#------------------------------------------------------------------------------
#$Date: 2016-01-07 05:51:37 +0200 (Thu, 07 Jan 2016) $
#$Revision: 173622 $
#$URL: svn://www.crystallography.net/cod/cif/7/11/83/7118355.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_7118355
loop_
_publ_author_name
'Lee, Yousoon'
'Jeon, Ie-Rang'
'Abboud, Khalil A.'
'García-Serres, Ricardo'
'Shearer, Jason'
'Murray, Leslie J.'
_publ_section_title
;
 A [3Fe-3S](3+) cluster with exclusively μ-sulfide donors.
;
_journal_issue                   6
_journal_name_full
'Chemical communications (Cambridge, England)'
_journal_page_first              1174
_journal_page_last               1177
_journal_paper_doi               10.1039/c5cc07813j
_journal_volume                  52
_journal_year                    2016
_chemical_formula_sum            'C69 H87 Fe3 N6 S3'
_chemical_formula_weight         1264.17
_space_group_crystal_system      hexagonal
_space_group_IT_number           176
_space_group_name_Hall           '-P 6c'
_space_group_name_H-M_alt        'P 63/m'
_symmetry_space_group_name_Hall  '-P 6c'
_symmetry_space_group_name_H-M   'P 63/m'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-2014/7
_audit_update_record
;
2015-11-17 deposited with the CCDC.
2015-11-17 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                120
_cell_formula_units_Z            2
_cell_length_a                   16.8444(10)
_cell_length_b                   16.8444(10)
_cell_length_c                   12.6713(8)
_cell_measurement_reflns_used    9961
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      28.0
_cell_measurement_theta_min      2.0
_cell_volume                     3113.6(3)
_computing_cell_refinement       'Bruker APEX2 (Bruker, 2014)'
_computing_data_collection       'Bruker APEX2 (Bruker, 2014)'
_computing_data_reduction        'Bruker Apex2 SAINT (Bruker, 2014)'
_computing_molecular_graphics    'XP in SHELXTL-plus, Bruker 2014'
_computing_publication_material  'SHELXL2014/7, Sheldrick, G. M. 2014'
_computing_structure_refinement  'SHELXL2014/7, Sheldrick G. M. 2014'
_computing_structure_solution    'SHELXL2014/7, Sheldrick G. M. 2014'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 1.000
_diffrn_measurement_device_type  'Bruker APEX-II DUO'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0508
_diffrn_reflns_av_unetI/netI     0.0183
_diffrn_reflns_laue_measured_fraction_full 1.000
_diffrn_reflns_laue_measured_fraction_max 1.000
_diffrn_reflns_limit_h_max       21
_diffrn_reflns_limit_h_min       -21
_diffrn_reflns_limit_k_max       21
_diffrn_reflns_limit_k_min       -21
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_number            48177
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 1.000
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.497
_diffrn_reflns_theta_min         1.396
_diffrn_source                   'fine-focus sealed tube'
_exptl_absorpt_coefficient_mu    0.837
_exptl_absorpt_correction_T_max  0.9618
_exptl_absorpt_correction_T_min  0.8578
_exptl_absorpt_correction_type   analytical
_exptl_absorpt_process_details
'based on measured indexed crystal faces, Bruker SHELXTL2014 (Sheldrick, 2014)'
_exptl_crystal_colour            green
_exptl_crystal_density_diffrn    1.348
_exptl_crystal_description       needles
_exptl_crystal_F_000             1338
_exptl_crystal_size_max          0.392
_exptl_crystal_size_mid          0.075
_exptl_crystal_size_min          0.069
_refine_diff_density_max         0.608
_refine_diff_density_min         -0.614
_refine_diff_density_rms         0.069
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.041
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     129
_refine_ls_number_reflns         2495
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.041
_refine_ls_R_factor_all          0.0591
_refine_ls_R_factor_gt           0.0444
_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)+(0.0771P)²+1.6048P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1218
_refine_ls_wR_factor_ref         0.1284
_reflns_Friedel_coverage         0.000
_reflns_number_gt                1938
_reflns_number_total             2495
_reflns_threshold_expression     'I > 2σ(I)'
_cod_data_source_file            c5cc07813j2.cif
_cod_data_source_block           ylee71
_cod_original_cell_volume        3113.6(4)
_cod_database_code               7118355
_shelx_shelxl_version_number     2014/7
_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. 
