#------------------------------------------------------------------------------
#$Date: 2016-02-18 17:37:37 +0200 (Thu, 18 Feb 2016) $
#$Revision: 176729 $
#$URL: svn://www.crystallography.net/cod/cif/1/50/80/1508049.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_1508049
loop_
_publ_author_name
'Lee, Yunho'
'Mankad, Neal P.'
'Peters, Jonas C.'
_publ_section_title
;
 Triggering N(2) uptake via redox-induced expulsion of coordinated NH(3)
 and N(2) silylation at trigonal bipyramidal iron.
;
_journal_issue                   7
_journal_name_full               'Nature chemistry'
_journal_page_first              558
_journal_page_last               565
_journal_paper_doi               10.1038/nchem.660
_journal_volume                  2
_journal_year                    2010
_chemical_formula_sum            'C48 H78 Fe N2 Na O3 P3 Si'
_chemical_formula_weight         930.62
_chemical_name_common            5
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           146
_symmetry_cell_setting           rhombohedral
_symmetry_space_group_name_Hall  'R 3'
_symmetry_space_group_name_H-M   'R 3 :H'
_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                   17.9312(3)
_cell_length_b                   17.9312(3)
_cell_length_c                   13.1252(4)
_cell_measurement_reflns_used    9889
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      68.32
_cell_measurement_theta_min      4.41
_cell_volume                     3654.73(14)
_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      100(2)
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.998
_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           CuK\a
_diffrn_radiation_wavelength     1.54178
_diffrn_reflns_av_R_equivalents  0.0295
_diffrn_reflns_av_sigmaI/netI    0.0429
_diffrn_reflns_limit_h_max       21
_diffrn_reflns_limit_h_min       -21
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -21
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_number            13327
_diffrn_reflns_theta_full        68.94
_diffrn_reflns_theta_max         68.94
_diffrn_reflns_theta_min         4.41
_exptl_absorpt_coefficient_mu    4.053
_exptl_absorpt_correction_T_max  0.667
_exptl_absorpt_correction_T_min  0.586
_exptl_absorpt_correction_type   multi-scan
_exptl_crystal_colour            brown
_exptl_crystal_density_diffrn    1.269
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       needle
_exptl_crystal_F_000             1860
_exptl_crystal_size_max          0.30
_exptl_crystal_size_mid          0.12
_exptl_crystal_size_min          0.10
_refine_diff_density_max         0.308
_refine_diff_density_min         -0.204
_refine_diff_density_rms         0.039
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   0.021(3)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.054
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     182
_refine_ls_number_reflns         2577
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.054
_refine_ls_R_factor_all          0.0245
_refine_ls_R_factor_gt           0.0240
_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)+(0.0309P)²+0.0000P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0598
_refine_ls_wR_factor_ref         0.0600
_reflns_number_gt                2523
_reflns_number_total             2577
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            nchem.660-s6.cif
_cod_data_source_block           d8-09022final
_cod_depositor_comments
;
The following automatic conversions were performed:

'_symmetry_cell_setting' value 'Rhombohedral' changed to
'rhombohedral' 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 1891 2012-01-12 08:04:46Z andrius 
;
_cod_original_sg_symbol_H-M      R3
_cod_database_code               1508049
loop_
_symmetry_equiv_pos_as_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'
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
Fe Fe 0.6667 0.3333 0.66788(3) 0.01164(12) Uani 1 3 d S
Si Si 0.6667 0.3333 0.49625(6) 0.01274(17) Uani 1 3 d S
P1 P 0.58585(3) 0.19344(3) 0.64435(3) 0.01315(11) Uani 1 1 d .
Na Na 0.6667 0.3333 1.06351(9) 0.0182(3) Uani 1 3 d S
N2 N 0.6667 0.3333 0.8896(2) 0.0253(7) Uani 1 3 d S
N1 N 0.6667 0.3333 0.8022(2) 0.0163(6) Uani 1 3 d S
O1 O 0.68945(10) 0.22329(10) 1.09564(12) 0.0281(3) Uani 1 1 d .
C2 C 0.54278(13) 0.21072(13) 0.34344(15) 0.0187(4) Uani 1 1 d .
H2 H 0.5713 0.2529 0.2920 0.022 Uiso 1 1 calc R
C1 C 0.57454(11) 0.22831(12) 0.44293(14) 0.0150(4) Uani 1 1 d .
C5 C 0.45773(12) 0.08695(12) 0.49309(15) 0.0177(4) Uani 1 1 d .
H5 H 0.4283 0.0448 0.5443 0.021 Uiso 1 1 calc R
C6 C 0.53157(12) 0.16462(12) 0.51821(14) 0.0153(4) Uani 1 1 d .
C3 C 0.46996(13) 0.13251(14) 0.31793(15) 0.0214(4) Uani 1 1 d .
H3 H 0.4498 0.1214 0.2496 0.026 Uiso 1 1 calc R
C101 C 0.64510(14) 0.07544(14) 1.07526(17) 0.0272(5) Uani 1 1 d .
