#------------------------------------------------------------------------------
#$Date: 2016-03-25 16:04:37 +0200 (Fri, 25 Mar 2016) $
#$Revision: 179950 $
#$URL: svn://www.crystallography.net/cod/cif/7/02/45/7024596.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_7024596
loop_
_publ_author_name
'Ramos, Alberto'
'Stephan, Douglas W.'
_publ_section_title
;
 Titanium ferrocenyl-phosphinimide complexes.
;
_journal_issue                   5
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              1328
_journal_page_last               1338
_journal_paper_doi               10.1039/b918919j
_journal_volume                  39
_journal_year                    2010
_chemical_formula_sum            'C32 H72 Fe N2 P2 Si2'
_chemical_formula_weight         658.89
_space_group_IT_number           15
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-C 2yc'
_symmetry_space_group_name_H-M   'C 1 2/c 1'
_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                 104.8850(10)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   26.915(3)
_cell_length_b                   9.7197(11)
_cell_length_c                   15.1251(18)
_cell_measurement_temperature    298(2)
_cell_measurement_theta_max      25.0
_cell_measurement_theta_min      2.0
_cell_volume                     3824.0(8)
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      298(2)
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 1.000
_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  0.0299
_diffrn_reflns_av_sigmaI/netI    0.0213
_diffrn_reflns_limit_h_max       32
_diffrn_reflns_limit_h_min       -32
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            17871
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         25.00
_diffrn_reflns_theta_min         2.24
_exptl_absorpt_coefficient_mu    0.563
_exptl_absorpt_correction_T_max  1.000000
_exptl_absorpt_correction_T_min  0.495593
_exptl_absorpt_correction_type   empirical
_exptl_crystal_density_diffrn    1.144
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             1448
_exptl_crystal_size_max          0.28
_exptl_crystal_size_mid          0.16
_exptl_crystal_size_min          0.14
_refine_diff_density_max         0.297
_refine_diff_density_min         -0.178
_refine_diff_density_rms         0.044
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.034
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     178
_refine_ls_number_reflns         3370
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.034
_refine_ls_R_factor_all          0.0435
_refine_ls_R_factor_gt           0.0338
_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)+(0.0611P)²+1.3658P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0910
_refine_ls_wR_factor_ref         0.0995
_reflns_number_gt                2817
_reflns_number_total             3370
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            b918919j.txt
_cod_data_source_block           '[Fe{5-C5H4PtBu2(NSiMe3)}2]'
_cod_original_cell_volume        3824.1(8)
_cod_original_sg_symbol_H-M      C2/c
_cod_database_code               7024596
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, y, -z+1/2'
'x+1/2, y+1/2, z'
'-x+1/2, y+1/2, -z+1/2'
'-x, -y, -z'
'x, -y, z-1/2'
'-x+1/2, -y+1/2, -z'
'x+1/2, -y+1/2, 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_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
Fe1 Fe 0.0000 0.77663(4) 0.2500 0.04281(14) Uani 1 2 d S
P1 P -0.125066(19) 0.85071(5) 0.27408(4) 0.04253(16) Uani 1 1 d .
N1 N -0.11803(8) 0.7612(2) 0.35910(13) 0.0603(5) Uani 1 1 d .
Si1 Si -0.11931(3) 0.65817(6) 0.44491(4) 0.05396(18) Uani 1 1 d .
C1 C -0.07800(7) 0.8104(2) 0.21158(13) 0.0435(4) Uani 1 1 d .
C2 C -0.05273(7) 0.8921(2) 0.15734(13) 0.0493(5) Uani 1 1 d .
H2A H -0.0533 0.9928 0.1534 0.059 Uiso 1 1 calc R
C3 C -0.02610(9) 0.8028(3) 0.11141(15) 0.0620(6) Uani 1 1 d .
H3A H -0.0053 0.8311 0.0701 0.074 Uiso 1 1 calc R
C4 C -0.03395(9) 0.6678(3) 0.13604(18) 0.0678(7) Uani 1 1 d .
H4A H -0.0199 0.5851 0.1143 0.081 Uiso 1 1 calc R
C5 C -0.06543(8) 0.6703(2) 0.19768(17) 0.0559(6) Uani 1 1 d .
H5A H -0.0771 0.5896 0.2256 0.067 Uiso 1 1 calc R
C6 C -0.12012(8) 1.0373(2) 0.30537(16) 0.0539(5) Uani 1 1 d .
C7 C -0.06377(10) 1.0688(3) 0.3526(2) 0.0745(7) Uani 1 1 d .
