#------------------------------------------------------------------------------
#$Date: 2016-03-26 02:49:11 +0200 (Sat, 26 Mar 2016) $
#$Revision: 180156 $
#$URL: svn://www.crystallography.net/cod/cif/7/10/52/7105206.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_7105206
loop_
_publ_author_name
'Dechambenoit, Pierre'
'Ferlay, Sylvie'
'Kyritsakas, Nathalie'
'Hosseini, Mir Wais'
_publ_section_title
;
 Molecular tectonics: crystal engineering of mixed valence
 Fe(II)/Fe(III) solid solutions.
;
_journal_issue                   6
_journal_name_full
'Chemical communications (Cambridge, England)'
_journal_page_first              868
_journal_page_last               870
_journal_paper_doi               10.1039/b919478a
_journal_volume                  46
_journal_year                    2010
_chemical_formula_moiety         '3(C26 H44 N4), 2(C6 Fe N6), 2(Na)'
_chemical_formula_sum            'C90 H132 Fe2 N24 Na2'
_chemical_formula_weight         1707.88
_chemical_name_systematic
;

?

;
_space_group_IT_number           147
_symmetry_cell_setting           trigonal
_symmetry_space_group_name_Hall  '-P 3'
_symmetry_space_group_name_H-M   'P -3'
_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            1
_cell_length_a                   19.1776(8)
_cell_length_b                   19.1776(8)
_cell_length_c                   6.9473(6)
_cell_measurement_reflns_used    1602
_cell_measurement_temperature    173(2)
_cell_measurement_theta_max      25.76
_cell_measurement_theta_min      2.93
_cell_volume                     2212.8(2)
_computing_cell_refinement       'Bruker SMART'
_computing_data_collection       'Bruker SMART'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      173(2)
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       'phi and omega 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  0.0465
_diffrn_reflns_av_sigmaI/netI    0.0626
_diffrn_reflns_limit_h_max       23
_diffrn_reflns_limit_h_min       -22
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -24
_diffrn_reflns_limit_l_max       9
_diffrn_reflns_limit_l_min       -4
_diffrn_reflns_number            10800
_diffrn_reflns_theta_full        27.47
_diffrn_reflns_theta_max         27.47
_diffrn_reflns_theta_min         2.12
_exptl_absorpt_coefficient_mu    0.398
_exptl_absorpt_correction_T_max  0.9882
_exptl_absorpt_correction_T_min  0.9613
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   sadabs
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    1.282
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       needle
_exptl_crystal_F_000             914
_exptl_crystal_size_max          0.10
_exptl_crystal_size_mid          0.04
_exptl_crystal_size_min          0.03
_refine_diff_density_max         0.450
_refine_diff_density_min         -0.529
_refine_diff_density_rms         0.072
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.073
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     180
_refine_ls_number_reflns         3379
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.073
_refine_ls_R_factor_all          0.0780
_refine_ls_R_factor_gt           0.0452
_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)+(0.0626P)²+0.0000P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1066
_refine_ls_wR_factor_ref         0.1207
_reflns_number_gt                2402
_reflns_number_total             3379
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            b919478a.txt
_cod_data_source_block           e712a
_cod_depositor_comments
;
The following automatic conversions were performed:
'_symmetry_cell_setting' value 'Trigonal' changed to 'trigonal' 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_enum 1527 2010-12-29 10:47:43Z saulius 
;
_cod_original_sg_symbol_H-M      P-3
_cod_database_code               7105206
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-y, x-y, z'
'-x+y, -x, z'
'-x, -y, -z'
'y, -x+y, -z'
'x-y, x, -z'
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
_atom_site_disorder_assembly
_atom_site_disorder_group
C1 C 0.95876(13) 0.55626(12) 0.6604(3) 0.0123(4) Uani 1 1 d . . .
N1 N 0.88282(10) 0.53490(10) 0.6375(2) 0.0137(4) Uani 1 1 d . . .
