#------------------------------------------------------------------------------
#$Date: 2016-03-21 18:11:13 +0200 (Mon, 21 Mar 2016) $
#$Revision: 178804 $
#$URL: svn://www.crystallography.net/cod/cif/4/10/58/4105819.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_4105819
loop_
_publ_author_name
'Yunho Lee'
'Jonas C. Peters'
_publ_section_title
;
 Silylation of Iron-Bound Carbon Monoxide Affords a Terminal Fe Carbyne
;
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              4438
_journal_page_last               4446
_journal_paper_doi               10.1021/ja109678y
_journal_volume                  133
_journal_year                    2011
_chemical_formula_sum            'C49 H78 Fe Na O4 P3 Si'
_chemical_formula_weight         930.95
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           146
_symmetry_cell_setting           trigonal
_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                   17.9012(7)
_cell_length_b                   17.9012(7)
_cell_length_c                   13.0887(10)
_cell_measurement_reflns_used    9887
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      30.60
_cell_measurement_theta_min      2.28
_cell_volume                     3632.4(3)
_computing_cell_refinement       'Bruker SAINT'
_computing_data_collection       'Bruker APEX2'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       'φ and ω 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  0.0360
_diffrn_reflns_av_sigmaI/netI    0.0359
_diffrn_reflns_limit_h_max       24
_diffrn_reflns_limit_h_min       -24
_diffrn_reflns_limit_k_max       24
_diffrn_reflns_limit_k_min       -24
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            18641
_diffrn_reflns_theta_full        29.12
_diffrn_reflns_theta_max         29.12
_diffrn_reflns_theta_min         2.04
_exptl_absorpt_coefficient_mu    0.486
_exptl_absorpt_correction_T_max  0.9432
_exptl_absorpt_correction_T_min  0.9355
_exptl_absorpt_correction_type   multi-scan
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    1.277
_exptl_crystal_description       block
_exptl_crystal_F_000             620
_exptl_crystal_size_max          0.40
_exptl_crystal_size_mid          0.40
_exptl_crystal_size_min          0.35
_refine_diff_density_max         0.316
_refine_diff_density_min         -0.190
_refine_diff_density_rms         0.047
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   -0.005(10)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.033
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     182
_refine_ls_number_reflns         4293
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.033
_refine_ls_R_factor_all          0.0295
_refine_ls_R_factor_gt           0.0272
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[σ²(Fo²)+(0.0374P)²+0.0000P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0635
_refine_ls_wR_factor_ref         0.0649
_reflns_number_gt                4076
_reflns_number_total             4293
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja109678y_si_002_2.cif
_cod_data_source_block           09120
_cod_original_sg_symbol_H-M      'R 3'
_cod_database_code               4105819
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 1.0000 1.0000 0.86628(2) 0.01165(8) Uani 1 3 d S
P1 P 0.86092(2) 0.91897(2) 0.88907(3) 0.01268(8) Uani 1 1 d .
Si Si 1.0000 1.0000 1.03884(5) 0.01237(14) Uani 1 3 d S
Na Na 1.0000 1.0000 0.47630(8) 0.0175(2) Uani 1 3 d S
O1 O 1.0000 1.0000 0.64315(15) 0.0282(5) Uani 1 3 d S
C7 C 0.78618(9) 0.96604(9) 0.89431(12) 0.0150(3) Uani 1 1 d .
H7 H 0.7987 1.0028 0.8321 0.018 Uiso 1 1 calc R
C13 C 1.0000 1.0000 0.7339(2) 0.0173(5) Uani 1 3 d S
O2 O 0.97680(8) 0.86722(7) 0.44077(10) 0.0268(3) Uani 1 1 d .
C6 C 0.83128(9) 0.86460(9) 1.01548(11) 0.0142(3) Uani 1 1 d .
C2 C 0.87634(10) 0.87620(10) 1.19153(12) 0.0179(3) Uani 1 1 d .
H2 H 0.9181 0.9051 1.2435 0.021 Uiso 1 1 calc R
C10 C 0.79423(10) 0.82812(10) 0.79782(12) 0.0174(3) Uani 1 1 d .
H10 H 0.7351 0.7936 0.8277 0.021 Uiso 1 1 calc R
C1 C 0.89456(9) 0.90781(9) 1.09178(11) 0.0140(3) Uani 1 1 d .
C8 C 0.80733(10) 1.02597(10) 0.98667(12) 0.0188(3) Uani 1 1 d .
H8A H 0.7761 1.0578 0.9810 0.028 Uiso 1 1 calc R
H8B H 0.8695 1.0668 0.9886 0.028 Uiso 1 1 calc R
H8C H 0.7899 0.9916 1.0495 0.028 Uiso 1 1 calc R
C5 C 0.75352(10) 0.79051(9) 1.04070(12) 0.0174(3) Uani 1 1 d .