H10A H 0.5936 0.0411 1.0323 0.033 Uiso 1 1 calc R
H10B H 0.6542 0.0359 1.1193 0.033 Uiso 1 1 calc R
C4 C 0.42716(13) 0.07103(13) 0.39322(15) 0.0202(4) Uani 1 1 d .
H4 H 0.3770 0.0181 0.3766 0.024 Uiso 1 1 calc R
C100 C 0.63460(16) 0.14034(15) 1.1391(2) 0.0351(5) Uani 1 1 d .
H10C H 0.5739 0.1269 1.1378 0.042 Uiso 1 1 calc R
H10D H 0.6512 0.1388 1.2106 0.042 Uiso 1 1 calc R
C102 C 0.72451(15) 0.13010(15) 1.00924(19) 0.0326(5) Uani 1 1 d .
H10E H 0.7670 0.1105 1.0159 0.039 Uiso 1 1 calc R
H10F H 0.7084 0.1274 0.9366 0.039 Uiso 1 1 calc R
C103 C 0.76033(15) 0.22036(15) 1.0509(2) 0.0317(5) Uani 1 1 d .
H10G H 0.8053 0.2328 1.1026 0.038 Uiso 1 1 calc R
H10H H 0.7859 0.2633 0.9954 0.038 Uiso 1 1 calc R
C7 C 0.63276(12) 0.11871(12) 0.63842(14) 0.0157(4) Uani 1 1 d .
H7 H 0.6693 0.1309 0.7006 0.019 Uiso 1 1 calc R
C8 C 0.56910(12) 0.02134(12) 0.63805(16) 0.0193(4) Uani 1 1 d .
H8A H 0.5333 0.0059 0.5766 0.029 Uiso 1 1 calc R
H8B H 0.5323 0.0058 0.6985 0.029 Uiso 1 1 calc R
H8C H 0.6011 -0.0098 0.6388 0.029 Uiso 1 1 calc R
C9 C 0.69291(13) 0.14031(13) 0.54677(15) 0.0198(4) Uani 1 1 d .
H9A H 0.7235 0.1079 0.5515 0.030 Uiso 1 1 calc R
H9B H 0.7347 0.2022 0.5464 0.030 Uiso 1 1 calc R
H9C H 0.6591 0.1246 0.4838 0.030 Uiso 1 1 calc R
C11 C 0.53036(14) 0.11753(13) 0.83913(15) 0.0235(4) Uani 1 1 d .
H11A H 0.5644 0.1744 0.8707 0.035 Uiso 1 1 calc R
H11B H 0.5668 0.0918 0.8286 0.035 Uiso 1 1 calc R
H11C H 0.4821 0.0804 0.8839 0.035 Uiso 1 1 calc R
C12 C 0.43641(14) 0.16460(14) 0.75145(17) 0.0257(4) Uani 1 1 d .
H12A H 0.3903 0.1283 0.7992 0.038 Uiso 1 1 calc R
H12B H 0.4112 0.1666 0.6860 0.038 Uiso 1 1 calc R
H12C H 0.4698 0.2230 0.7792 0.038 Uiso 1 1 calc R
C10 C 0.49544(13) 0.12708(12) 0.73594(15) 0.0183(4) Uani 1 1 d .
H10 H 0.4602 0.0682 0.7060 0.022 Uiso 1 1 calc R
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0181 0.0091 '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 0.0311 0.0180 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0492 0.0322 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Na Na 0.1353 0.1239 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Si Si 0.2541 0.3302 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
P P 0.2955 0.4335 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Fe Fe -1.1336 3.1974 '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 Fe P1 98.057(16) . 2_655
N1 Fe P1 98.057(16) . .
P1 Fe P1 118.069(7) 2_655 .
N1 Fe P1 98.057(16) . 3_665
P1 Fe P1 118.069(8) 2_655 3_665
P1 Fe P1 118.069(8) . 3_665
N1 Fe Si 180.000(1) . .
P1 Fe Si 81.943(16) 2_655 .
P1 Fe Si 81.943(16) . .
P1 Fe Si 81.943(16) 3_665 .
C1 Si C1 107.39(6) 2_655 .
C1 Si C1 107.39(6) 2_655 3_665
C1 Si C1 107.39(6) . 3_665
C1 Si Fe 111.48(6) 2_655 .
C1 Si Fe 111.48(6) . .
C1 Si Fe 111.48(6) 3_665 .
C6 P1 C10 103.11(9) . .
C6 P1 C7 97.01(8) . .
C10 P1 C7 97.16(8) . .
C6 P1 Fe 113.36(6) . .
C10 P1 Fe 119.83(6) . .
C7 P1 Fe 122.39(6) . .
O1 Na O1 116.56(3) . 2_655
O1 Na O1 116.56(3) . 3_665
O1 Na O1 116.56(3) 2_655 3_665
O1 Na N2 100.82(5) . .
O1 Na N2 100.82(5) 2_655 .
O1 Na N2 100.82(5) 3_665 .
N1 N2 Na 180.000(1) . .
N2 N1 Fe 180.000(1) . .
C103 O1 C100 106.77(17) . .
C103 O1 Na 120.82(13) . .
C100 O1 Na 131.04(14) . .
C1 C2 C3 121.44(18) . .
