#------------------------------------------------------------------------------
#$Date: 2016-03-23 21:54:53 +0200 (Wed, 23 Mar 2016) $
#$Revision: 179459 $
#$URL: svn://www.crystallography.net/cod/cif/4/33/56/4335698.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_4335698
loop_
_publ_author_name
'Christopher M. Zall'
'Laura J. Clouston'
'Victor G. Young'
'Keying Ding'
'Hyun Jung Kim'
'Danylo Zherebetskyy'
'Yu-Sheng Chen'
'Eckhard Bill'
'Laura Gagliardi'
'Connie C. Lu'
_publ_section_title
;
 Mixed-Valent Dicobalt and Iron-Cobalt Complexes with High-Spin
 Configurations and Short Metal-Metal Bonds
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              9216
_journal_page_last               9228
_journal_paper_doi               10.1021/ic400292g
_journal_volume                  52
_journal_year                    2013
_chemical_formula_moiety         'C45 H42 Co1.01 Fe0.99 N7'
_chemical_formula_sum            'C45 H42 Co1.01 Fe0.99 N7'
_chemical_formula_weight         795.66
_chemical_name_systematic
;
 ?
;
_space_group_crystal_system      trigonal
_space_group_IT_number           148
_space_group_name_Hall           '-R 3'
_space_group_name_H-M_alt        'R -3 :H'
_symmetry_space_group_name_Hall  '-R 3'
_symmetry_space_group_name_H-M   'R -3 :H'
_atom_sites_solution_hydrogens   geom
_audit_creation_method           SHELXL-2013
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                120
_cell_formula_units_Z            6
_cell_length_a                   14.9092(6)
_cell_length_b                   14.9092(6)
_cell_length_c                   29.1910(13)
_cell_measurement_reflns_used    9327
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      20.196
_cell_measurement_theta_min      2.461
_cell_volume                     5619.4(4)
_computing_cell_refinement       'SAINT, Bruker'
_computing_data_collection       'APEX II, Bruker'
_computing_data_reduction        'SAINT, Bruker'
_computing_structure_refinement  'SHELXL-2013 (Sheldrick, 2013)'
_computing_structure_solution    'SHELXL-97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 0.996
_diffrn_measured_fraction_theta_max 0.987
_diffrn_measurement_device_type  'Bruker APEX II CCD'
_diffrn_measurement_method       'area detector, omega scans per phi'
_diffrn_radiation_type           synchrotron
_diffrn_radiation_wavelength     0.4133
_diffrn_reflns_av_R_equivalents  0.0813
_diffrn_reflns_av_unetI/netI     0.0472
_diffrn_reflns_Laue_measured_fraction_full 0.996
_diffrn_reflns_Laue_measured_fraction_max 0.987
_diffrn_reflns_limit_h_max       24
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -23
_diffrn_reflns_limit_l_max       45
_diffrn_reflns_limit_l_min       -48
_diffrn_reflns_number            45843
_diffrn_reflns_point_group_measured_fraction_full 0.996
_diffrn_reflns_point_group_measured_fraction_max 0.987
_diffrn_reflns_theta_full        14.358
_diffrn_reflns_theta_max         20.298
_diffrn_reflns_theta_min         1.864
_diffrn_source                   '15 ID-B APS'
_exptl_absorpt_coefficient_mu    0.205
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS, R. Blessing, 1995'
_exptl_crystal_colour            brown
_exptl_crystal_density_diffrn    1.411
_exptl_crystal_description       'hexagonal plate'
_exptl_crystal_F_000             2484
_exptl_crystal_size_max          0.1
_exptl_crystal_size_mid          0.1
_exptl_crystal_size_min          0.1
_refine_diff_density_max         0.969
_refine_diff_density_min         -0.300
_refine_diff_density_rms         0.069
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.013
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     163
_refine_ls_number_reflns         6123
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.013
_refine_ls_R_factor_all          0.0625
_refine_ls_R_factor_gt           0.0377
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
;
 w=1/[σ²(Fo²)+(0.0403P)²+5.4850P]
 where P=(Fo²+2Fc²)/3
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0891
_refine_ls_wR_factor_ref         0.1006
_reflns_Friedel_coverage         0.000
_reflns_number_gt                4475
_reflns_number_total             6123
_reflns_threshold_expression     'I > 2σ(I)'
_cod_data_source_file            ic400292g_si_006.cif
_cod_data_source_block           hex30
_cod_original_cell_volume        5619.4(5)
_cod_database_code               4335698
#BEGIN Tags that were not found in dictionaries:
_shelx_space_group_comment
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;
_shelxl_version_number           2013-2
#END Tags that were not found in dictionaries
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-y, x-y, z'
'-x+y, -x, z'
'x+2/3, y+1/3, z+1/3'
'-y+2/3, x-y+1/3, z+1/3'
'-x+y+2/3, -x+1/3, z+1/3'
'x+1/3, y+2/3, z+2/3'
'-y+1/3, x-y+2/3, z+2/3'
'-x+y+1/3, -x+2/3, z+2/3'
'-x, -y, -z'
'y, -x+y, -z'
'x-y, x, -z'
'-x+2/3, -y+1/3, -z+1/3'
'y+2/3, -x+y+1/3, -z+1/3'
'x-y+2/3, x+1/3, -z+1/3'
'-x+1/3, -y+2/3, -z+2/3'
'y+1/3, -x+y+2/3, -z+2/3'
'x-y+1/3, x+2/3, -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_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
Co1 Co 0.3333 0.6667 -0.08243(2) 0.01724(6) Uani 0.951 3 d S T P
Fe1 Fe 0.3333 0.6667 -0.08243(2) 0.01724(6) Uani 0.048 3 d S T P
Fe2 Fe 0.3333 0.6667 -0.00759(2) 0.01630(6) Uani 0.939 3 d S T P
Co2 Co 0.3333 0.6667 -0.00759(2) 0.01630(6) Uani 0.06 3 d S T P
N1 N 0.3333 0.6667 -0.15489(5) 0.0189(3) Uani 1 3 d S T P
N2 N 0.21702(8) 0.68912(9) -0.08639(3) 0.0237(2) Uani 1 1 d . . .
