#------------------------------------------------------------------------------
#$Date: 2016-02-16 03:10:39 +0200 (Tue, 16 Feb 2016) $
#$Revision: 176453 $
#$URL: svn://www.crystallography.net/cod/cif/7/01/26/7012695.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_7012695
loop_
_publ_author_name
'Okazaki, Masaaki'
'Iwata, Masatoshi'
'Tobita, Hiromi'
'Ogino, Hiroshi'
_publ_section_title
;
 Reactions of M[(η5-C5Me5)Fe(CO)2] with ClSiMe2NR2 in THF, Et2O and
 toluene (M = Li and K; R = Me, Et, iPr and Ph)
;
_journal_issue                   6
_journal_name_full               'Dalton Transactions'
_journal_page_first              1114
_journal_paper_doi               10.1039/b300261f
_journal_year                    2003
_chemical_formula_moiety         'C30 H39 Fe N O3 Si '
_chemical_formula_sum            'C30 H39 Fe N O3 Si'
_chemical_formula_weight         545.58
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_symmetry_Int_Tables_number      2
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_audit_creation_date             'Tue Jan 28 13:58:04 2003'
_audit_creation_method           'by teXsan'
_cell_angle_alpha                96.519(5)
_cell_angle_beta                 97.382(3)
_cell_angle_gamma                93.474(1)
_cell_formula_units_Z            2
_cell_length_a                   8.4866(8)
_cell_length_b                   9.4172(5)
_cell_length_c                   17.867(2)
_cell_measurement_reflns_used    7442
_cell_measurement_temperature    150.2
_cell_measurement_theta_max      27.4
_cell_measurement_theta_min      1.2
_cell_volume                     1402.8(2)
_computing_cell_refinement       PROCESS-AUTO
_computing_data_collection       PROCESS-AUTO
_computing_data_reduction        'teXsan Ver. 1.11'
_computing_publication_material  'teXsan Ver. 1.11'
_computing_structure_refinement  'teXsan Ver. 1.10'
_computing_structure_solution    'DIRDIF94 (PATTY)'
_diffrn_detector_area_resol_mean 10.00
_diffrn_measured_fraction_theta_full 0.8564
_diffrn_measured_fraction_theta_max 0.8564
_diffrn_measurement_device_type  'Rigaku RAXIS-RAPID Imaging Plate'
_diffrn_measurement_method       ω
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.7107
_diffrn_reflns_av_R_equivalents  0.032
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_number            11070
_diffrn_reflns_theta_full        27.46
_diffrn_reflns_theta_max         27.46
_exptl_absorpt_coefficient_mu    0.611
_exptl_absorpt_correction_T_max  0.931
_exptl_absorpt_correction_T_min  0.838
_exptl_absorpt_correction_type   integration
_exptl_absorpt_process_details   '(Higashi, 1999)'
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.291
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_size_max          0.350
_exptl_crystal_size_mid          0.300
_exptl_crystal_size_min          0.100
_refine_diff_density_max         0.28
_refine_diff_density_min         -0.61
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.630
_refine_ls_hydrogen_treatment    noref
_refine_ls_number_parameters     325
_refine_ls_number_reflns         5470
_refine_ls_R_factor_gt           0.0457
_refine_ls_shift/su_max          0.0012
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w = 1/[σ²(Fo²) + (0.09500(Max(Fo²,0) + 2Fc²)/3)²]'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_ref         0.1798
_reflns_number_gt                4806
_reflns_number_total             5470
_reflns_threshold_expression     F²>2.0σ(F²)
_cod_data_source_file            b300261f.txt
_cod_data_source_block           of_1-Ph
_cod_original_cell_volume        1402.9(2)
_cod_original_formula_sum        'C30 H39 Fe N O3 Si '
_cod_database_code               7012695
loop_
_symmetry_equiv_pos_as_xyz
x,y,z
-x,-y,-z
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_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
Fe Fe -0.43767(4) 0.21113(4) -0.14189(2) 0.0174(1) Uani 1.00 d . . .
