#------------------------------------------------------------------------------
#$Date: 2022-09-14 17:31:13 +0300 (Wed, 14 Sep 2022) $
#$Revision: 277831 $
#$URL: file:///home/coder/svn-repositories/cod/cif/1/10/08/1100800.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_1100800
loop_
_publ_author_name
'Cano, Jesús'
'Sudupe, María'
'Royo, Pascual'
'Mosquera, Marta E. G.'
_publ_section_title
;
 Insertion Reactions into the Metal--Alkyl and Metal--Amido Bonds of
 1,3-Di(silyl-η-amido)cyclopentadienyl Titanium and Zirconium Complexes
;
_journal_issue                   10
_journal_name_full               Organometallics
_journal_page_first              2424
_journal_page_last               2432
_journal_paper_doi               10.1021/om048984e
_journal_volume                  24
_journal_year                    2005
_chemical_formula_moiety         'C36 H54 N4 Si2 Ti1'
_chemical_formula_sum            'C36 H54 N4 Si2 Ti'
_chemical_formula_weight         646.91
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_symmetry_cell_setting           triclinic
_symmetry_Int_Tables_number      2
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_cell_angle_alpha                98.372(6)
_cell_angle_beta                 102.866(10)
_cell_angle_gamma                99.863(7)
_cell_formula_units_Z            2
_cell_length_a                   9.7722(10)
_cell_length_b                   11.3369(4)
_cell_length_c                   17.0066(16)
_cell_measurement_reflns_used    120
_cell_measurement_temperature    200(2)
_cell_measurement_theta_max      21.149
_cell_measurement_theta_min      5.123
_cell_volume                     1776.2(3)
_diffrn_ambient_temperature      200(2)
_diffrn_detector                 'CCD plate'
_diffrn_measurement_device       '95mm CCD camera on κ-goniostat'
_diffrn_measurement_device_type  KappaCCD
_diffrn_measurement_method       'CCD rotation images, thick slices'
_diffrn_orient_matrix_type       X=UH
_diffrn_orient_matrix_UB_11      0.01
_diffrn_orient_matrix_UB_12      0
_diffrn_orient_matrix_UB_13      0
_diffrn_orient_matrix_UB_21      0
_diffrn_orient_matrix_UB_22      0.01
_diffrn_orient_matrix_UB_23      0
_diffrn_orient_matrix_UB_31      0
_diffrn_orient_matrix_UB_32      0
_diffrn_orient_matrix_UB_33      0.01
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0663
_diffrn_reflns_av_sigmaI/netI    0.0986
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_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            15135
_diffrn_reflns_theta_max         27.50
_diffrn_reflns_theta_min         3.04
_diffrn_source                   'Enraf Nonius FR590'
_exptl_absorpt_coefficient_mu    0.338
_exptl_absorpt_correction_T_max  1.242
_exptl_absorpt_correction_T_min  0.825
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
multi-scan from symmetry-related measurements
 Sortav (Blessing 1995)
;
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    1.210
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             696
_exptl_crystal_size_max          0.412
_exptl_crystal_size_mid          0.396
_exptl_crystal_size_min          0.194
_refine_ls_extinction_coef       ?
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.023
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     388
_refine_ls_number_reflns         8058
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.023
_refine_ls_R_factor_all          0.1097
_refine_ls_R_factor_gt           0.0614
_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)+(0.0706P)²+1.4230P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1466
_refine_ls_wR_factor_ref         0.1654
_reflns_number_gt                5192
_reflns_number_total             8058
_reflns_threshold_expression     >2sigma(I)
_cod_database_code               1100800
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_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
C10 C 0.2452(3) 0.2792(3) 0.1986(2) 0.0265(7) Uani 1 1 d . . .
H10A H 0.1793 0.2011 0.1928 0.040 Uiso 1 1 calc R . .
H10B H 0.2140 0.3167 0.1511 0.040 Uiso 1 1 calc R . .
H10C H 0.2452 0.3336 0.2490 0.040 Uiso 1 1 calc R . .
C6 C 0.6224(4) 0.6787(3) 0.3835(2) 0.0356(8) Uani 1 1 d . . .
H6A H 0.5913 0.7424 0.3550 0.053 Uiso 1 1 calc R . .
H6B H 0.7201 0.6739 0.3799 0.053 Uiso 1 1 calc R . .
H6C H 0.6211 0.6985 0.4413 0.053 Uiso 1 1 calc R . .
Ti1 Ti 0.59675(6) 0.23075(5) 0.30176(3) 0.01901(15) Uani 1 1 d . . .
Si1 Si 0.49779(10) 0.52856(8) 0.33424(6) 0.0236(2) Uani 1 1 d . . .
Si2 Si 0.81571(12) 0.16891(9) 0.42846(6) 0.0337(2) Uani 1 1 d . . .