N3 N 0.20211(8) 0.67877(8) -0.00857(3) 0.01938(17) Uani 1 1 d . . .
C1 C 0.23580(10) 0.66378(11) -0.16728(4) 0.0262(2) Uani 1 1 d . . .
H1A H 0.1797 0.5907 -0.1695 0.031 Uiso 1 1 calc R U .
H1B H 0.2439 0.6961 -0.1978 0.031 Uiso 1 1 calc R U .
C2 C 0.20479(11) 0.71988(11) -0.13260(4) 0.0265(2) Uani 1 1 d . . .
H2A H 0.2492 0.7957 -0.1363 0.032 Uiso 1 1 calc R U .
H2B H 0.1319 0.7015 -0.1376 0.032 Uiso 1 1 calc R U .
C3 C 0.16930(9) 0.69501(9) -0.04964(4) 0.01983(19) Uani 1 1 d . . .
C4 C 0.08944(9) 0.72677(9) -0.05410(4) 0.01894(19) Uani 1 1 d . . .
C5 C -0.00283(9) 0.66476(9) -0.07754(4) 0.0233(2) Uani 1 1 d . . .
H5A H -0.0172 0.5994 -0.0892 0.028 Uiso 1 1 calc R U .
C6 C -0.07387(10) 0.69822(11) -0.08389(4) 0.0256(2) Uani 1 1 d . . .
H6A H -0.1367 0.6558 -0.0999 0.031 Uiso 1 1 calc R U .
C7 C -0.05287(10) 0.79347(11) -0.06683(4) 0.0266(2) Uani 1 1 d . . .
H7A H -0.1016 0.8161 -0.0708 0.032 Uiso 1 1 calc R U .
C8 C 0.03914(11) 0.85563(10) -0.04395(4) 0.0261(2) Uani 1 1 d . . .
H8A H 0.0537 0.9213 -0.0327 0.031 Uiso 1 1 calc R U .
C9 C 0.11030(9) 0.82267(9) -0.03738(4) 0.0214(2) Uani 1 1 d . . .
H9A H 0.1731 0.8655 -0.0215 0.026 Uiso 1 1 calc R U .
C10 C 0.14260(9) 0.65723(9) 0.03173(4) 0.01832(19) Uani 1 1 d . . .
C11 C 0.03390(9) 0.60484(9) 0.03325(4) 0.0210(2) Uani 1 1 d . . .
H11A H -0.0045 0.5851 0.0055 0.025 Uiso 1 1 calc R U .
C12 C -0.01814(10) 0.58161(10) 0.07486(4) 0.0247(2) Uani 1 1 d . . .
H12A H -0.0917 0.5472 0.0751 0.030 Uiso 1 1 calc R U .
C13 C 0.03559(11) 0.60794(10) 0.11603(4) 0.0262(2) Uani 1 1 d . . .
H13A H -0.0005 0.5920 0.1444 0.031 Uiso 1 1 calc R U .
C14 C 0.14283(11) 0.65795(10) 0.11507(4) 0.0249(2) Uani 1 1 d . . .
H14A H 0.1806 0.6752 0.1430 0.030 Uiso 1 1 calc R U .
C15 C 0.19566(9) 0.68302(9) 0.07356(4) 0.0213(2) Uani 1 1 d . . .
H15A H 0.2692 0.7184 0.0736 0.026 Uiso 1 1 calc R U .
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0000 0.0000 '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 0.0000 0.0010 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Fe Fe 0.1990 0.3060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Co Co 0.2160 0.3560 '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
N2 Co1 N2 119.643(6) 3_565 2_665
N2 Co1 N2 119.642(6) 3_565 .
N2 Co1 N2 119.643(6) 2_665 .
N2 Co1 N1 86.56(3) 3_565 .
N2 Co1 N1 86.56(3) 2_665 .
N2 Co1 N1 86.56(3) . .
N2 Co1 Fe2 93.44(3) 3_565 .
N2 Co1 Fe2 93.44(3) 2_665 .
N2 Co1 Fe2 93.44(3) . .
N1 Co1 Fe2 180.0 . .