H1 H 0.8481 0.5070 0.7287 0.016 Uiso 1 1 calc R . .
C2 C 0.85444(13) 0.55611(13) 0.4650(3) 0.0153(5) Uani 1 1 d . . .
H2A H 0.8023 0.5531 0.4917 0.018 Uiso 1 1 calc R . .
H2B H 0.8461 0.5175 0.3607 0.018 Uiso 1 1 calc R . .
C3 C 0.91641(12) 0.64159(12) 0.4012(3) 0.0118(4) Uani 1 1 d . . .
C4 C 0.99642(13) 0.64265(14) 0.3745(3) 0.0140(5) Uani 1 1 d . . .
H4A H 0.9943 0.6144 0.2534 0.017 Uiso 1 1 calc R . .
H4B H 1.0406 0.6991 0.3627 0.017 Uiso 1 1 calc R . .
N2 N 1.01411(11) 0.60405(10) 0.5351(2) 0.0140(4) Uani 1 1 d . . .
H2 H 1.0636 0.6131 0.5485 0.017 Uiso 1 1 calc R . .
C5 C 0.89015(13) 0.65765(14) 0.2047(3) 0.0155(5) Uani 1 1 d . . .
H5A H 0.9310 0.7121 0.1610 0.019 Uiso 1 1 calc R . .
H5B H 0.8893 0.6185 0.1105 0.019 Uiso 1 1 calc R . .
C6 C 0.80774(14) 0.65201(14) 0.2031(3) 0.0188(5) Uani 1 1 d . . .
H6A H 0.7663 0.5975 0.2457 0.023 Uiso 1 1 calc R . .
H6B H 0.8081 0.6914 0.2960 0.023 Uiso 1 1 calc R . .
C7 C 0.78528(15) 0.66835(16) 0.0051(3) 0.0261(6) Uani 1 1 d . . .
H7A H 0.8275 0.7211 -0.0407 0.039 Uiso 1 1 calc R . .
H7B H 0.7341 0.6681 0.0132 0.039 Uiso 1 1 calc R . .
H7C H 0.7797 0.6265 -0.0847 0.039 Uiso 1 1 calc R . .
C8 C 0.92295(13) 0.70101(13) 0.5593(3) 0.0158(5) Uani 1 1 d . . .
H8A H 0.8678 0.6882 0.5942 0.019 Uiso 1 1 calc R . .
H8B H 0.9470 0.6912 0.6748 0.019 Uiso 1 1 calc R . .
C9 C 0.97159(14) 0.79033(13) 0.5115(3) 0.0214(5) Uani 1 1 d . . .
H9A H 1.0267 0.8040 0.4730 0.026 Uiso 1 1 calc R . .
H9B H 0.9464 0.8019 0.4009 0.026 Uiso 1 1 calc R . .
C10 C 0.97660(16) 0.84286(15) 0.6810(4) 0.0310(6) Uani 1 1 d . . .
H10A H 0.9221 0.8279 0.7233 0.047 Uiso 1 1 calc R . .
H10B H 1.0053 0.8995 0.6416 0.047 Uiso 1 1 calc R . .
H10C H 1.0056 0.8350 0.7871 0.047 Uiso 1 1 calc R . .
C11 C 0.98118(13) 0.52687(13) 0.8333(3) 0.0128(4) Uani 1 1 d . . .
C12 C 0.92480(13) 0.45359(13) 0.9143(3) 0.0138(4) Uani 1 1 d . . .
H12 H 0.8737 0.4220 0.8551 0.017 Uiso 1 1 calc R . .
C13 C 0.94337(13) 0.42685(13) 1.0817(3) 0.0140(5) Uani 1 1 d . . .
H13 H 0.9049 0.3772 1.1381 0.017 Uiso 1 1 calc R . .
Fe1 Fe 0.6667 0.3333 0.22362(7) 0.01133(16) Uani 1 3 d S . .