C1 C2 H2 119.3 . .
C3 C2 H2 119.3 . .
C2 C1 C6 118.41(17) . .
C2 C1 Si 128.24(14) . .
C6 C1 Si 113.19(14) . .
C4 C5 C6 120.32(18) . .
C4 C5 H5 119.8 . .
C6 C5 H5 119.8 . .
C5 C6 C1 120.15(17) . .
C5 C6 P1 126.17(15) . .
C1 C6 P1 113.60(14) . .
C4 C3 C2 119.58(18) . .
C4 C3 H3 120.2 . .
C2 C3 H3 120.2 . .
C100 C101 C102 104.67(18) . .
C100 C101 H10A 110.8 . .
C102 C101 H10A 110.8 . .
C100 C101 H10B 110.8 . .
C102 C101 H10B 110.8 . .
H10A C101 H10B 108.9 . .
C3 C4 C5 120.07(18) . .
C3 C4 H4 120.0 . .
C5 C4 H4 120.0 . .
O1 C100 C101 107.04(19) . .
O1 C100 H10C 110.3 . .
C101 C100 H10C 110.3 . .
O1 C100 H10D 110.3 . .
C101 C100 H10D 110.3 . .
H10C C100 H10D 108.6 . .
C103 C102 C101 104.00(18) . .
C103 C102 H10E 111.0 . .
C101 C102 H10E 111.0 . .
C103 C102 H10F 111.0 . .
C101 C102 H10F 111.0 . .
H10E C102 H10F 109.0 . .
O1 C103 C102 106.19(18) . .
O1 C103 H10G 110.5 . .
C102 C103 H10G 110.5 . .
O1 C103 H10H 110.5 . .
C102 C103 H10H 110.5 . .
H10G C103 H10H 108.7 . .
C9 C7 C8 108.32(16) . .
C9 C7 P1 110.91(13) . .
C8 C7 P1 117.44(13) . .
C9 C7 H7 106.5 . .
C8 C7 H7 106.5 . .
P1 C7 H7 106.5 . .
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 . .
C7 C9 H9A 109.5 . .
C7 C9 H9B 109.5 . .
H9A C9 H9B 109.5 . .
C7 C9 H9C 109.5 . .
H9A C9 H9C 109.5 . .
H9B C9 H9C 109.5 . .
C10 C11 H11A 109.5 . .
C10 C11 H11B 109.5 . .
H11A C11 H11B 109.5 . .
C10 C11 H11C 109.5 . .
H11A C11 H11C 109.5 . .
H11B C11 H11C 109.5 . .
C10 C12 H12A 109.5 . .
C10 C12 H12B 109.5 . .
H12A C12 H12B 109.5 . .
C10 C12 H12C 109.5 . .
H12A C12 H12C 109.5 . .
H12B C12 H12C 109.5 . .
C12 C10 C11 110.04(17) . .
C12 C10 P1 111.95(14) . .
C11 C10 P1 111.24(14) . .
C12 C10 H10 107.8 . .
C11 C10 H10 107.8 . .
P1 C10 H10 107.8 . .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
Fe N1 1.763(3) .
Fe P1 2.2029(4) 2_655
Fe P1 2.2029(4) .
Fe P1 2.2029(4) 3_665
Fe Si 2.2526(9) .
Si C1 1.9116(18) 2_655
Si C1 1.9116(18) .
Si C1 1.9116(18) 3_665
P1 C6 1.8581(19) .
P1 C10 1.8868(19) .
P1 C7 1.9068(18) .
Na O1 2.2459(15) .
Na O1 2.2459(15) 2_655
Na O1 2.2459(15) 3_665
Na N2 2.282(3) .
N2 N1 1.147(4) .
O1 C103 1.425(3) .
O1 C100 1.429(3) .
C2 C1 1.396(3) .
C2 C3 1.397(3) .
C2 H2 0.9500 .
C1 C6 1.412(3) .
C5 C4 1.394(3) .
C5 C6 1.399(3) .
C5 H5 0.9500 .
C3 C4 1.391(3) .
C3 H3 0.9500 .
C101 C100 1.520(3) .
C101 C102 1.531(3) .
C101 H10A 0.9900 .
C101 H10B 0.9900 .
C4 H4 0.9500 .
C100 H10C 0.9900 .
C100 H10D 0.9900 .
C102 C103 1.514(3) .
C102 H10E 0.9900 .
C102 H10F 0.9900 .
C103 H10G 0.9900 .
C103 H10H 0.9900 .
C7 C9 1.531(3) .
C7 C8 1.536(3) .
C7 H7 1.0000 .
C8 H8A 0.9800 .
C8 H8B 0.9800 .
C8 H8C 0.9800 .
C9 H9A 0.9800 .
C9 H9B 0.9800 .
C9 H9C 0.9800 .
C11 C10 1.537(3) .
C11 H11A 0.9800 .
C11 H11B 0.9800 .
C11 H11C 0.9800 .
C12 C10 1.525(3) .
C12 H12A 0.9800 .
C12 H12B 0.9800 .
C12 H12C 0.9800 .
C10 H10 1.0000 .
