#------------------------------------------------------------------------------
#$Date: 2016-03-24 01:31:19 +0200 (Thu, 24 Mar 2016) $
#$Revision: 179533 $
#$URL: svn://www.crystallography.net/cod/cif/4/50/02/4500246.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_4500246
loop_
_publ_author_name
'Zheng, Xiao-Dan'
'Hua, Yan-Long'
'Xiong, Ren-Gen'
'Ge, Jia-Zhen'
'Lu, Tong-Bu'
_publ_section_title
;
 Cyano-Bridged Homochiral Heterometallic Helical Complexes: Synthesis,
 Structures, Magnetic and Dielectric Properties
;
_journal_issue                   1
_journal_name_full               'Crystal Growth & Design'
_journal_page_first              302
_journal_paper_doi               10.1021/cg101314j
_journal_volume                  11
_journal_year                    2011
_chemical_absolute_configuration ad
_chemical_formula_sum            'C21 H38 Fe N10 Ni O2'
_chemical_formula_weight         577.13
_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                   10.2272(6)
_cell_length_b                   10.2272(6)
_cell_length_c                   23.3035(14)
_cell_measurement_reflns_used    4254
_cell_measurement_temperature    153(2)
_cell_measurement_theta_max      27.2
_cell_measurement_theta_min      3.9
_cell_volume                     2110.9(2)
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      153(2)
_diffrn_measured_fraction_theta_full 0.987
_diffrn_measured_fraction_theta_max 0.987
_diffrn_measurement_device_type  'Rigaku RAXIS-RAPID Imaging Plate'
_diffrn_measurement_method       Ω
_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  0.0370
_diffrn_reflns_av_sigmaI/netI    0.0365
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -30
_diffrn_reflns_number            12995
_diffrn_reflns_theta_full        27.48
_diffrn_reflns_theta_max         27.48
_diffrn_reflns_theta_min         3.49
_exptl_absorpt_coefficient_mu    1.220
_exptl_absorpt_correction_T_max  0.910
_exptl_absorpt_correction_T_min  0.7925
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   Higashi,T.(1995).
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    1.362
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       needle
_exptl_crystal_F_000             912
_exptl_crystal_size_max          0.48
_exptl_crystal_size_mid          0.15
_exptl_crystal_size_min          0.09
_refine_diff_density_max         0.439
_refine_diff_density_min         -0.270
_refine_diff_density_rms         0.055
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   -0.019(13)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.036
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     162
_refine_ls_number_reflns         3198
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.036
_refine_ls_R_factor_all          0.0309
_refine_ls_R_factor_gt           0.0279
_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)+(0.0347P)²+0.2012P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0646
_refine_ls_wR_factor_ref         0.0659
_reflns_number_gt                2981
_reflns_number_total             3198
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            cg101314j_si_002.cif
_cod_data_source_block           L-3
_cod_depositor_comments
;
The following automatic conversions were performed:

'_exptl_absorpt_correction_type' value 'MULTI-SCAN' changed to
'multi-scan' according to
/home/saulius/struct/CIF-dictionaries/cif_core.dic dictionary named
'cif_core.dic' version 2.4.1 from 2010-06-29.

Automatic conversion script
Id: cif_fix_values 1715 2011-07-08 13:25:40Z adriana 
;
_cod_original_sg_symbol_H-M      P3221
_cod_database_code               4500246
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, -x+y, -z+2/3'
'x-y, -y, -z+1/3'
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 0.4513(2) -0.0497(2) 0.27356(9) 0.0294(5) Uani 1 1 d .
H1A H 0.3804 -0.0372 0.2973 0.035 Uiso 1 1 calc R
H1B H 0.5321 -0.0411 0.2979 0.035 Uiso 1 1 calc R
C2 C 0.5756(2) 0.2037(2) 0.08804(10) 0.0313(5) Uani 1 1 d .
H2A H 0.6635 0.2186 0.1093 0.038 Uiso 1 1 calc R
H2B H 0.6093 0.2811 0.0587 0.038 Uiso 1 1 calc R
C3 C 0.5463(2) 0.3600(2) 0.16355(10) 0.0284(4) Uani 1 1 d .
C4 C 0.6404(2) 0.4997(2) 0.12535(11) 0.0364(6) Uani 1 1 d .
H4A H 0.5756 0.5083 0.0977 0.055 Uiso 1 1 calc R
H4B H 0.7170 0.4887 0.1058 0.055 Uiso 1 1 calc R
H4C H 0.6870 0.5887 0.1488 0.055 Uiso 1 1 calc R
C5 C 0.4231(2) 0.3797(2) 0.19249(11) 0.0353(5) Uani 1 1 d .
