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#$Date: 2016-03-25 16:04:37 +0200 (Fri, 25 Mar 2016) $
#$Revision: 179950 $
#$URL: svn://www.crystallography.net/cod/cif/7/02/45/7024597.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_7024597
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            'C28 H48 Cl6 Fe N2 P2 Ti'
_chemical_formula_weight         791.07
_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                 98.55(3)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   19.361(4)
_cell_length_b                   10.900(2)
_cell_length_c                   17.105(3)
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      25.0
_cell_measurement_theta_min      2.0
_cell_volume                     3569.6(12)
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 0.988
_diffrn_measured_fraction_theta_max 0.988
_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  0.0331
_diffrn_reflns_av_sigmaI/netI    0.0332
_diffrn_reflns_limit_h_max       24
_diffrn_reflns_limit_h_min       -24
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_number            12144
_diffrn_reflns_theta_full        27.52
_diffrn_reflns_theta_max         27.52
_diffrn_reflns_theta_min         3.11
_exptl_absorpt_coefficient_mu    1.191
_exptl_absorpt_correction_T_max  0.829
_exptl_absorpt_correction_T_min  0.661
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
multi-scan from symmetry-related measurements
Sortav (Blessing 1995)
;
_exptl_crystal_density_diffrn    1.472
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             1640
_exptl_crystal_size_max          0.23
_exptl_crystal_size_mid          0.21
_exptl_crystal_size_min          0.18
_refine_diff_density_max         0.746
_refine_diff_density_min         -0.622
_refine_diff_density_rms         0.073
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.064
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     182
_refine_ls_number_reflns         4060
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.064
_refine_ls_R_factor_all          0.0419
_refine_ls_R_factor_gt           0.0322
_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)+(0.0380P)²+5.6284P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0805
_refine_ls_wR_factor_ref         0.0864
_reflns_number_gt                3431
_reflns_number_total             4060
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            b918919j.txt
_cod_data_source_block           CpFe(C5H3(PBu2N)2TiCl2
_cod_original_cell_volume        3569.8(12)
_cod_original_sg_symbol_H-M      C2/c
_cod_database_code               7024597
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 0.26953(4) 0.2500 0.01558(10) Uani 1 2 d S
Ti1 Ti 0.0000 -0.15677(4) 0.2500 0.01294(11) Uani 1 2 d S
Cl1 Cl 0.04659(3) -0.27902(5) 0.16113(3) 0.03027(14) Uani 1 1 d .
Cl11 Cl 0.09442(3) -0.45789(5) 0.01319(3) 0.03179(14) Uani 1 1 d .
Cl22 Cl 0.17072(4) -0.59173(6) -0.09440(4) 0.04614(18) Uani 1 1 d .
P1 P -0.12141(2) 0.04244(4) 0.16870(3) 0.01388(11) Uani 1 1 d .
N1 N -0.06922(8) -0.06579(15) 0.19870(10) 0.0171(3) Uani 1 1 d .
C1 C -0.09912(10) 0.31012(19) 0.19451(13) 0.0212(4) Uani 1 1 d .
H1A H -0.1113 0.3389 0.1399 0.025 Uiso 1 1 calc R
C2 C -0.09515(9) 0.18409(18) 0.21945(11) 0.0164(4) Uani 1 1 d .
C3 C -0.07413(9) 0.1850(2) 0.30362(11) 0.0190(4) Uani 1 1 d .
H3A H -0.0668 0.1123 0.3376 0.023 Uiso 1 1 calc R
C4 C -0.06598(10) 0.3085(2) 0.32944(13) 0.0244(4) Uani 1 1 d .
H4A H -0.0521 0.3358 0.3841 0.029 Uiso 1 1 calc R
C5 C -0.08101(11) 0.3858(2) 0.26205(14) 0.0262(5) Uani 1 1 d .
H5A H -0.0790 0.4756 0.2622 0.031 Uiso 1 1 calc R
C6 C -0.20941(10) 0.01145(19) 0.19761(12) 0.0184(4) Uani 1 1 d .
C7 C -0.25579(11) 0.1261(2) 0.19109(14) 0.0270(5) Uani 1 1 d .