Si Si -0.14590(9) -0.32214(8) -0.35739(4) 0.0182(2) Uani 1.00 d . . .
O1 O -0.1498(2) -0.2997(2) -0.2644(1) 0.0219(5) Uani 1.00 d . . .
O2 O -0.3742(3) 0.2179(3) -0.2975(1) 0.0348(7) Uani 1.00 d . . .
O3 O -0.6562(3) -0.0446(3) -0.1691(1) 0.0376(7) Uani 1.00 d . . .
N N 0.0360(3) -0.3878(2) -0.3762(1) 0.0184(6) Uani 1.00 d . . .
C1 C -0.2441(3) 0.0909(3) -0.1216(2) 0.0206(7) Uani 1.00 d . . .
C2 C -0.2166(4) -0.0303(3) -0.1819(2) 0.0232(7) Uani 1.00 d . . .
C3 C -0.0843(4) -0.1208(3) -0.1530(2) 0.0223(7) Uani 1.00 d . . .
C4 C -0.0217(4) -0.2124(3) -0.2165(2) 0.0245(7) Uani 1.00 d . . .
C5 C -0.1589(4) -0.1478(3) -0.3954(2) 0.0258(8) Uani 1.00 d . . .
C6 C -0.3201(4) -0.4467(3) -0.3976(2) 0.0267(8) Uani 1.00 d . . .
C7 C 0.1584(3) -0.2917(3) -0.3958(1) 0.0182(6) Uani 1.00 d . . .
C8 C 0.1516(4) -0.2532(3) -0.4691(2) 0.0258(7) Uani 1.00 d . . .
C9 C 0.2691(4) -0.1589(4) -0.4865(2) 0.0316(8) Uani 1.00 d . . .
C10 C 0.3936(4) -0.1024(3) -0.4312(2) 0.0299(8) Uani 1.00 d . . .
C11 C 0.4021(4) -0.1406(3) -0.3585(2) 0.0257(7) Uani 1.00 d . . .
C12 C 0.2845(3) -0.2350(3) -0.3406(2) 0.0215(7) Uani 1.00 d . . .
C13 C 0.0815(3) -0.5261(3) -0.3638(2) 0.0204(7) Uani 1.00 d . . .
C14 C 0.2131(4) -0.5811(3) -0.3928(2) 0.0240(7) Uani 1.00 d . . .
C15 C 0.2520(4) -0.7193(3) -0.3829(2) 0.0318(8) Uani 1.00 d . . .
C16 C 0.1629(4) -0.8060(3) -0.3441(2) 0.0357(9) Uani 1.00 d . . .
C17 C 0.0332(4) -0.7524(3) -0.3151(2) 0.0335(9) Uani 1.00 d . . .
C18 C -0.0069(4) -0.6136(3) -0.3232(2) 0.0259(8) Uani 1.00 d . . .
C19 C -0.3989(3) 0.2141(3) -0.2359(2) 0.0227(7) Uani 1.00 d . . .
C20 C -0.5655(3) 0.0550(3) -0.1601(2) 0.0237(7) Uani 1.00 d . . .
C21 C -0.6076(4) 0.3405(3) -0.0984(2) 0.0252(7) Uani 1.00 d . . .
C22 C -0.4995(4) 0.4257(3) -0.1325(2) 0.0236(7) Uani 1.00 d . . .
C23 C -0.3418(3) 0.4172(3) -0.0928(2) 0.0215(7) Uani 1.00 d . . .
C24 C -0.3559(3) 0.3298(3) -0.0333(1) 0.0202(7) Uani 1.00 d . . .
C25 C -0.5180(4) 0.2800(3) -0.0375(2) 0.0224(7) Uani 1.00 d . . .
C26 C -0.7858(4) 0.3219(4) -0.1181(2) 0.0395(10) Uani 1.00 d . . .
