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#$Date: 2016-03-24 03:31:49 +0200 (Thu, 24 Mar 2016) $
#$Revision: 179635 $
#$URL: svn://www.crystallography.net/cod/cif/4/50/99/4509990.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_4509990
loop_
_publ_author_name
'Yue, Cheng-Yang'
'Lei, Xiao-Wu'
'Ma, Yun-Xiang'
'Sheng, Ning'
'Yang, Ya-Dong'
'Liu, Guo-Dong'
'Zhai, Xiu-Rong'
_publ_section_title
;
 [TM(en)3][SnSb4S9] (TM = Ni, Co): 3D Chiral Framework of Mixed Main-Group
 Metals and [Mn(dien)2]2Sb4S9: 1D Chains with Mixed-Valent Sb Centers
;
_journal_issue                   1
_journal_name_full               'Crystal Growth & Design'
_journal_page_first              101
_journal_paper_doi               10.1021/cg401208p
_journal_volume                  14
_journal_year                    2014
_chemical_formula_sum            'C6 H24 N6 Ni S9 Sb4 Sn'
_chemical_formula_weight         1133.25
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           154
_symmetry_cell_setting           trigonal
_symmetry_space_group_name_Hall  'P 32 2"'
_symmetry_space_group_name_H-M   'P 32 2 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                 90.00
_cell_angle_gamma                120.00
_cell_formula_units_Z            3
_cell_length_a                   14.4328(8)
_cell_length_b                   14.4328(8)
_cell_length_c                   11.3654(13)
_cell_measurement_temperature    296(2)
_cell_volume                     2050.3(3)
_computing_cell_refinement       'APEX2 Software Suite (Bruker,2005)'
_computing_data_collection       'APEX2 Software Suite (Bruker,2005)'
_computing_data_reduction        'APEX2 Software Suite (Bruker,2005)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      296(2)
_diffrn_measured_fraction_theta_full 0.996
_diffrn_measured_fraction_theta_max 0.996
_diffrn_measurement_device_type  'Bruker SMART CCD area detector'
_diffrn_measurement_method       omega-scan
_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  0.0387
_diffrn_reflns_av_sigmaI/netI    0.0241
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_h_min       -18
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       14
_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_number            23936
_diffrn_reflns_theta_full        27.58
_diffrn_reflns_theta_max         27.58
_diffrn_reflns_theta_min         3.26
_exptl_absorpt_coefficient_mu    6.167
_exptl_absorpt_correction_T_max  0.5775
_exptl_absorpt_correction_T_min  0.4581
_exptl_absorpt_correction_type   multi-scan
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    2.753
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             1584
_exptl_crystal_size_max          0.15
_exptl_crystal_size_mid          0.10
_exptl_crystal_size_min          0.10
_refine_diff_density_max         2.389
_refine_diff_density_min         -0.600
_refine_diff_density_rms         0.094
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   -0.02(2)
_refine_ls_extinction_coef       ,
_refine_ls_extinction_method     SHELXL
_refine_ls_goodness_of_fit_ref   1.029
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     124
_refine_ls_number_reflns         3149
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.029
_refine_ls_R_factor_all          0.0240
_refine_ls_R_factor_gt           0.0206
_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)+(0.0156P)²+2.2126P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0409
_refine_ls_wR_factor_ref         0.0419
_reflns_number_gt                2939
_reflns_number_total             3149
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            cg401208p_si_002.cif
_cod_data_source_block           C6N6H24NiSnSb4S9
_cod_original_sg_symbol_H-M      P3221
_cod_database_code               4509990
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-y, x-y, z+2/3'
'-x+y, -x, z+1/3'
'y, x, -z'
'x-y, -y, -z+1/3'
'-x, -x+y, -z+2/3'
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
C1 C 0.1460(5) 0.0109(5) 0.7286(6) 0.0585(16) Uani 1 1 d .
H1 H 0.1039 -0.0555 0.7712 0.070 Uiso 1 1 calc .