N3 N 0.6500(3) 0.3256(2) 0.22320(15) 0.0171(5) Uani 1 1 d . . .
N1 N 0.4972(3) 0.4790(2) 0.23103(16) 0.0200(5) Uani 1 1 d . . .
N4 N 0.4210(3) 0.1426(2) 0.21100(16) 0.0222(6) Uani 1 1 d . . .
N2 N 0.7401(3) 0.1270(2) 0.32307(16) 0.0233(6) Uani 1 1 d . . .
C31 C 0.7562(3) 0.3754(3) 0.18271(19) 0.0185(6) Uani 1 1 d . . .
C36 C 0.7407(3) 0.3244(3) 0.0997(2) 0.0224(7) Uani 1 1 d . . .
C37 C 0.6184(4) 0.2214(3) 0.0530(2) 0.0273(7) Uani 1 1 d . . .
H37A H 0.6269 0.1990 -0.0034 0.041 Uiso 1 1 calc R . .
H37B H 0.5272 0.2470 0.0517 0.041 Uiso 1 1 calc R . .
H37C H 0.6212 0.1509 0.0800 0.041 Uiso 1 1 calc R . .
C11 C 0.4762(3) 0.5526(3) 0.1639(2) 0.0229(7) Uani 1 1 d . . .
C30 C 0.5130(3) 0.3544(3) 0.21154(18) 0.0184(6) Uani 1 1 d . . .
C32 C 0.8778(3) 0.4677(3) 0.2246(2) 0.0234(7) Uani 1 1 d . . .
C41 C 0.3067(3) 0.0371(3) 0.1773(2) 0.0249(7) Uani 1 1 d . . .
C22 C 0.7935(4) 0.0448(3) 0.2651(2) 0.0260(7) Uani 1 1 d . . .
C5 C 0.6969(4) 0.3870(3) 0.41899(19) 0.0279(7) Uani 1 1 d . . .
H5 H 0.7825 0.4433 0.4215 0.034 Uiso 1 1 calc R . .
C13 C 0.3992(4) 0.4693(3) 0.0806(2) 0.0336(8) Uani 1 1 d . . .
H13A H 0.3080 0.4218 0.0845 0.050 Uiso 1 1 calc R . .
H13B H 0.4599 0.4137 0.0658 0.050 Uiso 1 1 calc R . .
H13C H 0.3806 0.5191 0.0385 0.050 Uiso 1 1 calc R . .
C2 C 0.4616(4) 0.3005(3) 0.3997(2) 0.0309(8) Uani 1 1 d . . .
H2 H 0.3597 0.2864 0.3856 0.037 Uiso 1 1 calc R . .
C33 C 0.9768(3) 0.5090(3) 0.1818(2) 0.0299(8) Uani 1 1 d . . .
H33 H 1.0574 0.5723 0.2097 0.036 Uiso 1 1 calc R . .
C25 C 0.6681(4) -0.0236(3) 0.1928(2) 0.0391(9) Uani 1 1 d . . .
H25A H 0.5950 -0.0714 0.2134 0.059 Uiso 1 1 calc R . .
H25B H 0.7028 -0.0783 0.1553 0.059 Uiso 1 1 calc R . .
H25C H 0.6260 0.0352 0.1635 0.059 Uiso 1 1 calc R . .
C35 C 0.8438(4) 0.3693(3) 0.0596(2) 0.0289(7) Uani 1 1 d . . .
H35 H 0.8324 0.3360 0.0034 0.035 Uiso 1 1 calc R . .
C43 C 0.1562(4) -0.1463(3) 0.1933(3) 0.0400(10) Uani 1 1 d . . .
H43 H 0.1316 -0.2020 0.2271 0.048 Uiso 1 1 calc R . .
C7 C 0.3205(4) 0.5450(3) 0.3556(2) 0.0350(8) Uani 1 1 d . . .
H7A H 0.2492 0.4691 0.3311 0.053 Uiso 1 1 calc R . .
H7B H 0.2883 0.6123 0.3318 0.053 Uiso 1 1 calc R . .
H7C H 0.3316 0.5621 0.4151 0.053 Uiso 1 1 calc R . .
C1 C 0.5555(4) 0.4047(3) 0.3880(2) 0.0261(7) Uani 1 1 d . . .
C4 C 0.6922(4) 0.2726(3) 0.4459(2) 0.0309(8) Uani 1 1 d . . .
C34 C 0.9612(4) 0.4607(3) 0.1003(2) 0.0332(8) Uani 1 1 d . . .
H34 H 1.0305 0.4901 0.0725 0.040 Uiso 1 1 calc R . .
C46 C 0.2307(4) 0.0150(3) 0.0938(2) 0.0303(8) Uani 1 1 d . . .