C27 C -0.5418(5) 0.5154(4) -0.1955(2) 0.0387(10) Uani 1.00 d . . .
C28 C -0.1911(4) 0.4932(3) -0.1070(2) 0.0338(9) Uani 1.00 d . . .
C29 C -0.2251(4) 0.3002(3) 0.0262(2) 0.0318(8) Uani 1.00 d . . .
C30 C -0.5871(4) 0.1905(3) 0.0158(2) 0.0354(9) Uani 1.00 d . . .
H1 H -0.1419 0.1567 -0.1141 0.0249 Uiso 1.00 calc . . .
H2 H -0.2664 0.0503 -0.0745 0.0249 Uiso 1.00 calc . . .
H3 H -0.3249 -0.0970 -0.1984 0.0283 Uiso 1.00 calc . . .
H4 H -0.1865 0.0109 -0.2257 0.0283 Uiso 1.00 calc . . .
H5 H 0.0090 -0.0596 -0.1253 0.0262 Uiso 1.00 calc . . .
H6 H -0.1271 -0.1866 -0.1175 0.0262 Uiso 1.00 calc . . .
H7 H 0.0536 -0.2783 -0.1961 0.0310 Uiso 1.00 calc . . .
H8 H 0.0374 -0.1538 -0.2470 0.0310 Uiso 1.00 calc . . .
H9 H -0.0784 -0.0911 -0.3769 0.0324 Uiso 1.00 calc . . .
H10 H -0.1718 -0.1656 -0.4469 0.0324 Uiso 1.00 calc . . .
H11 H -0.2512 -0.1139 -0.3840 0.0324 Uiso 1.00 calc . . .
H12 H -0.4121 -0.4012 -0.3916 0.0325 Uiso 1.00 calc . . .
H13 H -0.3379 -0.4472 -0.4381 0.0325 Uiso 1.00 calc . . .
H14 H -0.3267 -0.5198 -0.3802 0.0325 Uiso 1.00 calc . . .
H15 H 0.0701 -0.2934 -0.5058 0.0306 Uiso 1.00 calc . . .
H16 H 0.2657 -0.1423 -0.5300 0.0371 Uiso 1.00 calc . . .
H17 H 0.4637 -0.0448 -0.4391 0.0348 Uiso 1.00 calc . . .
H18 H 0.4894 -0.0987 -0.3197 0.0312 Uiso 1.00 calc . . .
H19 H 0.2899 -0.2564 -0.2876 0.0263 Uiso 1.00 calc . . .
H20 H 0.2800 -0.5224 -0.4215 0.0291 Uiso 1.00 calc . . .
H21 H 0.3179 -0.7422 -0.3999 0.0388 Uiso 1.00 calc . . .
H22 H 0.1825 -0.8826 -0.3403 0.0436 Uiso 1.00 calc . . .
H23 H -0.0373 -0.8178 -0.2881 0.0407 Uiso 1.00 calc . . .
H24 H -0.0763 -0.5800 -0.3018 0.0311 Uiso 1.00 calc . . .
H25 H -0.8462 0.3709 -0.0765 0.0477 Uiso 1.00 calc . . .
H26 H -0.8157 0.3517 -0.1631 0.0477 Uiso 1.00 calc . . .
H27 H -0.8271 0.2239 -0.1285 0.0477 Uiso 1.00 calc . . .
H28 H -0.4459 0.5263 -0.2233 0.0492 Uiso 1.00 calc . . .
H29 H -0.6219 0.4780 -0.2284 0.0492 Uiso 1.00 calc . . .
H30 H -0.5659 0.6005 -0.1744 0.0492 Uiso 1.00 calc . . .
H31 H -0.1073 0.4328 -0.1116 0.0429 Uiso 1.00 calc . . .
H32 H -0.2033 0.5169 -0.1515 0.0429 Uiso 1.00 calc . . .
H33 H -0.1674 0.5803 -0.0631 0.0429 Uiso 1.00 calc . . .