H7A H -0.0603 1.1642 0.3693 0.112 Uiso 1 1 calc R
H7B H -0.0428 1.0487 0.3116 0.112 Uiso 1 1 calc R
H7C H -0.0529 1.0131 0.4066 0.112 Uiso 1 1 calc R
C8 C -0.15083(12) 1.0619(3) 0.3766(2) 0.0799(8) Uani 1 1 d .
H8A H -0.1487 1.1573 0.3936 0.120 Uiso 1 1 calc R
H8B H -0.1368 1.0065 0.4297 0.120 Uiso 1 1 calc R
H8C H -0.1861 1.0373 0.3509 0.120 Uiso 1 1 calc R
C9 C -0.13895(12) 1.1372(3) 0.2250(2) 0.0780(8) Uani 1 1 d .
H9A H -0.1350 1.2302 0.2472 0.117 Uiso 1 1 calc R
H9B H -0.1745 1.1197 0.1963 0.117 Uiso 1 1 calc R
H9C H -0.1191 1.1243 0.1813 0.117 Uiso 1 1 calc R
C10 C -0.18672(8) 0.8130(3) 0.18576(17) 0.0596(6) Uani 1 1 d .
C11 C -0.18797(11) 0.8708(4) 0.09111(18) 0.0882(9) Uani 1 1 d .
H11A H -0.2203 0.8483 0.0492 0.132 Uiso 1 1 calc R
H11B H -0.1604 0.8313 0.0699 0.132 Uiso 1 1 calc R
H11C H -0.1840 0.9689 0.0949 0.132 Uiso 1 1 calc R
C12 C -0.19108(10) 0.6554(3) 0.1781(2) 0.0828(8) Uani 1 1 d .
H12A H -0.2222 0.6311 0.1336 0.124 Uiso 1 1 calc R
H12B H -0.1916 0.6173 0.2364 0.124 Uiso 1 1 calc R
H12C H -0.1621 0.6193 0.1595 0.124 Uiso 1 1 calc R
C13 C -0.23291(9) 0.8653(4) 0.2180(2) 0.0892(9) Uani 1 1 d .
H13A H -0.2641 0.8452 0.1723 0.134 Uiso 1 1 calc R
H13B H -0.2299 0.9629 0.2277 0.134 Uiso 1 1 calc R
H13C H -0.2336 0.8204 0.2743 0.134 Uiso 1 1 calc R
C14 C -0.11061(15) 0.4740(3) 0.4161(2) 0.0987(11) Uani 1 1 d .
H14A H -0.1376 0.4476 0.3640 0.148 Uiso 1 1 calc R
H14B H -0.1118 0.4169 0.4673 0.148 Uiso 1 1 calc R
H14C H -0.0780 0.4631 0.4022 0.148 Uiso 1 1 calc R
C15 C -0.18118(13) 0.6717(4) 0.4788(2) 0.1029(11) Uani 1 1 d .
H15A H -0.2092 0.6487 0.4275 0.154 Uiso 1 1 calc R
H15B H -0.1854 0.7641 0.4981 0.154 Uiso 1 1 calc R
H15C H -0.1807 0.6093 0.5282 0.154 Uiso 1 1 calc R
C16 C -0.06577(12) 0.7020(3) 0.54710(17) 0.0768(8) Uani 1 1 d .
H16A H -0.0335 0.6948 0.5314 0.115 Uiso 1 1 calc R
H16B H -0.0661 0.6393 0.5960 0.115 Uiso 1 1 calc R
H16C H -0.0702 0.7943 0.5663 0.115 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'
N N 0.0061 0.0033 '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
C5 Fe1 C5 118.46(13) 2 .
C5 Fe1 C4 40.82(9) 2 2
C5 Fe1 C4 102.89(10) . 2
C5 Fe1 C4 102.89(10) 2 .
C5 Fe1 C4 40.82(9) . .
C4 Fe1 C4 117.13(17) 2 .
C5 Fe1 C3 119.99(10) 2 .
C5 Fe1 C3 68.12(10) . .
C4 Fe1 C3 153.56(12) 2 .
C4 Fe1 C3 40.02(11) . .
C5 Fe1 C3 68.12(10) 2 2
C5 Fe1 C3 119.99(10) . 2
C4 Fe1 C3 40.02(11) 2 2
C4 Fe1 C3 153.56(12) . 2
C3 Fe1 C3 165.73(16) . 2
C5 Fe1 C2 68.42(9) 2 2
C5 Fe1 C2 158.01(9) . 2
C4 Fe1 C2 67.90(10) 2 2
C4 Fe1 C2 161.16(9) . 2
C3 Fe1 C2 128.73(10) . 2
C3 Fe1 C2 40.40(9) 2 2
C5 Fe1 C2 158.02(9) 2 .