H7A H -0.3002 0.1060 0.2064 0.041 Uiso 1 1 calc R
H7B H -0.2626 0.1550 0.1375 0.041 Uiso 1 1 calc R
H7C H -0.2336 0.1889 0.2253 0.041 Uiso 1 1 calc R
C8 C -0.19764(11) -0.0309(2) 0.28429(13) 0.0261(5) Uani 1 1 d .
H8A H -0.2419 -0.0476 0.3010 0.039 Uiso 1 1 calc R
H8B H -0.1740 0.0325 0.3169 0.039 Uiso 1 1 calc R
H8C H -0.1697 -0.1040 0.2891 0.039 Uiso 1 1 calc R
C9 C -0.24565(11) -0.0938(2) 0.14737(13) 0.0252(5) Uani 1 1 d .
H9A H -0.2906 -0.1089 0.1626 0.038 Uiso 1 1 calc R
H9B H -0.2176 -0.1666 0.1556 0.038 Uiso 1 1 calc R
H9C H -0.2513 -0.0714 0.0925 0.038 Uiso 1 1 calc R
C10 C -0.12473(10) 0.06074(19) 0.05965(11) 0.0193(4) Uani 1 1 d .
C11 C -0.18529(11) 0.1409(2) 0.02075(12) 0.0260(5) Uani 1 1 d .
H11A H -0.1838 0.1464 -0.0350 0.039 Uiso 1 1 calc R
H11B H -0.1811 0.2216 0.0435 0.039 Uiso 1 1 calc R
H11C H -0.2288 0.1051 0.0293 0.039 Uiso 1 1 calc R
C12 C -0.12884(11) -0.0673(2) 0.02135(12) 0.0247(5) Uani 1 1 d .
H12A H -0.1306 -0.0591 -0.0348 0.037 Uiso 1 1 calc R
H12B H -0.1701 -0.1085 0.0324 0.037 Uiso 1 1 calc R
H12C H -0.0884 -0.1141 0.0426 0.037 Uiso 1 1 calc R
C13 C -0.05539(11) 0.1184(2) 0.04472(12) 0.0230(4) Uani 1 1 d .
H13A H -0.0559 0.1288 -0.0111 0.035 Uiso 1 1 calc R
H13B H -0.0174 0.0657 0.0656 0.035 Uiso 1 1 calc R
H13C H -0.0496 0.1969 0.0704 0.035 Uiso 1 1 calc R
C51 C 0.10122(19) -0.5924(3) -0.0409(2) 0.0671(11) Uani 1 1 d .
H51A H 0.1065 -0.6615 -0.0048 0.081 Uiso 1 1 calc R
H51B H 0.0582 -0.6041 -0.0772 0.081 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'
P P 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Ti Ti 0.2776 0.4457 '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
C3 Fe1 C3 126.14(12) . 2
C3 Fe1 C4 161.14(9) . 2
C3 Fe1 C4 40.71(8) 2 2
C3 Fe1 C4 40.71(8) . .
C3 Fe1 C4 161.15(9) 2 .
C4 Fe1 C4 156.01(13) 2 .
C3 Fe1 C5 157.88(9) . 2
C3 Fe1 C5 68.50(9) 2 2
C4 Fe1 C5 40.67(9) 2 2
C4 Fe1 C5 120.11(9) . 2
C3 Fe1 C5 68.49(9) . .
C3 Fe1 C5 157.88(9) 2 .
C4 Fe1 C5 120.11(9) 2 .
C4 Fe1 C5 40.67(9) . .
C5 Fe1 C5 103.66(12) 2 .
C3 Fe1 C1 124.13(8) . 2
C3 Fe1 C1 68.51(8) 2 2
C4 Fe1 C1 68.28(9) 2 2
C4 Fe1 C1 106.31(8) . 2
C5 Fe1 C1 40.45(8) 2 2
C5 Fe1 C1 119.70(9) . 2
C3 Fe1 C1 68.51(8) . .
C3 Fe1 C1 124.13(8) 2 .
C4 Fe1 C1 106.31(8) 2 .
C4 Fe1 C1 68.28(9) . .
C5 Fe1 C1 119.70(9) 2 .
C5 Fe1 C1 40.45(8) . .
C1 Fe1 C1 155.18(12) 2 .
