9 C10 . 1.393(8)
C10 C1 2_656 1.402(8)
C10 C17 . 1.536(8)
C11 C12 . 1.369(8)
C11 C16 . 1.379(9)
C12 C13 . 1.400(8)
C12 H12 . 0.9400
C13 C14 . 1.332(10)
C13 H13 . 0.9400
C14 C15 . 1.347(10)
C14 H14 . 0.9400
C15 C16 . 1.396(9)
C15 H15 . 0.9400
C16 H16 . 0.9400
C17 C22 . 1.359(10)
C17 C18 . 1.377(10)
C18 C19 . 1.395(11)
C18 H18 . 0.9400
C19 C20 . 1.394(14)
C19 H19 . 0.9400
C20 C21 . 1.339(13)
C20 H20 . 0.9400
C21 C22 . 1.398(10)
C21 H21 . 0.9400
C22 H22 . 0.9400
Sb2 Cl3 . 2.311(3)
Sb2 Cl3 2_567 2.311(3)
Sb2 Cl2 2_567 2.374(2)
Sb2 Cl2 . 2.374(2)
Sb2 Cl4 . 2.393(4)
Sb2 Cl4 2_567 2.393(4)
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
_geom_hbond_publ_flag
C7 H7 Cl3 2_567 0.94 2.76 3.490(8) 135 yes
C8 H8 Cl4 . 0.94 2.74 3.593(8) 151 yes
C12 H12 Cl3 1_554 0.94 2.69 3.539(8) 151 yes
