#------------------------------------------------------------------------------
#$Date: 2016-03-24 00:31:19 +0100 (jue 24 de mar de 2016) $
#$Revision: 179533 $
#$URL: svn://www.crystallography.net/cod/cif/4/50/02/4500245.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_4500245
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           152
_symmetry_cell_setting           trigonal
_symmetry_space_group_name_Hall  'P 31 2"'
_symmetry_space_group_name_H-M   'P 31 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                   10.2422(6)
_cell_length_b                   10.2422(6)
_cell_length_c                   23.3430(16)
_cell_measurement_reflns_used    2587
_cell_measurement_temperature    153(2)
_cell_measurement_theta_max      24.8
_cell_measurement_theta_min      3.4
_cell_volume                     2120.7(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 0.983
_diffrn_measured_fraction_theta_max 0.983
_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  0.0721
_diffrn_reflns_av_sigmaI/netI    0.0867
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_l_max       27
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_number            5480
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         25.00
_diffrn_reflns_theta_min         3.48
_exptl_absorpt_coefficient_mu    1.215
_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    1.356
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       needle
_exptl_crystal_F_000             912
_exptl_crystal_size_max          0.45
_exptl_crystal_size_mid          0.16
_exptl_crystal_size_min          0.08
_refine_diff_density_max         0.793
_refine_diff_density_min         -0.752
_refine_diff_density_rms         0.119
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   0.17(4)
_refine_ls_extinction_coef       0.0057(10)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4^
_refine_ls_extinction_method     SHELXL
_refine_ls_goodness_of_fit_ref   1.095
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     163
_refine_ls_number_reflns         2364
_refine_ls_number_restraints     6
_refine_ls_restrained_S_all      1.095
_refine_ls_R_factor_all          0.1114
_refine_ls_R_factor_gt           0.0469
_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)+(0.0341P)²+4.3855P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0905
_refine_ls_wR_factor_ref         0.1298
_reflns_number_gt                1520
_reflns_number_total             2364
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            cg101314j_si_002.cif
_cod_data_source_block           D-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      P3121
_cod_database_code               4500245
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-y, x-y, z+1/3'
'-x+y, -x, z+2/3'
'y, x, -z'
'-x, -x+y, -z+1/3'
'x-y, -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 -0.0504(8) 0.4982(8) 0.0602(3) 0.0376(18) Uani 1 1 d .
H1B H -0.0423 0.4252 0.0362 0.045 Uiso 1 1 calc R
H1C H -0.0372 0.5810 0.0360 0.045 Uiso 1 1 calc R
C2 C 0.2032(8) 0.6290(8) 0.2457(3) 0.0395(18) Uani 1 1 d .
H2B H 0.2796 0.6738 0.2753 0.047 Uiso 1 1 calc R
H2C H 0.2200 0.5566 0.2250 0.047 Uiso 1 1 calc R
C3 C 0.3595(7) 0.8133(8) 0.1696(3) 0.0350(17) Uani 1 1 d .
C4 C 0.3802(9) 0.9573(8) 0.1403(3) 0.045(2) Uani 1 1 d .
H4A H 0.2943 0.9325 0.1166 0.068 Uiso 1 1 calc R
H4B H 0.4695 1.0003 0.1171 0.068 Uiso 1 1 calc R
H4C H 0.3897 1.0287 0.1690 0.068 Uiso 1 1 calc R
C5 C 0.5011(9) 0.8583(9) 0.2076(3) 0.049(2) Uani 1 1 d .
H5A H 0.4911 0.7701 0.2262 0.074 Uiso 1 1 calc R
H5B H 0.5094 0.9298 0.2360 0.074 Uiso 1 1 calc R
H5C H 0.5898 0.9025 0.1841 0.074 Uiso 1 1 calc R
C6 C 0.3472(9) 0.6968(8) 0.1254(3) 0.0432(18) Uani 1 1 d .