H5 H 0.7116 0.7608 0.9891 0.021 Uiso 1 1 calc R
C3 C 0.79792(10) 0.80294(10) 1.21657(12) 0.0200(3) Uani 1 1 d .
H3 H 0.7865 0.7828 1.2851 0.024 Uiso 1 1 calc R
C15 C 1.02110(11) 0.76319(12) 0.45852(14) 0.0265(4) Uani 1 1 d .
H15A H 1.0725 0.7801 0.5017 0.032 Uiso 1 1 calc R
H15B H 1.0124 0.7150 0.4135 0.032 Uiso 1 1 calc R
C4 C 0.73695(10) 0.75989(10) 1.14091(12) 0.0195(3) Uani 1 1 d .
H4 H 0.6840 0.7096 1.1573 0.023 Uiso 1 1 calc R
C11 C 0.83012(11) 0.76782(11) 0.78295(14) 0.0241(3) Uani 1 1 d .
H11A H 0.7926 0.7211 0.7363 0.036 Uiso 1 1 calc R
H11B H 0.8326 0.7434 0.8490 0.036 Uiso 1 1 calc R
H11C H 0.8883 0.8001 0.7539 0.036 Uiso 1 1 calc R
C9 C 0.68854(9) 0.90246(10) 0.89456(12) 0.0182(3) Uani 1 1 d .
H9A H 0.6730 0.8662 0.9558 0.027 Uiso 1 1 calc R
H9B H 0.6728 0.8659 0.8336 0.027 Uiso 1 1 calc R
H9C H 0.6575 0.9347 0.8945 0.027 Uiso 1 1 calc R
C12 C 0.78525(11) 0.86282(11) 0.69384(13) 0.0231(3) Uani 1 1 d .
H12A H 0.8424 0.8977 0.6631 0.035 Uiso 1 1 calc R
H12B H 0.7585 0.8985 0.7035 0.035 Uiso 1 1 calc R
H12C H 0.7491 0.8144 0.6486 0.035 Uiso 1 1 calc R
C14 C 1.03183(13) 0.83943(13) 0.39561(16) 0.0331(4) Uani 1 1 d .
H14A H 1.0926 0.8867 0.3970 0.040 Uiso 1 1 calc R
H14B H 1.0150 0.8219 0.3237 0.040 Uiso 1 1 calc R
C16 C 0.94114(12) 0.73703(12) 0.52480(15) 0.0307(4) Uani 1 1 d .
H16A H 0.8987 0.6749 0.5169 0.037 Uiso 1 1 calc R
H16B H 0.9570 0.7495 0.5978 0.037 Uiso 1 1 calc R
C17 C 0.90551(12) 0.79237(12) 0.48389(16) 0.0312(4) Uani 1 1 d .
H17A H 0.8610 0.7605 0.4312 0.037 Uiso 1 1 calc R
H17B H 0.8792 0.8087 0.5398 0.037 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 0.0033 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'
O O 0.0106 0.0060 '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'
Si Si 0.0817 0.0704 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
P P 0.1023 0.0942 '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
C13 Fe P1 97.844(13) . 3_675
C13 Fe P1 97.843(13) . 2_765
P1 Fe P1 118.168(6) 3_675 2_765
C13 Fe P1 97.843(13) . .
P1 Fe P1 118.169(6) 3_675 .
P1 Fe P1 118.168(6) 2_765 .
C13 Fe Si 180.000(1) . .
P1 Fe Si 82.156(13) 3_675 .
P1 Fe Si 82.157(13) 2_765 .
P1 Fe Si 82.157(13) . .
C6 P1 C10 102.74(7) . .
C6 P1 C7 96.88(6) . .
C10 P1 C7 97.03(7) . .
C6 P1 Fe 113.67(5) . .
C10 P1 Fe 120.38(5) . .
C7 P1 Fe 121.99(5) . .
C1 Si C1 107.62(5) . 3_675
C1 Si C1 107.62(5) . 2_765
C1 Si C1 107.62(5) 3_675 2_765
C1 Si Fe 111.26(5) . .
C1 Si Fe 111.26(5) 3_675 .
C1 Si Fe 111.26(5) 2_765 .
O1 Na O2 101.94(4) . 3_675
O1 Na O2 101.94(4) . .
O2 Na O2 115.83(3) 3_675 .
O1 Na O2 101.94(4) . 2_765
O2 Na O2 115.84(3) 3_675 2_765
O2 Na O2 115.83(3) . 2_765
C13 O1 Na 180.000(1) . .