N3 Fe2 N3 119.983(1) 3_565 .
N3 Fe2 N3 119.978(1) 3_565 2_665
N3 Fe2 N3 119.982(1) . 2_665
N3 Fe2 Co1 89.20(3) 3_565 .
N3 Fe2 Co1 89.20(3) . .
N3 Fe2 Co1 89.20(3) 2_665 .
C1 N1 C1 114.22(6) . 3_565
C1 N1 C1 114.22(6) . 2_665
C1 N1 C1 114.22(6) 3_565 2_665
C1 N1 Co1 104.16(8) . .
C1 N1 Co1 104.16(8) 3_565 .
C1 N1 Co1 104.16(8) 2_665 .
C3 N2 C2 125.06(11) . .
C3 N2 Co1 121.79(8) . .
C2 N2 Co1 111.92(8) . .
C3 N3 C10 122.26(10) . .
C3 N3 Fe2 118.09(7) . .
C10 N3 Fe2 119.16(7) . .
N1 C1 C2 112.67(10) . .
N2 C2 C1 108.68(10) . .
N2 C3 N3 116.89(10) . .
N2 C3 C4 119.66(10) . .
N3 C3 C4 123.26(10) . .
C9 C4 C5 119.55(11) . .
C9 C4 C3 119.49(10) . .
C5 C4 C3 120.82(10) . .
C6 C5 C4 120.23(11) . .
C7 C6 C5 119.86(12) . .
C8 C7 C6 120.02(11) . .
C7 C8 C9 120.46(12) . .
C8 C9 C4 119.87(11) . .
C15 C10 C11 117.48(10) . .
C15 C10 N3 117.39(10) . .
C11 C10 N3 124.94(10) . .
C12 C11 C10 120.78(11) . .
C13 C12 C11 121.03(12) . .
C14 C13 C12 118.83(11) . .
C13 C14 C15 120.54(11) . .
C14 C15 C10 121.32(11) . .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
Co1 N2 1.9269(10) 3_565
Co1 N2 1.9269(10) 2_665
Co1 N2 1.9269(10) .
Co1 N1 2.1153(16) .
Co1 Fe2 2.1846(4) .
Fe2 N3 2.0528(10) 3_565
Fe2 N3 2.0528(9) .
Fe2 N3 2.0528(9) 2_665
N1 C1 1.4780(13) .
N1 C1 1.4780(13) 3_565
N1 C1 1.4780(13) 2_665
N2 C3 1.3144(15) .
N2 C2 1.4652(15) .
N3 C3 1.3614(14) .
N3 C10 1.4103(14) .
C1 C2 1.5246(18) .
C3 C4 1.4908(16) .
C4 C9 1.3910(16) .
C4 C5 1.3942(16) .
C5 C6 1.3905(17) .
C6 C7 1.3848(19) .
C7 C8 1.384(2) .
C8 C9 1.3874(17) .
C10 C15 1.4002(16) .
C10 C11 1.4045(16) .
C11 C12 1.3887(17) .
C12 C13 1.3877(18) .
C13 C14 1.3861(19) .
C14 C15 1.3908(17) .
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
C1 N1 C1 C2 -80.90(18) 3_565
C1 N1 C1 C2 145.03(12) 2_665
Co1 N1 C1 C2 32.07(11) .
C3 N2 C2 C1 -157.69(12) .
Co1 N2 C2 C1 34.88(13) .
N1 C1 C2 N2 -45.37(15) .
C2 N2 C3 N3 -169.81(12) .
Co1 N2 C3 N3 -3.55(16) .
C2 N2 C3 C4 5.37(19) .
Co1 N2 C3 C4 171.63(8) .
C10 N3 C3 N2 -163.76(11) .
Fe2 N3 C3 N2 8.08(15) .
C10 N3 C3 C4 21.25(17) .
Fe2 N3 C3 C4 -166.91(8) .
N2 C3 C4 C9 -110.21(13) .
N3 C3 C4 C9 64.64(16) .
N2 C3 C4 C5 65.38(16) .
N3 C3 C4 C5 -119.76(13) .
C9 C4 C5 C6 -0.45(18) .
C3 C4 C5 C6 -176.05(11) .
C4 C5 C6 C7 -0.03(18) .
C5 C6 C7 C8 0.68(19) .
C6 C7 C8 C9 -0.85(19) .
C7 C8 C9 C4 0.36(18) .
C5 C4 C9 C8 0.29(17) .
C3 C4 C9 C8 175.94(11) .
C3 N3 C10 C15 -154.46(11) .
Fe2 N3 C10 C15 33.78(13) .
C3 N3 C10 C11 30.68(17) .
Fe2 N3 C10 C11 -141.09(9) .
C15 C10 C11 C12 1.18(16) .
N3 C10 C11 C12 176.04(11) .
C10 C11 C12 C13 -1.05(18) .
C11 C12 C13 C14 -0.17(19) .
C12 C13 C14 C15 1.22(19) .
C13 C14 C15 C10 -1.07(19) .
C11 C10 C15 C14 -0.13(17) .
N3 C10 C15 C14 -175.39(10) .