H2 H 0.1178 0.0577 0.7471 0.070 Uiso 1 1 calc .
C2 C 0.5384(4) 0.1988(4) 0.7307(4) 0.0384(12) Uani 1 1 d .
H3 H 0.6116 0.2333 0.7588 0.046 Uiso 1 1 calc .
H4 H 0.5046 0.2372 0.7620 0.046 Uiso 1 1 calc .
C3 C 0.5365(4) 0.2000(4) 0.5989(4) 0.0378(12) Uani 1 1 d .
H5 H 0.5702 0.2731 0.5706 0.045 Uiso 1 1 calc .
H6 H 0.5758 0.1670 0.5678 0.045 Uiso 1 1 calc .
N1 N 0.2573(3) 0.0612(3) 0.7679(4) 0.0404(10) Uani 1 1 d .
H7 H 0.2596 0.0471 0.8447 0.048 Uiso 1 1 calc .
H8 H 0.2893 0.1326 0.7588 0.048 Uiso 1 1 calc .
N2 N 0.4791(3) 0.0850(3) 0.7700(3) 0.0369(10) Uani 1 1 d .
H9 H 0.4614 0.0815 0.8464 0.044 Uiso 1 1 calc .
H10 H 0.5209 0.0555 0.7618 0.044 Uiso 1 1 calc .
N3 N 0.2838(3) -0.1399(3) 0.7744(3) 0.0371(10) Uani 1 1 d .
H11 H 0.3000 -0.1209 0.8503 0.045 Uiso 1 1 calc .
H12 H 0.2123 -0.1812 0.7680 0.045 Uiso 1 1 calc .
Ni1 Ni 0.33907(6) 0.0000 0.6667 0.02587(17) Uani 1 2 d S
Sn1 Sn 0.0000 0.37244(3) 0.8333 0.02547(10) Uani 1 2 d S
Sb1 Sb 0.16352(3) 0.27372(3) 0.89136(3) 0.03373(8) Uani 1 1 d .
Sb2 Sb 0.36512(2) 0.43559(2) 0.64215(3) 0.02769(7) Uani 1 1 d .
S1 S 0.08083(10) 0.53375(9) 0.70286(10) 0.0303(2) Uani 1 1 d .
S2 S 0.08667(10) 0.27983(10) 0.70645(10) 0.0307(2) Uani 1 1 d .
S3 S 0.16895(10) 0.43560(11) 0.95585(10) 0.0351(3) Uani 1 1 d .
S4 S 0.34794(9) 0.33350(10) 0.82178(10) 0.0306(2) Uani 1 1 d .
S5 S 0.28660(11) 0.28660(11) 0.5000 0.0305(3) Uani 1 2 d S
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'
Ni Ni 0.3393 1.1124 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Sn Sn -0.6537 1.4246 '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
C1 C1 N1 112.4(4) 5_556 .
C1 C1 H1 109.1 5_556 .
N1 C1 H1 109.1 . .
C1 C1 H2 109.1 5_556 .
N1 C1 H2 109.1 . .
H1 C1 H2 107.8 . .
N2 C2 C3 107.9(4) . .
N2 C2 H3 110.1 . .
C3 C2 H3 110.1 . .
N2 C2 H4 110.1 . .
C3 C2 H4 110.1 . .
H3 C2 H4 108.4 . .
N3 C3 C2 108.7(4) 5_556 .
N3 C3 H5 110.0 5_556 .
C2 C3 H5 110.0 . .
N3 C3 H6 110.0 5_556 .
C2 C3 H6 110.0 . .
H5 C3 H6 108.3 . .
C1 N1 Ni1 109.1(3) . .
C1 N1 H7 109.9 . .
Ni1 N1 H7 109.9 . .
C1 N1 H8 109.9 . .
Ni1 N1 H8 109.9 . .
H7 N1 H8 108.3 . .
C2 N2 Ni1 109.1(3) . .
C2 N2 H9 109.9 . .