C14 C 0.73137(13) 0.42050(13) 0.0513(3) 0.0144(5) Uani 1 1 d . . .
N3 N 0.76394(12) 0.46614(12) -0.0724(3) 0.0223(5) Uani 1 1 d . . .
C15 C 0.75945(13) 0.35147(12) 0.3763(3) 0.0134(5) Uani 1 1 d . . .
N4 N 0.81513(11) 0.35965(11) 0.4634(3) 0.0185(4) Uani 1 1 d . . .
Na1 Na 0.6667 0.3333 -0.2949(2) 0.0243(4) Uani 1 3 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'
Fe Fe 0.3463 0.8444 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Na Na 0.0362 0.0249 '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'
H H 0.0000 0.0000 '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
_geom_angle_publ_flag
N1 C1 N2 121.18(19) . . ?
N1 C1 C11 117.96(19) . . ?
N2 C1 C11 120.84(19) . . ?
C1 N1 C2 121.66(18) . . ?
C1 N1 H1 119.2 . . ?
C2 N1 H1 119.2 . . ?
N1 C2 C3 109.80(17) . . ?
N1 C2 H2A 109.7 . . ?
C3 C2 H2A 109.7 . . ?
N1 C2 H2B 109.7 . . ?
C3 C2 H2B 109.7 . . ?
H2A C2 H2B 108.2 . . ?
C2 C3 C4 106.53(17) . . ?
C2 C3 C5 108.32(17) . . ?
C4 C3 C5 108.38(17) . . ?
C2 C3 C8 108.51(17) . . ?
C4 C3 C8 111.39(17) . . ?
C5 C3 C8 113.44(18) . . ?
N2 C4 C3 112.49(17) . . ?
N2 C4 H4A 109.1 . . ?
C3 C4 H4A 109.1 . . ?
N2 C4 H4B 109.1 . . ?
C3 C4 H4B 109.1 . . ?
H4A C4 H4B 107.8 . . ?
C1 N2 C4 122.75(18) . . ?
C1 N2 H2 118.6 . . ?
C4 N2 H2 118.6 . . ?
C6 C5 C3 115.00(18) . . ?
C6 C5 H5A 108.5 . . ?
C3 C5 H5A 108.5 . . ?
C6 C5 H5B 108.5 . . ?
C3 C5 H5B 108.5 . . ?
H5A C5 H5B 107.5 . . ?
C7 C6 C5 112.41(19) . . ?
C7 C6 H6A 109.1 . . ?
C5 C6 H6A 109.1 . . ?
C7 C6 H6B 109.1 . . ?
C5 C6 H6B 109.1 . . ?
H6A C6 H6B 107.9 . . ?
C6 C7 H7A 109.5 . . ?
C6 C7 H7B 109.5 . . ?
H7A C7 H7B 109.5 . . ?
C6 C7 H7C 109.5 . . ?
H7A C7 H7C 109.5 . . ?
H7B C7 H7C 109.5 . . ?
C9 C8 C3 116.99(18) . . ?
C9 C8 H8A 108.0 . . ?
C3 C8 H8A 108.0 . . ?
C9 C8 H8B 108.0 . . ?
C3 C8 H8B 108.0 . . ?
H8A C8 H8B 107.3 . . ?
C10 C9 C8 112.1(2) . . ?
C10 C9 H9A 109.2 . . ?
C8 C9 H9A 109.2 . . ?
C10 C9 H9B 109.2 . . ?
C8 C9 H9B 109.2 . . ?
H9A C9 H9B 107.9 . . ?
C9 C10 H10A 109.5 . . ?
C9 C10 H10B 109.5 . . ?
H10A C10 H10B 109.5 . . ?
C9 C10 H10C 109.5 . . ?
H10A C10 H10C 109.5 . . ?
H10B C10 H10C 109.5 . . ?
C12 C11 C13 120.36(19) . 4_767 ?
C12 C11 C1 119.06(19) . . ?
C13 C11 C1 120.54(19) 4_767 . ?