C3 Fe1 C2 110.16(8) . 2
C3 Fe1 C2 41.06(8) 2 2
C4 Fe1 C2 68.84(8) 2 2
C4 Fe1 C2 123.29(8) . 2
C5 Fe1 C2 68.69(8) 2 2
C5 Fe1 C2 157.22(8) . 2
C1 Fe1 C2 40.83(8) 2 2
C1 Fe1 C2 161.96(8) . 2
C3 Fe1 C2 41.06(8) . .
C3 Fe1 C2 110.16(8) 2 .
C4 Fe1 C2 123.29(8) 2 .
C4 Fe1 C2 68.84(8) . .
C5 Fe1 C2 157.21(8) 2 .
C5 Fe1 C2 68.69(8) . .
C1 Fe1 C2 161.96(8) 2 .
C1 Fe1 C2 40.83(8) . .
C2 Fe1 C2 126.27(11) 2 .
N1 Ti1 N1 112.66(11) . 2
N1 Ti1 Cl1 109.58(6) . .
N1 Ti1 Cl1 107.82(6) 2 .
N1 Ti1 Cl1 107.83(6) . 2
N1 Ti1 Cl1 109.59(6) 2 2
Cl1 Ti1 Cl1 109.33(4) . 2
N1 P1 C2 111.07(9) . .
N1 P1 C10 109.14(9) . .
C2 P1 C10 110.74(9) . .
N1 P1 C6 109.91(9) . .
C2 P1 C6 103.25(9) . .
C10 P1 C6 112.65(9) . .
P1 N1 Ti1 164.72(11) . .
C5 C1 C2 108.52(19) . .
C5 C1 Fe1 69.46(12) . .
C2 C1 Fe1 69.67(11) . .
C3 C2 C1 106.61(17) . .
C3 C2 P1 120.31(15) . .
C1 C2 P1 132.48(15) . .
C3 C2 Fe1 68.51(11) . .
C1 C2 Fe1 69.50(11) . .
P1 C2 Fe1 133.24(10) . .
C4 C3 C2 108.66(18) . .
C4 C3 Fe1 69.94(11) . .
C2 C3 Fe1 70.43(11) . .
C3 C4 C5 108.06(18) . .
C3 C4 Fe1 69.35(11) . .
C5 C4 Fe1 69.94(12) . .
C1 C5 C4 108.14(19) . .
C1 C5 Fe1 70.09(12) . .
C4 C5 Fe1 69.40(12) . .
C7 C6 C8 108.42(17) . .
C7 C6 C9 110.69(17) . .
C8 C6 C9 107.76(17) . .
C7 C6 P1 112.31(14) . .
C8 C6 P1 107.37(13) . .
C9 C6 P1 110.13(14) . .
C11 C10 C13 108.96(17) . .
C11 C10 C12 110.16(17) . .
C13 C10 C12 106.94(17) . .
C11 C10 P1 113.90(14) . .
C13 C10 P1 107.95(13) . .
C12 C10 P1 108.69(14) . .
Cl22 C51 Cl11 113.60(16) . .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
Fe1 C3 2.0353(19) .
Fe1 C3 2.0354(19) 2
Fe1 C4 2.043(2) 2
Fe1 C4 2.043(2) .
Fe1 C5 2.050(2) 2
Fe1 C5 2.050(2) .
Fe1 C1 2.059(2) 2
Fe1 C1 2.059(2) .
Fe1 C2 2.0610(19) 2
Fe1 C2 2.0611(19) .
Ti1 N1 1.7888(16) .
Ti1 N1 1.7889(16) 2
Ti1 Cl1 2.3038(7) .
Ti1 Cl1 2.3038(7) 2
Cl11 C51 1.750(3) .
Cl22 C51 1.736(3) .
P1 N1 1.5881(17) .
P1 C2 1.807(2) .
P1 C10 1.867(2) .
P1 C6 1.8740(19) .
C1 C5 1.421(3) .
C1 C2 1.437(3) .
C2 C3 1.437(3) .
C3 C4 1.419(3) .
C4 C5 1.422(3) .
C6 C7 1.533(3) .
C6 C8 1.537(3) .
C6 C9 1.538(3) .
C10 C11 1.533(3) .
C10 C13 1.538(3) .
C10 C12 1.538(3) .