Ni1 N2 H9 109.9 . .
C2 N2 H10 109.9 . .
Ni1 N2 H10 109.9 . .
H9 N2 H10 108.3 . .
C3 N3 Ni1 108.5(3) 5_556 .
C3 N3 H11 110.0 5_556 .
Ni1 N3 H11 110.0 . .
C3 N3 H12 110.0 5_556 .
Ni1 N3 H12 110.0 . .
H11 N3 H12 108.4 . .
N2 Ni1 N2 96.7(2) . 5_556
N2 Ni1 N1 91.53(16) . .
N2 Ni1 N1 170.12(16) 5_556 .
N2 Ni1 N1 170.12(16) . 5_556
N2 Ni1 N1 91.53(16) 5_556 5_556
N1 Ni1 N1 80.9(2) . 5_556
N2 Ni1 N3 91.52(15) . .
N2 Ni1 N3 80.91(15) 5_556 .
N1 Ni1 N3 93.42(15) . .
N1 Ni1 N3 95.21(16) 5_556 .
N2 Ni1 N3 80.91(15) . 5_556
N2 Ni1 N3 91.52(15) 5_556 5_556
N1 Ni1 N3 95.21(16) . 5_556
N1 Ni1 N3 93.42(15) 5_556 5_556
N3 Ni1 N3 168.6(2) . 5_556
S1 Sn1 S1 91.60(5) . 6_556
S1 Sn1 S3 95.45(4) . 6_556
S1 Sn1 S3 94.21(4) 6_556 6_556
S1 Sn1 S3 94.21(4) . .
S1 Sn1 S3 95.45(4) 6_556 .
S3 Sn1 S3 166.13(6) 6_556 .
S1 Sn1 S2 91.64(4) . .
S1 Sn1 S2 176.30(4) 6_556 .
S3 Sn1 S2 87.27(4) 6_556 .
S3 Sn1 S2 82.53(4) . .
S1 Sn1 S2 176.30(4) . 6_556
S1 Sn1 S2 91.64(4) 6_556 6_556
S3 Sn1 S2 82.53(4) 6_556 6_556
S3 Sn1 S2 87.27(4) . 6_556
S2 Sn1 S2 85.18(5) . 6_556
S2 Sb1 S3 91.28(4) . .
S2 Sb1 S4 98.24(4) . .
S3 Sb1 S4 104.50(4) . .
S1 Sb2 S4 86.03(4) 5_666 .
S1 Sb2 S5 96.10(4) 5_666 .
S4 Sb2 S5 99.03(3) . .
Sb2 S1 Sn1 99.08(4) 5_566 .
Sb1 S2 Sn1 83.45(3) . .
Sb1 S3 Sn1 85.73(4) . .
Sb2 S4 Sb1 104.03(4) . .
Sb2 S5 Sb2 96.52(6) . 4_556
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
C1 C1 1.433(13) 5_556
C1 N1 1.463(7) .
C1 H1 0.9700 .
C1 H2 0.9700 .
C2 N2 1.492(6) .
C2 C3 1.498(7) .
C2 H3 0.9700 .
C2 H4 0.9700 .
C3 N3 1.482(6) 5_556
C3 H5 0.9700 .
C3 H6 0.9700 .
N1 Ni1 2.130(4) .
N1 H7 0.9000 .
N1 H8 0.9000 .
N2 Ni1 2.119(4) .
N2 H9 0.9000 .
N2 H10 0.9000 .
N3 C3 1.482(6) 5_556
N3 Ni1 2.145(4) .
N3 H11 0.9000 .
N3 H12 0.9000 .
Ni1 N2 2.119(4) 5_556
Ni1 N1 2.130(4) 5_556
Ni1 N3 2.145(4) 5_556
Sn1 S1 2.5028(12) .
Sn1 S1 2.5028(12) 6_556
Sn1 S3 2.5481(12) 6_556
Sn1 S3 2.5481(12) .
Sn1 S2 2.6652(12) .
