#------------------------------------------------------------------------------
#$Date: 2016-03-26 13:44:51 +0200 (Sat, 26 Mar 2016) $
#$Revision: 180234 $
#$URL: svn://www.crystallography.net/cod/cif/7/11/20/7112029.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_7112029
loop_
_publ_author_name
'Nathaniel S. Sickerman'
'Sonja M. Peterson'
'Joseph W. Ziller'
'A. S. Borovik'
_publ_section_title
;
 Synthesis, structure and reactivity of FeII/III-NH3 complexes bearing a
 tripodal sulfonamido ligand
;
_journal_name_full               Chem.Commun.
_journal_page_first              2515
_journal_paper_doi               10.1039/c3cc48804g
_journal_volume                  50
_journal_year                    2014
_chemical_absolute_configuration ad
_chemical_formula_sum            'C33 H48 Fe N5 O6 S3'
_chemical_formula_weight         762.79
_chemical_name_systematic
; 
 ? 
;
_space_group_crystal_system      hexagonal
_space_group_IT_number           173
_space_group_name_Hall           'P 6c'
_space_group_name_H-M_alt        'P 63'
_symmetry_space_group_name_Hall  'P 6c'
_symmetry_space_group_name_H-M   'P 63'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-2013
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                120
_cell_formula_units_Z            2
_cell_length_a                   13.6656(9)
_cell_length_b                   13.6656(9)
_cell_length_c                   12.2841(8)
_cell_measurement_reflns_used    9990
_cell_measurement_temperature    88(2)
_cell_measurement_theta_max      28.23
_cell_measurement_theta_min      2.39
_cell_volume                     1986.7(2)
_computing_cell_refinement       'Bruker SAINT 7.68a, 2009'
_computing_data_collection       'Bruker APEX2 2011.4-1, 2011'
_computing_data_reduction        'Bruker SAINT 7.68a, 2009'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-2013 (Sheldrick, 2013)'
_computing_structure_solution    'Bruker SHELXTL 2008/4'
_diffrn_ambient_temperature      88(2)
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device_type  'Bruker SMART APEX II CCD'
_diffrn_measurement_method       'φ and ω scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0246
_diffrn_reflns_av_unetI/netI     0.0195
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_h_min       -18
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_number            23645
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.992
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         28.278
_diffrn_reflns_theta_min         1.721
_diffrn_source                   'fine-focus sealed tube'
_exptl_absorpt_coefficient_mu    0.583
_exptl_absorpt_correction_T_max  0.9721
_exptl_absorpt_correction_T_min  0.8556
_exptl_absorpt_correction_type   numerical
_exptl_absorpt_process_details   'Bruker SADABS 2008/1'
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    1.275
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    not_measured
_exptl_crystal_description       hexagon
_exptl_crystal_F_000             806
_exptl_crystal_size_max          0.294
_exptl_crystal_size_mid          0.178
_exptl_crystal_size_min          0.134
_refine_diff_density_max         0.316
_refine_diff_density_min         -0.256
_refine_diff_density_rms         0.041
_refine_ls_abs_structure_details
; 
 Flack x determined using 1459 quotients [(I+)-(I-)]/[(I+)+(I-)] 
 (Parsons and Flack (2004), Acta Cryst. A60, s61). 
;
_refine_ls_abs_structure_Flack   0.025(4)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.067
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     149
_refine_ls_number_reflns         3279
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.066
_refine_ls_R_factor_all          0.0233
_refine_ls_R_factor_gt           0.0221
_refine_ls_shift/su_max          0.026
_refine_ls_shift/su_mean         0.001
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[σ²(Fo²)+(0.0399P)²+0.1507P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0611
_refine_ls_wR_factor_ref         0.0616
_reflns_Friedel_coverage         0.900
_reflns_Friedel_fraction_full    0.996
_reflns_Friedel_fraction_max     0.985
_reflns_number_gt                3176
_reflns_number_total             3279
_reflns_threshold_expression     'I > 2σ(I)'
_cod_data_source_file            c3cc48804g.txt
_cod_data_source_block           asb240
_cod_depositor_comments
;
The following automatic conversions were performed:

'_exptl_crystal_density_meas' value 'not_measured' was changed to '?'
- the value is perceived as not measured.

Automatic conversion script
Id: cif_fix_values 3008 2015-01-20 13:52:24Z robertas 
;
_cod_original_cell_volume        1986.7(3)
_cod_database_code               7112029
#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. 
;
_shelx_estimated_absorpt_t_min   0.847
_shelx_estimated_absorpt_t_max   0.926
_shelxl_version_number           2013-3
#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, -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 0.3333 0.6667 0.97482(4) 0.01601(11) Uani 1 3 d S T P
S1 S 0.48339(4) 0.93012(3) 0.99426(4) 0.01677(11) Uani 1 1 d . . .
N1 N 0.3333 0.6667 0.7880(3) 0.0213(6) Uani 1 3 d S T P
N2 N 0.47075(13) 0.81429(13) 0.94821(14) 0.0189(3) Uani 1 1 d . . .
N3 N 0.3333 0.6667 1.1442(2) 0.0172(6) Uani 1 3 d S T P
H3A H 0.2615 0.6225 1.1689 0.026 Uiso 0.3333 1 calc R U P
H3B H 0.3611 0.7385 1.1689 0.026 Uiso 0.3333 1 calc R U P
H3C H 0.3775 0.6389 1.1689 0.026 Uiso 0.3333 1 calc R U P
O1 O 0.42291(12) 0.90284(12) 1.09691(12) 0.0201(3) Uani 1 1 d . . .
O2 O 0.44977(12) 0.98481(12) 0.91376(12) 0.0225(3) Uani 1 1 d . . .