C3 C 0.5436(4) 0.2232(3) 0.4349(2) 0.0316(8) Uani 1 1 d . . .
H3 H 0.5059 0.1488 0.4494 0.038 Uiso 1 1 calc R . .
C42 C 0.2716(4) -0.0475(3) 0.2267(2) 0.0336(8) Uani 1 1 d . . .
C14 C 0.3807(4) 0.6419(3) 0.1829(2) 0.0336(8) Uani 1 1 d . . .
H14A H 0.2889 0.5961 0.1871 0.050 Uiso 1 1 calc R . .
H14B H 0.3635 0.6882 0.1386 0.050 Uiso 1 1 calc R . .
H14C H 0.4289 0.6982 0.2349 0.050 Uiso 1 1 calc R . .
C12 C 0.6189(4) 0.6260(3) 0.1577(2) 0.0327(8) Uani 1 1 d . . .
H12A H 0.6685 0.6792 0.2108 0.049 Uiso 1 1 calc R . .
H12B H 0.6005 0.6758 0.1155 0.049 Uiso 1 1 calc R . .
H12C H 0.6790 0.5700 0.1428 0.049 Uiso 1 1 calc R . .
C47 C 0.2707(4) 0.0898(3) 0.0320(2) 0.0383(9) Uani 1 1 d . . .
H47A H 0.3510 0.1580 0.0601 0.057 Uiso 1 1 calc R . .
H47B H 0.1879 0.1213 0.0064 0.057 Uiso 1 1 calc R . .
H47C H 0.2990 0.0381 -0.0104 0.057 Uiso 1 1 calc R . .
C48 C 0.3511(5) -0.0343(4) 0.3149(3) 0.0460(10) Uani 1 1 d . . .
H48A H 0.4287 0.0385 0.3303 0.069 Uiso 1 1 calc R . .
H48B H 0.3917 -0.1065 0.3221 0.069 Uiso 1 1 calc R . .
H48C H 0.2848 -0.0265 0.3500 0.069 Uiso 1 1 calc R . .
C9 C 0.7926(6) 0.0453(4) 0.4897(3) 0.0568(12) Uani 1 1 d . . .
H9A H 0.8572 -0.0097 0.4810 0.085 Uiso 1 1 calc R . .
H9B H 0.6930 -0.0008 0.4720 0.085 Uiso 1 1 calc R . .
H9C H 0.8154 0.0819 0.5482 0.085 Uiso 1 1 calc R . .
C45 C 0.1167(4) -0.0866(3) 0.0634(3) 0.0417(10) Uani 1 1 d . . .
H45 H 0.0652 -0.1018 0.0073 0.050 Uiso 1 1 calc R . .
C23 C 0.8607(4) -0.0493(3) 0.3078(3) 0.0392(9) Uani 1 1 d . . .
H23A H 0.7889 -0.0986 0.3284 0.059 Uiso 1 1 calc R . .
H23B H 0.9423 -0.0070 0.3538 0.059 Uiso 1 1 calc R . .
H23C H 0.8939 -0.1024 0.2685 0.059 Uiso 1 1 calc R . .
C38 C 0.9023(4) 0.5273(4) 0.3128(2) 0.0439(10) Uani 1 1 d . . .
H38A H 0.8250 0.4895 0.3350 0.066 Uiso 1 1 calc R . .
H38B H 0.9032 0.6145 0.3163 0.066 Uiso 1 1 calc R . .
H38C H 0.9947 0.5168 0.3446 0.066 Uiso 1 1 calc R . .
C44 C 0.0775(4) -0.1656(3) 0.1138(3) 0.0471(11) Uani 1 1 d . . .
H44 H -0.0029 -0.2318 0.0931 0.057 Uiso 1 1 calc R . .
C8 C 1.0076(5) 0.2521(4) 0.4596(3) 0.0576(12) Uani 1 1 d . . .
H8A H 1.0692 0.1948 0.4497 0.086 Uiso 1 1 calc R . .
H8B H 1.0338 0.2891 0.5181 0.086 Uiso 1 1 calc R . .
H8C H 1.0205 0.3161 0.4273 0.086 Uiso 1 1 calc R . .
C24 C 0.9079(4) 0.1204(3) 0.2331(3) 0.0427(10) Uani 1 1 d . . .
H24A H 0.8667 0.1812 0.2057 0.064 Uiso 1 1 calc R . .
H24B H 0.9404 0.0664 0.1940 0.064 Uiso 1 1 calc R . .
H24C H 0.9896 0.1618 0.2793 0.064 Uiso 1 1 calc R . .
C40 C 0.3949(3) 0.2582(3) 0.20313(19) 0.0213(6) Uani 1 1 d . . .
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'
Ti Ti 0.2776 0.4457 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