;
_shelx_estimated_absorpt_t_min   0.735
_shelx_estimated_absorpt_t_max   0.945
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-y, x-y, z'
'-x+y, -x, z'
'-x, -y, z+1/2'
'y, -x+y, z+1/2'
'x-y, x, z+1/2'
'-x, -y, -z'
'y, -x+y, -z'
'x-y, x, -z'
'x, y, -z-1/2'
'-y, x-y, -z-1/2'
'-x+y, -x, -z-1/2'
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
Fe1 Fe 0.70073(3) 0.23021(3) 0.7500 0.03298(19) Uani 1 2 d S T P
S1 S 0.55423(5) 0.18335(5) 0.7500 0.0371(3) Uani 1 2 d S T P
N1 N 0.72165(11) 0.16558(11) 0.62982(19) 0.0338(5) Uani 1 1 d . . .
C1 C 0.71663(14) 0.18999(14) 0.5193(2) 0.0371(6) Uani 1 1 d . . .
H1A H 0.6706 0.1347 0.4811 0.044 Uiso 1 1 calc R U .
H1B H 0.7768 0.2116 0.4850 0.044 Uiso 1 1 calc R U .
C2 C 0.74052(13) 0.09881(13) 0.6489(2) 0.0372(6) Uani 1 1 d . . .
C3 C 0.7483(2) 0.0696(2) 0.7500 0.0376(9) Uani 1 2 d S T P
H3A H 0.7612 0.0208 0.7500 0.045 Uiso 1 2 calc R U P
C4 C 0.75573(18) 0.05105(16) 0.5563(3) 0.0473(7) Uani 1 1 d . . .
H4A H 0.7008 0.0228 0.5119 0.071 Uiso 1 1 calc R U .
H4B H 0.7681 0.0036 0.5825 0.071 Uiso 1 1 calc R U .
H4C H 0.8081 0.0959 0.5147 0.071 Uiso 1 1 calc R U .
C5 C 0.69061(13) 0.26462(13) 0.5109(2) 0.0338(6) Uani 1 1 d . . .
C6 C 0.59755(14) 0.24032(13) 0.5102(2) 0.0326(5) Uani 1 1 d . . .
C7 C 0.52352(15) 0.13963(14) 0.5036(2) 0.0388(6) Uani 1 1 d . . .
H7A H 0.5447 0.1018 0.5404 0.047 Uiso 1 1 calc R U .
H7B H 0.4674 0.1306 0.5394 0.047 Uiso 1 1 calc R U .
C8 C 0.50140(16) 0.10866(16) 0.3894(3) 0.0462(7) Uani 1 1 d . . .
H8A H 0.4551 0.0434 0.3872 0.069 Uiso 1 1 calc R U .
H8B H 0.5571 0.1184 0.3536 0.069 Uiso 1 1 calc R U .
H8C H 0.4777 0.1442 0.3538 0.069 Uiso 1 1 calc R U .
C9 C 0.8219(2) 0.1487(2) 0.2500 0.0622(14) Uani 1 2 d S T P
H9A H 0.8671 0.2119 0.2500 0.075 Uiso 1 2 calc R U P
C10 C 0.7310(2) 0.1233(2) 0.2500 0.0461(10) Uani 1 2 d S T P
H10A H 0.7130 0.1685 0.2500 0.055 Uiso 1 2 calc R U P
C11 C 0.6658(2) 0.0312(2) 0.2500 0.0434(9) Uani 1 2 d S T P
H11A H 0.6025 0.0128 0.2500 0.052 Uiso 1 2 calc R U P
C12 C 0.6923(2) -0.0343(2) 0.2500 0.0498(11) Uani 1 2 d S T P
H12A H 0.6472 -0.0975 0.2500 0.060 Uiso 1 2 calc R U P
C13 C 0.7831(3) -0.0084(2) 0.2500 0.0722(17) Uani 1 2 d S T P
H13A H 0.8014 -0.0534 0.2500 0.087 Uiso 1 2 calc R U P
C14 C 0.8486(2) 0.0843(2) 0.2500 0.084(2) Uani 1 2 d S T P
H14A H 0.9120 0.1029 0.2500 0.101 Uiso 1 2 calc R U P
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'
Fe Fe 0.3463 0.8444 '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 Fe1 N1 98.98(11) 10_557 .