C8 C7 C9 107.95(12) . .
C8 C7 P1 110.82(10) . .
C9 C7 P1 117.56(10) . .
C8 C7 H7 106.6 . .
C9 C7 H7 106.6 . .
P1 C7 H7 106.6 . .
O1 C13 Fe 180.000(1) . .
C17 O2 C14 106.52(13) . .
C17 O2 Na 121.15(10) . .
C14 O2 Na 131.01(11) . .
C5 C6 C1 119.77(14) . .
C5 C6 P1 126.49(12) . .
C1 C6 P1 113.66(11) . .
C1 C2 C3 121.40(15) . .
C1 C2 H2 119.3 . .
C3 C2 H2 119.3 . .
C11 C10 C12 109.91(14) . .
C11 C10 P1 112.55(11) . .
C12 C10 P1 111.17(11) . .
C11 C10 H10 107.7 . .
C12 C10 H10 107.7 . .
P1 C10 H10 107.7 . .
C2 C1 C6 118.54(14) . .
C2 C1 Si 128.27(12) . .
C6 C1 Si 113.03(11) . .
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 . .
C4 C5 C6 120.61(14) . .
C4 C5 H5 119.7 . .
C6 C5 H5 119.7 . .
C4 C3 C2 119.69(15) . .
C4 C3 H3 120.2 . .
C2 C3 H3 120.2 . .
C14 C15 C16 105.07(14) . .
C14 C15 H15A 110.7 . .
C16 C15 H15A 110.7 . .
C14 C15 H15B 110.7 . .
C16 C15 H15B 110.7 . .
H15A C15 H15B 108.8 . .
C3 C4 C5 119.95(14) . .
C3 C4 H4 120.0 . .
C5 C4 H4 120.0 . .
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 . .
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 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 . .
O2 C14 C15 106.71(14) . .
O2 C14 H14A 110.4 . .
C15 C14 H14A 110.4 . .
O2 C14 H14B 110.4 . .
C15 C14 H14B 110.4 . .
H14A C14 H14B 108.6 . .
C17 C16 C15 103.52(14) . .
C17 C16 H16A 111.1 . .
C15 C16 H16A 111.1 . .
C17 C16 H16B 111.1 . .
C15 C16 H16B 111.1 . .
H16A C16 H16B 109.0 . .
O2 C17 C16 106.39(14) . .
O2 C17 H17A 110.5 . .
C16 C17 H17A 110.5 . .
O2 C17 H17B 110.5 . .
C16 C17 H17B 110.5 . .
H17A C17 H17B 108.6 . .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
Fe C13 1.732(3) .
Fe P1 2.1864(4) 3_675
Fe P1 2.1864(4) 2_765
Fe P1 2.1864(4) .
Fe Si 2.2586(8) .
P1 C6 1.8574(15) .
P1 C10 1.8855(16) .
P1 C7 1.9059(15) .
Si C1 1.9109(15) .
Si C1 1.9109(15) 3_675
Si C1 1.9109(15) 2_765
Na O1 2.184(2) .
Na O2 2.2475(11) 3_675
Na O2 2.2475(11) .
Na O2 2.2476(11) 2_765
O1 C13 1.188(3) .
C7 C8 1.533(2) .
C7 C9 1.537(2) .
C7 H7 1.0000 .
O2 C17 1.426(2) .
O2 C14 1.434(2) .
C6 C5 1.400(2) .
C6 C1 1.415(2) .
C2 C1 1.395(2) .
C2 C3 1.399(2) .
C2 H2 0.9500 .
C10 C11 1.520(2) .
C10 C12 1.537(2) .
C10 H10 1.0000 .
C8 H8A 0.9800 .
C8 H8B 0.9800 .
C8 H8C 0.9800 .
C5 C4 1.395(2) .
C5 H5 0.9500 .
C3 C4 1.387(2) .
C3 H3 0.9500 .
C15 C14 1.522(3) .
C15 C16 1.533(2) .
C15 H15A 0.9900 .
C15 H15B 0.9900 .
C4 H4 0.9500 .
C11 H11A 0.9800 .
C11 H11B 0.9800 .
C11 H11C 0.9800 .
C9 H9A 0.9800 .
C9 H9B 0.9800 .
C9 H9C 0.9800 .
C12 H12A 0.9800 .
C12 H12B 0.9800 .
C12 H12C 0.9800 .
C14 H14A 0.9900 .
C14 H14B 0.9900 .
C16 C17 1.519(2) .
C16 H16A 0.9900 .
C16 H16B 0.9900 .
C17 H17A 0.9900 .
C17 H17B 0.9900 .