H6A H 0.4432 0.7395 0.1056 0.052 Uiso 1 1 calc R
H6B H 0.3349 0.6097 0.1464 0.052 Uiso 1 1 calc R
C7 C 0.2238(8) 0.6394(8) 0.0796(3) 0.0366(18) Uani 1 1 d .
H7A H 0.2334 0.7262 0.0583 0.044 Uiso 1 1 calc R
C8 C 0.2519(10) 0.5388(9) 0.0381(3) 0.053(2) Uani 1 1 d .
H8A H 0.1763 0.5014 0.0087 0.079 Uiso 1 1 calc R
H8B H 0.2471 0.4556 0.0588 0.079 Uiso 1 1 calc R
H8C H 0.3498 0.5969 0.0210 0.079 Uiso 1 1 calc R
C9 C 0.0054(8) 0.8785(9) 0.0658(3) 0.0386(19) Uani 1 1 d .
N6 N 0.1148(8) 1.1148(8) 0.0000 0.035(2) Uani 1 2 d S
C11 C -0.1472(9) 1.0289(9) 0.0480(3) 0.0384(19) Uani 1 1 d .
Fe1 Fe -0.04215(14) 0.95785(14) 0.0000 0.0333(4) Uani 1 2 d S
N1 N 0.0689(6) 0.5551(7) 0.1046(2) 0.0340(14) Uani 1 1 d .
H1A H 0.0619 0.4723 0.1219 0.041 Uiso 1 1 calc R
N2 N 0.2190(6) 0.7488(6) 0.2056(2) 0.0366(15) Uani 1 1 d .
H2A H 0.2305 0.8261 0.2283 0.044 Uiso 1 1 calc R
N3 N 0.0282(7) 0.8217(7) 0.1051(3) 0.0387(16) Uani 1 1 d .
N5 N -0.2082(8) 1.0739(8) 0.0778(3) 0.0543(18) Uani 1 1 d .
O1 O 0.2293(9) 1.2293(9) 0.0000 0.067(3) Uani 1 2 d S
C10 C -0.2282(11) 0.7718(11) 0.0000 0.037(3) Uani 1 2 d SU
Ni1 Ni 0.0000 0.66074(12) 0.1667 0.0301(3) Uani 1 2 d S
N4 N -0.3434(11) 0.6566(11) 0.0000 0.055(3) Uani 1 2 d S
O1W O 0.0000 0.2694(8) 0.1667 0.079(3) Uani 1 2 d S
H1WA H 0.0521 0.2728 0.1888 0.119 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'
Fe Fe 0.3463 0.8444 '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'
H H 0.0000 0.0000 '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'
N N 0.0061 0.0033 '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 110.3(5) . 5
N1 C1 H1B 109.6 . .
C2 C1 H1B 109.6 5 .
N1 C1 H1C 109.6 . .
C2 C1 H1C 109.6 5 .
H1B C1 H1C 108.1 . .
N2 C2 C1 112.0(6) . 5
N2 C2 H2B 109.2 . .
C1 C2 H2B 109.2 5 .
N2 C2 H2C 109.2 . .
C1 C2 H2C 109.2 5 .
H2B C2 H2C 107.9 . .
N2 C3 C6 110.2(6) . .
N2 C3 C4 108.2(5) . .
C6 C3 C4 111.4(6) . .
N2 C3 C5 110.8(6) . .
C6 C3 C5 108.4(5) . .
C4 C3 C5 107.9(6) . .
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 119.9(6) . .
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 112.6(5) . .
N1 C7 C8 111.0(6) . .
C6 C7 C8 107.5(6) . .
N1 C7 H7A 108.6 . .
C6 C7 H7A 108.6 . .
C8 C7 H7A 108.6 . .
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 176.1(7) . .
O1 N6 Fe1 180.000(1) . .
N5 C11 Fe1 178.6(7) . .
N6 Fe1 C10 180.000(1) . .
N6 Fe1 C9 94.9(2) . .