N1 Fe1 S1 106.13(5) 10_557 .
N1 Fe1 S1 106.13(5) . .
N1 Fe1 S1 106.49(5) 10_557 2_655
N1 Fe1 S1 106.49(5) . 2_655
S1 Fe1 S1 128.76(4) . 2_655
Fe1 S1 Fe1 111.24(4) . 3_665
C2 N1 C1 118.5(2) . .
C2 N1 Fe1 120.09(19) . .
C1 N1 Fe1 121.38(12) . .
N1 C1 C5 112.0(2) . .
N1 C1 H1A 109.2 . .
C5 C1 H1A 109.2 . .
N1 C1 H1B 109.2 . .
C5 C1 H1B 109.2 . .
H1A C1 H1B 107.9 . .
N1 C2 C3 124.3(2) . .
N1 C2 C4 118.9(2) . .
C3 C2 C4 116.8(2) . .
C2 C3 C2 132.2(3) 10_557 .
C2 C3 H3A 113.9 10_557 .
C2 C3 H3A 113.9 . .
C2 C4 H4A 109.5 . .
C2 C4 H4B 109.5 . .
H4A C4 H4B 109.5 . .
C2 C4 H4C 109.5 . .
H4A C4 H4C 109.5 . .
H4B C4 H4C 109.5 . .
C6 C5 C6 120.43(19) 2_655 .
C6 C5 C1 119.68(17) 2_655 .
C6 C5 C1 119.79(17) . .
C5 C6 C5 119.56(19) 3_665 .
C5 C6 C7 120.62(18) 3_665 .
C5 C6 C7 119.76(18) . .
C8 C7 C6 111.0(2) . .
C8 C7 H7A 109.4 . .
C6 C7 H7A 109.4 . .
C8 C7 H7B 109.4 . .
C6 C7 H7B 109.4 . .
H7A C7 H7B 108.0 . .
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 . .
C14 C9 C10 120.9(3) . .
C14 C9 H9A 119.5 . .
C10 C9 H9A 119.5 . .
C9 C10 C11 119.2(3) . .
C9 C10 H10A 120.4 . .
C11 C10 H10A 120.4 . .
C12 C11 C10 120.2(3) . .
C12 C11 H11A 119.9 . .
C10 C11 H11A 119.9 . .
C13 C12 C11 120.2(3) . .
C13 C12 H12A 119.9 . .
C11 C12 H12A 119.9 . .
C12 C13 C14 119.4(3) . .
C12 C13 H13A 120.3 . .
C14 C13 H13A 120.3 . .
C9 C14 C13 120.0(3) . .
C9 C14 H14A 120.0 . .
C13 C14 H14A 120.0 . .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
Fe1 N1 2.003(2) 10_557
Fe1 N1 2.003(2) .
Fe1 S1 2.1828(8) .
Fe1 S1 2.1911(8) 2_655
S1 Fe1 2.1910(8) 3_665
N1 C2 1.335(3) .
N1 C1 1.474(4) .
C1 C5 1.528(3) .
C1 H1A 0.9900 .
C1 H1B 0.9900 .
C2 C3 1.402(3) .
C2 C4 1.514(4) .
C3 C2 1.402(3) 10_557
C3 H3A 0.9500 .
C4 H4A 0.9800 .
C4 H4B 0.9800 .
C4 H4C 0.9800 .
C5 C6 1.404(3) 2_655
C5 C6 1.408(3) .
C6 C5 1.404(3) 3_665
C6 C7 1.524(3) .
C7 C8 1.520(4) .
C7 H7A 0.9900 .
C7 H7B 0.9900 .
C8 H8A 0.9800 .
C8 H8B 0.9800 .
C8 H8C 0.9800 .
C9 C14 1.365(5) .
C9 C10 1.369(5) .
C9 H9A 0.9500 .
C10 C11 1.382(5) .
C10 H10A 0.9500 .
C11 C12 1.382(5) .
C11 H11A 0.9500 .
C12 C13 1.365(5) .
C12 H12A 0.9500 .
C13 C14 1.391(5) .
C13 H13A 0.9500 .
C14 H14A 0.9500 .