C5 Fe1 C2 68.42(9) . .
C4 Fe1 C2 161.16(9) 2 .
C4 Fe1 C2 67.91(10) . .
C3 Fe1 C2 40.40(9) . .
C3 Fe1 C2 128.73(10) 2 .
C2 Fe1 C2 113.71(13) 2 .
C5 Fe1 C1 41.12(8) 2 2
C5 Fe1 C1 156.47(9) . 2
C4 Fe1 C1 68.83(9) 2 2
C4 Fe1 C1 121.86(9) . 2
C3 Fe1 C1 109.04(9) . 2
C3 Fe1 C1 68.53(8) 2 2
C2 Fe1 C1 40.82(8) 2 2
C2 Fe1 C1 125.60(8) . 2
C5 Fe1 C1 156.47(9) 2 .
C5 Fe1 C1 41.12(8) . .
C4 Fe1 C1 121.86(9) 2 .
C4 Fe1 C1 68.83(9) . .
C3 Fe1 C1 68.53(8) . .
C3 Fe1 C1 109.04(8) 2 .
C2 Fe1 C1 125.60(8) 2 .
C2 Fe1 C1 40.81(8) . .
C1 Fe1 C1 161.61(11) 2 .
N1 P1 C1 111.47(10) . .
N1 P1 C6 110.77(11) . .
C1 P1 C6 109.17(10) . .
N1 P1 C10 112.61(11) . .
C1 P1 C10 101.27(10) . .
C6 P1 C10 111.17(11) . .
P1 N1 Si1 171.59(15) . .
N1 Si1 C15 111.96(14) . .
N1 Si1 C14 111.65(13) . .
C15 Si1 C14 107.77(17) . .
N1 Si1 C16 110.17(12) . .
C15 Si1 C16 107.98(15) . .
C14 Si1 C16 107.10(14) . .
C5 C1 C2 106.16(18) . .
C5 C1 P1 120.44(16) . .
C2 C1 P1 132.77(16) . .
C5 C1 Fe1 68.09(11) . .
C2 C1 Fe1 69.51(11) . .
P1 C1 Fe1 133.53(11) . .
C3 C2 C1 108.4(2) . .
C3 C2 Fe1 69.61(13) . .
C1 C2 Fe1 69.68(11) . .
C4 C3 C2 108.4(2) . .
C4 C3 Fe1 69.24(15) . .
C2 C3 Fe1 69.99(12) . .
C3 C4 C5 108.5(2) . .
C3 C4 Fe1 70.74(13) . .
C5 C4 Fe1 69.24(13) . .
C4 C5 C1 108.6(2) . .
C4 C5 Fe1 69.94(13) . .
C1 C5 Fe1 70.79(11) . .
C7 C6 C8 106.8(2) . .
C7 C6 C9 109.2(2) . .
C8 C6 C9 109.2(2) . .
C7 C6 P1 108.00(15) . .
C8 C6 P1 108.18(16) . .
C9 C6 P1 115.15(17) . .
C11 C10 C13 110.6(2) . .
C11 C10 C12 108.2(2) . .
C13 C10 C12 107.5(2) . .
C11 C10 P1 113.38(16) . .
C13 C10 P1 110.42(19) . .
C12 C10 P1 106.49(17) . .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
Fe1 C5 2.020(2) 2
Fe1 C5 2.020(2) .
Fe1 C4 2.029(2) 2
Fe1 C4 2.029(2) .
Fe1 C3 2.048(2) .
Fe1 C3 2.048(2) 2
Fe1 C2 2.053(2) 2
Fe1 C2 2.053(2) .
Fe1 C1 2.0558(19) 2
Fe1 C1 2.0558(19) .
P1 N1 1.5234(19) .
P1 C1 1.807(2) .
P1 C6 1.871(2) .
P1 C10 1.880(2) .
N1 Si1 1.6469(19) .
Si1 C15 1.869(3) .
Si1 C14 1.871(3) .
Si1 C16 1.871(3) .
C1 C5 1.432(3) .
C1 C2 1.433(3) .
C2 C3 1.416(3) .
C3 C4 1.395(4) .
C4 C5 1.412(3) .
C6 C7 1.532(3) .
C6 C8 1.535(3) .
C6 C9 1.536(3) .
C10 C11 1.530(3) .
C10 C13 1.534(4) .
C10 C12 1.539(4) .