C1 C 0.42614(19) 0.77962(18) 0.75324(18) 0.0243(4) Uani 1 1 d . . .
H1A H 0.3975 0.8331 0.7466 0.029 Uiso 1 1 calc R U .
H1B H 0.4558 0.7738 0.6815 0.029 Uiso 1 1 calc R U .
C2 C 0.51971(18) 0.82192(17) 0.83851(19) 0.0239(4) Uani 1 1 d . . .
H2A H 0.5568 0.7756 0.8362 0.029 Uiso 1 1 calc R U .
H2B H 0.5774 0.9013 0.8228 0.029 Uiso 1 1 calc R U .
C3 C 0.63011(15) 1.02108(15) 1.02331(16) 0.0169(4) Uani 1 1 d . . .
C4 C 0.69704(16) 1.12011(16) 0.96167(16) 0.0208(4) Uani 1 1 d . . .
C5 C 0.81034(16) 1.18862(15) 0.9915(2) 0.0246(4) Uani 1 1 d . . .
H5A H 0.8563 1.2550 0.9504 0.030 Uiso 1 1 calc R U .
C6 C 0.85823(19) 1.16321(18) 1.0792(2) 0.0286(5) Uani 1 1 d . . .
C7 C 0.79075(18) 1.06579(18) 1.13741(19) 0.0264(5) Uani 1 1 d . . .
H7A H 0.8227 1.0477 1.1974 0.032 Uiso 1 1 calc R U .
C8 C 0.67759(17) 0.99296(16) 1.11160(17) 0.0204(4) Uani 1 1 d . . .
C9 C 0.65702(18) 1.15963(18) 0.86514(19) 0.0246(4) Uani 1 1 d . . .
H9A H 0.7207 1.2283 0.8348 0.037 Uiso 1 1 calc R U .
H9B H 0.5981 1.1758 0.8887 0.037 Uiso 1 1 calc R U .
H9C H 0.6264 1.1004 0.8094 0.037 Uiso 1 1 calc R U .
C10 C 0.9813(2) 1.2395(2) 1.1087(3) 0.0422(7) Uani 1 1 d . . .
H10A H 1.0113 1.3109 1.0687 0.063 Uiso 1 1 calc R U .
H10B H 1.0244 1.2023 1.0894 0.063 Uiso 1 1 calc R U .
H10C H 0.9879 1.2547 1.1871 0.063 Uiso 1 1 calc R U .
C11 C 0.61310(17) 0.88900(17) 1.18167(18) 0.0215(4) Uani 1 1 d . . .
H11A H 0.6663 0.8785 1.2268 0.032 Uiso 1 1 calc R U .
H11B H 0.5708 0.8227 1.1350 0.032 Uiso 1 1 calc R U .
H11C H 0.5604 0.8984 1.2287 0.032 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 0.0033 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'
O O 0.0106 0.0060 '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
N2 Fe1 N2 117.33(3) 2_665 .
N2 Fe1 N2 117.33(3) 2_665 3_565
N2 Fe1 N2 117.33(3) . 3_565
N2 Fe1 N3 99.51(5) 2_665 .
N2 Fe1 N3 99.51(5) . .
N2 Fe1 N3 99.51(5) 3_565 .
N2 Fe1 N1 80.49(5) 2_665 .
N2 Fe1 N1 80.49(5) . .
N2 Fe1 N1 80.49(5) 3_565 .
N3 Fe1 N1 180.0 . .
O2 S1 O1 116.10(9) . .
O2 S1 N2 111.28(9) . .
O1 S1 N2 106.62(8) . .
O2 S1 C3 108.22(9) . .
O1 S1 C3 107.57(9) . .
N2 S1 C3 106.60(8) . .
C1 N1 C1 112.14(13) 2_665 .
C1 N1 C1 112.14(13) 2_665 3_565
C1 N1 C1 112.14(13) . 3_565
C1 N1 Fe1 106.65(15) 2_665 .
C1 N1 Fe1 106.65(15) . .
C1 N1 Fe1 106.65(15) 3_565 .
C2 N2 S1 115.31(14) . .
C2 N2 Fe1 112.72(13) . .
S1 N2 Fe1 121.73(9) . .
N1 C1 C2 108.33(19) . .
N2 C2 C1 109.49(17) . .
C8 C3 C4 120.39(17) . .
C8 C3 S1 118.16(14) . .
C4 C3 S1 121.43(15) . .
C5 C4 C3 117.99(19) . .
C5 C4 C9 116.28(18) . .
C3 C4 C9 125.74(18) . .
C6 C5 C4 122.47(19) . .
C7 C6 C5 118.1(2) . .
C7 C6 C10 121.1(2) . .
C5 C6 C10 120.8(2) . .
C6 C7 C8 122.6(2) . .
C7 C8 C3 118.49(19) . .
C7 C8 C11 117.31(19) . .
C3 C8 C11 124.19(17) . .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
Fe1 N2 1.9785(16) 2_665
Fe1 N2 1.9786(16) .
Fe1 N2 1.9786(16) 3_565
Fe1 N3 2.080(3) .
Fe1 N1 2.295(3) .
S1 O2 1.4460(15) .
S1 O1 1.4504(15) .
S1 N2 1.6069(17) .
S1 C3 1.7890(19) .
N1 C1 1.488(2) 2_665
N1 C1 1.488(2) .
N1 C1 1.488(2) 3_565
N2 C2 1.485(3) .
C1 C2 1.526(3) .
C3 C8 1.412(3) .
C3 C4 1.415(3) .
C4 C5 1.399(3) .
C4 C9 1.514(3) .
C5 C6 1.392(3) .
C6 C7 1.381(3) .
C6 C10 1.514(3) .
C7 C8 1.394(3) .
C8 C11 1.511(3) .