C13 C12 C11 119.9(2) . . ?
C13 C12 H12 120.1 . . ?
C11 C12 H12 120.1 . . ?
C12 C13 C11 119.7(2) . 4_767 ?
C12 C13 H13 120.1 . . ?
C11 C13 H13 120.1 4_767 . ?
C14 Fe1 C14 85.30(9) 2_655 3_665 ?
C14 Fe1 C14 85.30(9) 2_655 . ?
C14 Fe1 C14 85.30(9) 3_665 . ?
C14 Fe1 C15 173.70(9) 2_655 . ?
C14 Fe1 C15 88.56(9) 3_665 . ?
C14 Fe1 C15 92.81(9) . . ?
C14 Fe1 C15 92.81(9) 2_655 2_655 ?
C14 Fe1 C15 173.70(9) 3_665 2_655 ?
C14 Fe1 C15 88.56(9) . 2_655 ?
C15 Fe1 C15 93.15(9) . 2_655 ?
C14 Fe1 C15 88.56(9) 2_655 3_665 ?
C14 Fe1 C15 92.81(9) 3_665 3_665 ?
C14 Fe1 C15 173.70(9) . 3_665 ?
C15 Fe1 C15 93.15(9) . 3_665 ?
C15 Fe1 C15 93.15(9) 2_655 3_665 ?
C14 Fe1 Na1 128.53(6) 2_655 1_556 ?
C14 Fe1 Na1 128.53(6) 3_665 1_556 ?
C14 Fe1 Na1 128.53(6) . 1_556 ?
C15 Fe1 Na1 57.00(6) . 1_556 ?
C15 Fe1 Na1 57.00(6) 2_655 1_556 ?
C15 Fe1 Na1 57.00(6) 3_665 1_556 ?
N3 C14 Fe1 170.7(2) . . ?
N3 C14 Na1 74.25(15) . . ?
Fe1 C14 Na1 96.53(8) . . ?
C14 N3 Na1 81.85(15) . . ?
N4 C15 Fe1 177.02(19) . . ?
N4 C15 Na1 94.32(15) . 1_556 ?
Fe1 C15 Na1 87.43(8) . 1_556 ?
N3 Na1 N3 91.63(7) . 2_655 ?
N3 Na1 N3 91.63(7) . 3_665 ?
N3 Na1 N3 91.63(7) 2_655 3_665 ?
N3 Na1 C15 159.44(8) . 3_664 ?
N3 Na1 C15 100.62(6) 2_655 3_664 ?
N3 Na1 C15 104.33(6) 3_665 3_664 ?
N3 Na1 C15 100.62(6) . 2_654 ?
N3 Na1 C15 104.33(6) 2_655 2_654 ?
N3 Na1 C15 159.44(8) 3_665 2_654 ?
C15 Na1 C15 60.50(8) 3_664 2_654 ?
N3 Na1 C15 104.33(6) . 1_554 ?
N3 Na1 C15 159.44(8) 2_655 1_554 ?
N3 Na1 C15 100.62(6) 3_665 1_554 ?
C15 Na1 C15 60.50(8) 3_664 1_554 ?
C15 Na1 C15 60.50(8) 2_654 1_554 ?
N3 Na1 C14 23.90(6) . . ?
N3 Na1 C14 75.40(7) 2_655 . ?
N3 Na1 C14 74.92(7) 3_665 . ?
C15 Na1 C14 175.87(7) 3_664 . ?
C15 Na1 C14 121.24(6) 2_654 . ?
C15 Na1 C14 123.60(6) 1_554 . ?
N3 Na1 C14 75.40(7) . 3_665 ?
N3 Na1 C14 74.93(7) 2_655 3_665 ?
N3 Na1 C14 23.90(6) 3_665 3_665 ?
C15 Na1 C14 123.60(6) 3_664 3_665 ?
C15 Na1 C14 175.87(7) 2_654 3_665 ?