H5A H 0.3629 0.2942 0.2166 0.053 Uiso 1 1 calc R
H5B H 0.3602 0.3875 0.1637 0.053 Uiso 1 1 calc R
H5C H 0.4689 0.4699 0.2153 0.053 Uiso 1 1 calc R
C6 C 0.6508(2) 0.3473(2) 0.20795(9) 0.0300(4) Uani 1 1 d .
H6A H 0.7255 0.3347 0.1868 0.036 Uiso 1 1 calc R
H6B H 0.7045 0.4436 0.2276 0.036 Uiso 1 1 calc R
C7 C 0.5852(2) 0.2243(2) 0.25397(9) 0.0290(4) Uani 1 1 d .
H7A H 0.5085 0.2342 0.2756 0.035 Uiso 1 1 calc R
C8 C 0.7140(3) 0.2512(3) 0.29491(10) 0.0393(5) Uani 1 1 d .
H8A H 0.6758 0.1755 0.3244 0.059 Uiso 1 1 calc R
H8B H 0.7549 0.3493 0.3121 0.059 Uiso 1 1 calc R
H8C H 0.7917 0.2457 0.2738 0.059 Uiso 1 1 calc R
C9 C 0.1284(2) 0.0054(2) 0.26625(9) 0.0244(4) Uani 1 1 d .
C10 C 0.1781(2) 0.0296(2) 0.38184(10) 0.0294(5) Uani 1 1 d .
C11 C 0.0000 -0.2325(3) 0.3333 0.0257(6) Uani 1 2 d S
Fe1 Fe 0.0000 -0.04213(4) 0.3333 0.02132(10) Uani 1 2 d S
N1 N 0.51387(18) 0.06921(18) 0.22875(7) 0.0235(3) Uani 1 1 d .
H1C H 0.5896 0.0617 0.2115 0.028 Uiso 1 1 calc R
N2 N 0.46989(17) 0.21896(18) 0.12765(8) 0.0238(4) Uani 1 1 d .
H2C H 0.4043 0.2302 0.1047 0.029 Uiso 1 1 calc R
N3 N 0.20722(18) 0.02948(18) 0.22797(8) 0.0252(4) Uani 1 1 d .
N4 N 0.2826(2) 0.0735(2) 0.41103(10) 0.0444(5) Uani 1 1 d .
N5 N 0.0000 -0.3451(3) 0.3333 0.0397(7) Uani 1 2 d S
N6 N 0.0000 0.1199(2) 0.3333 0.0302(6) Uani 1 2 d S
Ni1 Ni 0.33956(3) 0.0000 0.1667 0.01944(9) Uani 1 2 d S
O1 O 0.0000 0.2316(2) 0.3333 0.0607(9) Uani 1 2 d S
O1W O 0.7308(2) 0.0000 0.1667 0.0592(8) Uani 1 2 d S
H1WA H 0.8220 0.0572 0.1565 0.089 Uiso 1 1 d R
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'
Fe Fe 0.3463 0.8444 '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'
Ni Ni 0.3393 1.1124 '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'
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
N1 C1 C2 109.48(17) . 6
N1 C1 H1A 109.8 . .
C2 C1 H1A 109.8 6 .
N1 C1 H1B 109.8 . .
C2 C1 H1B 109.8 6 .
H1A C1 H1B 108.2 . .
N2 C2 C1 111.36(16) . 6
N2 C2 H2A 109.4 . .
C1 C2 H2A 109.4 6 .
N2 C2 H2B 109.4 . .
C1 C2 H2B 109.4 6 .
H2A C2 H2B 108.0 . .
N2 C3 C5 107.73(16) . .
N2 C3 C6 110.04(16) . .
C5 C3 C6 111.6(2) . .
N2 C3 C4 110.54(19) . .
C5 C3 C4 107.81(17) . .
C6 C3 C4 109.14(16) . .
C3 C4 H4A 109.5 . .
C3 C4 H4B 109.5 . .
H4A C4 H4B 109.5 . .
C3 C4 H4C 109.5 . .
H4A C4 H4C 109.5 . .
H4B C4 H4C 109.5 . .
C3 C5 H5A 109.5 . .
C3 C5 H5B 109.5 . .
H5A C5 H5B 109.5 . .
C3 C5 H5C 109.5 . .
H5A C5 H5C 109.5 . .
H5B C5 H5C 109.5 . .
C7 C6 C3 120.24(16) . .
C7 C6 H6A 107.3 . .
C3 C6 H6A 107.3 . .
C7 C6 H6B 107.3 . .
C3 C6 H6B 107.3 . .
H6A C6 H6B 106.9 . .
N1 C7 C6 112.19(18) . .
N1 C7 C8 110.75(17) . .