Sn1 S2 2.6652(12) 6_556
Sb1 S2 2.3984(12) .
Sb1 S3 2.4123(13) .
Sb1 S4 2.4815(12) .
Sb2 S1 2.4389(12) 5_666
Sb2 S4 2.4565(11) .
Sb2 S5 2.4660(11) .
S1 Sb2 2.4389(12) 5_566
S5 Sb2 2.4660(11) 4_556
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
_geom_hbond_site_symmetry_A
N1 H7 S2 0.90 2.78 3.603(4) 153.1 3
N1 H8 S4 0.90 2.68 3.520(4) 155.8 .
N2 H9 S3 0.90 2.69 3.512(4) 151.9 4_557
N2 H10 S4 0.90 2.72 3.548(4) 153.4 6_656
N3 H11 S2 0.90 2.83 3.522(4) 134.6 3
N3 H11 S1 0.90 2.90 3.669(4) 144.6 3
N3 H12 S5 0.90 2.76 3.611(4) 159.1 3
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
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_4
N2 C2 C3 N3 55.7(5) . 5_556
C1 C1 N1 Ni1 -34.0(8) 5_556 .
C3 C2 N2 Ni1 -42.3(4) . .
C2 N2 Ni1 N2 106.0(3) . 5_556
C2 N2 Ni1 N1 -79.5(3) . .
C2 N2 Ni1 N1 -39.9(10) . 5_556
C2 N2 Ni1 N3 -172.9(3) . .
C2 N2 Ni1 N3 15.6(3) . 5_556
C1 N1 Ni1 N2 -174.8(4) . .
C1 N1 Ni1 N2 -28.6(11) . 5_556
C1 N1 Ni1 N1 11.5(3) . 5_556
C1 N1 Ni1 N3 -83.2(4) . .
C1 N1 Ni1 N3 104.1(4) . 5_556
C3 N3 Ni1 N2 -82.7(3) 5_556 .
C3 N3 Ni1 N2 13.8(3) 5_556 5_556
C3 N3 Ni1 N1 -174.3(3) 5_556 .
C3 N3 Ni1 N1 104.6(3) 5_556 5_556
C3 N3 Ni1 N3 -34.8(3) 5_556 5_556
S1 Sn1 S1 Sb2 -42.84(2) 6_556 5_566
S3 Sn1 S1 Sb2 51.54(5) 6_556 5_566
S3 Sn1 S1 Sb2 -138.42(4) . 5_566
S2 Sn1 S1 Sb2 138.95(4) . 5_566
S2 Sn1 S1 Sb2 108.2(6) 6_556 5_566
S3 Sb1 S2 Sn1 -30.98(4) . .
S4 Sb1 S2 Sn1 -135.83(4) . .
S1 Sn1 S2 Sb1 123.46(4) . .
S1 Sn1 S2 Sb1 -27.6(6) 6_556 .
S3 Sn1 S2 Sb1 -141.16(4) 6_556 .
S3 Sn1 S2 Sb1 29.43(4) . .
S2 Sn1 S2 Sb1 -58.43(3) 6_556 .
S2 Sb1 S3 Sn1 32.44(4) . .
S4 Sb1 S3 Sn1 131.29(4) . .
S1 Sn1 S3 Sb1 -120.23(4) . .
S1 Sn1 S3 Sb1 147.76(4) 6_556 .
S3 Sn1 S3 Sb1 13.8(2) 6_556 .
S2 Sn1 S3 Sb1 -29.13(4) . .
S2 Sn1 S3 Sb1 56.37(4) 6_556 .
S1 Sb2 S4 Sb1 179.10(5) 5_666 .
S5 Sb2 S4 Sb1 -85.34(4) . .
S2 Sb1 S4 Sb2 24.29(5) . .
S3 Sb1 S4 Sb2 -69.19(5) . .
S1 Sb2 S5 Sb2 -41.18(3) 5_666 4_556
S4 Sb2 S5 Sb2 -128.11(3) . 4_556