H34 H -0.2401 0.2030 0.0403 0.0388 Uiso 1.00 calc . . .
H35 H -0.1240 0.3112 0.0105 0.0388 Uiso 1.00 calc . . .
H36 H -0.2207 0.3566 0.0680 0.0388 Uiso 1.00 calc . . .
H37 H -0.6175 0.2497 0.0590 0.0443 Uiso 1.00 calc . . .
H38 H -0.6876 0.1477 -0.0063 0.0443 Uiso 1.00 calc . . .
H39 H -0.5190 0.1160 0.0312 0.0443 Uiso 1.00 calc . . .
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.003 0.002
;International Tables for Crystallography
(1992, Vol. C, Tables 4.2.6.8 and 6.1.1.1)
;
H H 0.000 0.000
;International Tables for Crystallography
(1992, Vol. C, Table 6.1.1.2)
;
Fe Fe 0.346 0.844
;International Tables for Crystallography
(1992, Vol. C, Tables 4.2.6.8 and 6.1.1.1)
;
Si Si 0.082 0.070
;International Tables for Crystallography
(1992, Vol. C, Tables 4.2.6.8 and 6.1.1.1)
;
N N 0.006 0.003
;International Tables for Crystallography
(1992, Vol. C, Tables 4.2.6.8 and 6.1.1.1)
;
O O 0.011 0.006
;International Tables for Crystallography
(1992, Vol. C, Tables 4.2.6.8 and 6.1.1.1)
;
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_2
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
C1 FE C19 89.3(1) . . . yes
C1 FE C20 90.4(1) . . . yes
C1 FE C21 148.8(1) . . . yes
C1 FE C22 141.1(1) . . . yes
C1 FE C23 101.5(1) . . . yes
C1 FE C24 86.4(1) . . . yes
C1 FE C25 109.2(1) . . . yes
C19 FE C20 96.0(1) . . . yes
C19 FE C21 120.5(1) . . . yes
C19 FE C22 92.7(1) . . . yes
C19 FE C23 100.7(1) . . . yes
C19 FE C24 137.1(1) . . . yes
C19 FE C25 158.7(1) . . . yes
C20 FE C21 94.8(1) . . . yes
C20 FE C22 127.9(1) . . . yes
C20 FE C23 159.5(1) . . . yes
C20 FE C24 126.7(1) . . . yes
C20 FE C25 94.2(1) . . . yes
C21 FE C22 39.3(1) . . . yes
C21 FE C23 66.5(1) . . . yes
C21 FE C24 65.9(1) . . . yes
C21 FE C25 39.8(1) . . . yes
C22 FE C23 40.0(1) . . . yes
C22 FE C24 66.2(1) . . . yes
C22 FE C25 66.4(1) . . . yes
C23 FE C24 39.4(1) . . . yes
C23 FE C25 66.2(1) . . . yes
C24 FE C25 38.9(1) . . . yes
O1 SI N 109.5(1) . . . yes
O1 SI C5 109.9(1) . . . yes
O1 SI C6 105.7(1) . . . yes
N SI C5 107.4(1) . . . yes
N SI C6 113.2(1) . . . yes
C5 SI C6 111.1(1) . . . yes
SI O1 C4 118.7(2) . . . yes
SI N C7 119.4(2) . . . yes
SI N C13 124.4(2) . . . yes
C7 N C13 115.7(2) . . . yes
FE C1 C2 119.2(2) . . . yes
C1 C2 C3 112.0(2) . . . yes
C2 C3 C4 113.0(2) . . . yes
O1 C4 C3 111.0(2) . . . yes
N C7 C8 120.9(2) . . . yes
N C7 C12 119.7(2) . . . yes
C8 C7 C12 119.5(2) . . . yes
C7 C8 C9 119.9(3) . . . yes