C6 C7 C8 107.71(18) . .
N1 C7 H7A 108.7 . .
C6 C7 H7A 108.7 . .
C8 C7 H7A 108.7 . .
C7 C8 H8A 109.5 . .
C7 C8 H8B 109.5 . .
H8A C8 H8B 109.5 . .
C7 C8 H8C 109.5 . .
H8A C8 H8C 109.5 . .
H8B C8 H8C 109.5 . .
N3 C9 Fe1 176.55(18) . .
N4 C10 Fe1 178.8(2) . .
N5 C11 Fe1 180.0 . .
N6 Fe1 C9 95.04(5) . .
N6 Fe1 C9 95.04(5) . 5
C9 Fe1 C9 169.91(11) . 5
N6 Fe1 C11 180.000(1) . .
C9 Fe1 C11 84.96(5) . .
C9 Fe1 C11 84.96(5) 5 .
N6 Fe1 C10 95.21(6) . 5
C9 Fe1 C10 89.95(9) . 5
C9 Fe1 C10 89.13(9) 5 5
C11 Fe1 C10 84.79(6) . 5
N6 Fe1 C10 95.21(6) . .
C9 Fe1 C10 89.13(9) . .
C9 Fe1 C10 89.95(9) 5 .
C11 Fe1 C10 84.79(6) . .
C10 Fe1 C10 169.58(13) 5 .
C1 N1 C7 112.00(16) . .
C1 N1 Ni1 105.07(11) . .
C7 N1 Ni1 120.29(12) . .
C1 N1 H1C 106.2 . .
C7 N1 H1C 106.2 . .
Ni1 N1 H1C 106.2 . .
C2 N2 C3 112.92(15) . .
C2 N2 Ni1 104.90(12) . .
C3 N2 Ni1 121.14(13) . .
C2 N2 H2C 105.6 . .
C3 N2 H2C 105.6 . .
Ni1 N2 H2C 105.6 . .
C9 N3 Ni1 159.94(16) . .
O1 N6 Fe1 180.000(1) . .
N3 Ni1 N3 87.99(10) . 6
N3 Ni1 N1 88.99(6) . .
N3 Ni1 N1 170.23(6) 6 .
N3 Ni1 N1 170.23(6) . 6
N3 Ni1 N1 88.99(6) 6 6
N1 Ni1 N1 95.44(9) . 6
N3 Ni1 N2 83.98(6) . 6
N3 Ni1 N2 104.32(6) 6 6
N1 Ni1 N2 84.59(6) . 6
N1 Ni1 N2 87.77(6) 6 6
N3 Ni1 N2 104.32(6) . .
N3 Ni1 N2 83.98(6) 6 .
N1 Ni1 N2 87.77(6) . .
N1 Ni1 N2 84.59(6) 6 .
N2 Ni1 N2 168.63(8) 6 .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
C1 N1 1.483(3) .
C1 C2 1.515(3) 6
C1 H1A 0.9700 .
C1 H1B 0.9700 .
C2 N2 1.488(3) .
C2 C1 1.515(3) 6
C2 H2A 0.9700 .
C2 H2B 0.9700 .
C3 N2 1.505(3) .
C3 C5 1.529(3) .
C3 C6 1.539(3) .
C3 C4 1.544(3) .
C4 H4A 0.9600 .
C4 H4B 0.9600 .
C4 H4C 0.9600 .
C5 H5A 0.9600 .
C5 H5B 0.9600 .
C5 H5C 0.9600 .
C6 C7 1.529(3) .
C6 H6A 0.9700 .
C6 H6B 0.9700 .
C7 N1 1.495(3) .
C7 C8 1.535(3) .
C7 H7A 0.9800 .
C8 H8A 0.9600 .
C8 H8B 0.9600 .
C8 H8C 0.9600 .
C9 N3 1.143(3) .
C9 Fe1 1.941(2) .
C10 N4 1.152(3) .
C10 Fe1 1.948(2) .
C11 N5 1.151(4) .
C11 Fe1 1.947(3) .
Fe1 N6 1.657(2) .
Fe1 C9 1.941(2) 5
Fe1 C10 1.948(2) 5
N1 Ni1 2.1238(16) .
N1 H1C 0.9100 .
N2 Ni1 2.1525(16) .
N2 H2C 0.9100 .
N3 Ni1 2.0909(18) .
N6 O1 1.142(3) .
Ni1 N3 2.0909(18) 6
Ni1 N1 2.1238(16) 6
Ni1 N2 2.1525(16) 6
O1W H1WA 0.8500 .
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 H1C O1W 0.91 2.12 3.015(3) 168.4 .
O1W H1WA N4 0.85 2.29 2.932(2) 132.0 2_654