C15 Na1 C14 121.24(6) 1_554 3_665 ?
C14 Na1 C14 54.64(8) . 3_665 ?
N3 Na1 C14 74.92(7) . 2_655 ?
N3 Na1 C14 23.90(6) 2_655 2_655 ?
N3 Na1 C14 75.40(7) 3_665 2_655 ?
C15 Na1 C14 121.24(6) 3_664 2_655 ?
C15 Na1 C14 123.60(6) 2_654 2_655 ?
C15 Na1 C14 175.87(7) 1_554 2_655 ?
C14 Na1 C14 54.64(8) . 2_655 ?
C14 Na1 C14 54.64(8) 3_665 2_655 ?
N3 Na1 Fe1 124.10(5) . 1_554 ?
N3 Na1 Fe1 124.10(5) 2_655 1_554 ?
N3 Na1 Fe1 124.10(5) 3_665 1_554 ?
C15 Na1 Fe1 35.57(5) 3_664 1_554 ?
C15 Na1 Fe1 35.57(5) 2_654 1_554 ?
C15 Na1 Fe1 35.57(5) 1_554 1_554 ?
C14 Na1 Fe1 148.00(5) . 1_554 ?
C14 Na1 Fe1 148.00(5) 3_665 1_554 ?
C14 Na1 Fe1 148.00(5) 2_655 1_554 ?
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
C1 N1 1.310(3) . ?
C1 N2 1.324(3) . ?
C1 C11 1.479(3) . ?
N1 C2 1.456(3) . ?
N1 H1 0.8800 . ?
C2 C3 1.532(3) . ?
C2 H2A 0.9900 . ?
C2 H2B 0.9900 . ?
C3 C4 1.536(3) . ?
C3 C5 1.538(3) . ?
C3 C8 1.542(3) . ?
C4 N2 1.470(3) . ?
C4 H4A 0.9900 . ?
C4 H4B 0.9900 . ?
N2 H2 0.8800 . ?
C5 C6 1.529(3) . ?
C5 H5A 0.9900 . ?
C5 H5B 0.9900 . ?
C6 C7 1.520(3) . ?
C6 H6A 0.9900 . ?
C6 H6B 0.9900 . ?
C7 H7A 0.9800 . ?
C7 H7B 0.9800 . ?
C7 H7C 0.9800 . ?
C8 C9 1.522(3) . ?
C8 H8A 0.9900 . ?
C8 H8B 0.9900 . ?
C9 C10 1.521(3) . ?
C9 H9A 0.9900 . ?
C9 H9B 0.9900 . ?
C10 H10A 0.9800 . ?
C10 H10B 0.9800 . ?
C10 H10C 0.9800 . ?
C11 C12 1.393(3) . ?
C11 C13 1.395(3) 4_767 ?
C12 C13 1.387(3) . ?
C12 H12 0.9500 . ?
C13 C11 1.395(3) 4_767 ?
C13 H13 0.9500 . ?
Fe1 C14 1.922(2) 2_655 ?
Fe1 C14 1.922(2) 3_665 ?
Fe1 C14 1.922(2) . ?
Fe1 C15 1.948(2) . ?
Fe1 C15 1.948(2) 2_655 ?
Fe1 C15 1.948(2) 3_665 ?
Fe1 Na1 3.3447(16) 1_556 ?
C14 N3 1.161(3) . ?
C14 Na1 2.837(2) . ?
N3 Na1 2.758(2) . ?
C15 N4 1.168(3) . ?
C15 Na1 2.808(2) 1_556 ?
Na1 N3 2.758(2) 2_655 ?
Na1 N3 2.758(2) 3_665 ?
Na1 C15 2.808(2) 3_664 ?
Na1 C15 2.808(2) 2_654 ?
Na1 C15 2.808(2) 1_554 ?
Na1 C14 2.837(2) 3_665 ?
Na1 C14 2.837(2) 2_655 ?
Na1 Fe1 3.3447(16) 1_554 ?