C8 C9 C10 120.3(3) . . . yes
C9 C10 C11 120.3(3) . . . yes
C10 C11 C12 119.8(3) . . . yes
C7 C12 C11 120.2(3) . . . yes
N C13 C14 121.2(2) . . . yes
N C13 C18 120.9(3) . . . yes
C14 C13 C18 117.9(3) . . . yes
C13 C14 C15 120.5(3) . . . yes
C14 C15 C16 121.4(3) . . . yes
C15 C16 C17 118.4(3) . . . yes
C16 C17 C18 121.3(3) . . . yes
C13 C18 C17 120.4(3) . . . yes
FE C19 O2 179.1(3) . . . yes
FE C20 O3 175.8(3) . . . yes
FE C21 C22 70.4(2) . . . yes
FE C21 C25 70.2(2) . . . yes
FE C21 C26 127.7(2) . . . yes
C22 C21 C25 108.1(3) . . . yes
C22 C21 C26 127.1(3) . . . yes
C25 C21 C26 124.8(3) . . . yes
FE C22 C21 70.3(2) . . . yes
FE C22 C23 69.8(1) . . . yes
FE C22 C27 127.9(2) . . . yes
C21 C22 C23 107.7(2) . . . yes
C21 C22 C27 126.4(3) . . . yes
C23 C22 C27 125.8(3) . . . yes
FE C23 C22 70.2(2) . . . yes
FE C23 C24 71.4(1) . . . yes
FE C23 C28 126.9(2) . . . yes
C22 C23 C24 107.8(2) . . . yes
C22 C23 C28 126.8(3) . . . yes
C24 C23 C28 125.3(3) . . . yes
FE C24 C23 69.2(1) . . . yes
FE C24 C25 69.7(1) . . . yes
FE C24 C29 129.0(2) . . . yes
C23 C24 C25 108.3(2) . . . yes
C23 C24 C29 126.7(3) . . . yes
C25 C24 C29 125.0(3) . . . yes
FE C25 C21 69.9(2) . . . yes
FE C25 C24 71.4(2) . . . yes
FE C25 C30 128.2(2) . . . yes
C21 C25 C24 108.1(3) . . . yes
C21 C25 C30 125.4(3) . . . yes
C24 C25 C30 126.3(3) . . . yes
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_1
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
FE C1 2.068(3) . . yes
FE C19 1.757(3) . . yes
FE C20 1.747(3) . . yes
FE C21 2.111(3) . . yes
FE C22 2.112(3) . . yes
FE C23 2.107(3) . . yes
FE C24 2.136(3) . . yes
FE C25 2.115(3) . . yes
SI O1 1.655(2) . . yes
SI N 1.755(2) . . yes
SI C5 1.851(3) . . yes
SI C6 1.845(3) . . yes
O1 C4 1.444(3) . . yes
O2 C19 1.149(4) . . yes
O3 C20 1.159(4) . . yes
N C7 1.439(3) . . yes
N C13 1.414(4) . . yes
C1 C2 1.528(4) . . yes
C2 C3 1.523(4) . . yes
C3 C4 1.517(4) . . yes
C7 C8 1.393(4) . . yes
C7 C12 1.394(4) . . yes
C8 C9 1.383(4) . . yes
C9 C10 1.385(4) . . yes
C10 C11 1.382(4) . . yes
C11 C12 1.388(4) . . yes
C13 C14 1.393(4) . . yes
C13 C18 1.403(4) . . yes
C14 C15 1.386(4) . . yes
C15 C16 1.382(5) . . yes
C16 C17 1.374(5) . . yes
C17 C18 1.389(4) . . yes
C21 C22 1.422(4) . . yes
C21 C25 1.439(4) . . yes
C21 C26 1.503(4) . . yes
C22 C23 1.443(4) . . yes
C22 C27 1.503(4) . . yes
C23 C24 1.429(4) . . yes
C23 C28 1.491(4) . . yes
C24 C25 1.416(4) . . yes
C24 C29 1.497(4) . . yes
C25 C30 1.492(4) . . yes