C10 Fe1 C9 85.1(2) . .
N6 Fe1 C9 94.9(2) . 4_465
C10 Fe1 C9 85.1(2) . 4_465
C9 Fe1 C9 170.2(5) . 4_465
N6 Fe1 C11 95.2(2) . 4_465
C10 Fe1 C11 84.8(2) . 4_465
C9 Fe1 C11 89.0(3) . 4_465
C9 Fe1 C11 90.1(3) 4_465 4_465
N6 Fe1 C11 95.2(2) . .
C10 Fe1 C11 84.8(2) . .
C9 Fe1 C11 90.1(3) . .
C9 Fe1 C11 89.0(3) 4_465 .
C11 Fe1 C11 169.7(4) 4_465 .
C1 N1 C7 112.5(5) . .
C1 N1 Ni1 105.0(4) . .
C7 N1 Ni1 119.9(4) . .
C1 N1 H1A 106.2 . .
C7 N1 H1A 106.2 . .
Ni1 N1 H1A 106.2 . .
C2 N2 C3 113.6(5) . .
C2 N2 Ni1 105.0(4) . .
C3 N2 Ni1 121.0(4) . .
C2 N2 H2A 105.3 . .
C3 N2 H2A 105.3 . .
Ni1 N2 H2A 105.3 . .
C9 N3 Ni1 160.9(6) . .
N4 C10 Fe1 180.0(16) . .
N3 Ni1 N3 88.3(3) 5 .
N3 Ni1 N1 89.0(2) 5 5
N3 Ni1 N1 170.0(2) . 5
N3 Ni1 N1 170.0(2) 5 .
N3 Ni1 N1 89.0(2) . .
N1 Ni1 N1 95.3(3) 5 .
N3 Ni1 N2 83.8(2) 5 .
N3 Ni1 N2 104.8(2) . .
N1 Ni1 N2 84.4(2) 5 .
N1 Ni1 N2 87.7(2) . .
N3 Ni1 N2 104.8(2) 5 5
N3 Ni1 N2 83.8(2) . 5
N1 Ni1 N2 87.7(2) 5 5
N1 Ni1 N2 84.4(2) . 5
N2 Ni1 N2 168.3(3) . 5
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
C1 N1 1.482(8) .
C1 C2 1.500(9) 5
C1 H1B 0.9700 .
C1 H1C 0.9700 .
C2 N2 1.487(8) .
C2 C1 1.500(9) 5
C2 H2B 0.9700 .
C2 H2C 0.9700 .
C3 N2 1.505(8) .
C3 C6 1.534(9) .
C3 C4 1.540(10) .
C3 C5 1.561(9) .
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 1.530(9) .
C6 H6A 0.9700 .
C6 H6B 0.9700 .
C7 N1 1.494(8) .
C7 C8 1.543(9) .
C7 H7A 0.9800 .
C8 H8A 0.9600 .
C8 H8B 0.9600 .
C8 H8C 0.9600 .
C9 N3 1.171(8) .
C9 Fe1 1.911(8) .
N6 O1 1.173(10) .
N6 Fe1 1.608(8) .
C11 N5 1.173(9) .
C11 Fe1 1.930(8) .
Fe1 C10 1.905(12) .
Fe1 C9 1.911(8) 4_465
Fe1 C11 1.930(8) 4_465
N1 Ni1 2.129(5) .
N1 H1A 0.9100 .
N2 Ni1 2.156(5) .
N2 H2A 0.9100 .
N3 Ni1 2.096(7) .
C10 N4 1.180(13) .
Ni1 N3 2.096(7) 5
Ni1 N1 2.129(5) 5
Ni1 N2 2.156(5) 5
O1W H1WA 0.7306 .
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
O1W H1WA N5 0.73 2.20 2.931(7) 179.7 5_545
C4 H4A N3 0.96 2.39 3.255(10) 150.3 .
N1 H1A O1W 0.91 2.12 3.016(9) 168.2 .
