#------------------------------------------------------------------------------
#$Date: 2016-03-21 09:08:49 +0200 (Mon, 21 Mar 2016) $
#$Revision: 178618 $
#$URL: svn://www.crystallography.net/cod/cif/4/07/29/4072992.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_4072992
loop_
_publ_author_name
'Hanna, Tamara E.'
'Bernskoetter, Wesley H.'
'Bouwkamp, Marco W.'
'Lobkovsky, Emil'
'Chirik, Paul J.'
_publ_section_title
;
 Bis(cyclopentadienyl) Titanium Dinitrogen Chemistry:  Synthesis
 and Characterization of a Side-on Bound Haptomer
;
_journal_issue                   9
_journal_name_full               Organometallics
_journal_page_first              2431
_journal_paper_doi               10.1021/om0611913
_journal_volume                  26
_journal_year                    2007
_chemical_formula_moiety         'C52 H92 N2 Si6 Ti2'
_chemical_formula_sum            'C52 H92 N2 Si6 Ti2'
_chemical_formula_weight         1009.62
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           13
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2yac'
_symmetry_space_group_name_H-M   'P 1 2/n 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                 103.955(2)
_cell_angle_gamma                90.00
_cell_formula_units_Z            2
_cell_length_a                   16.9449(9)
_cell_length_b                   10.5645(4)
_cell_length_c                   18.0529(10)
_cell_measurement_reflns_used    2513
_cell_measurement_temperature    173(2)
_cell_measurement_theta_max      21.01
_cell_measurement_theta_min      2.32
_cell_volume                     3136.3(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, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      173(2)
_diffrn_measured_fraction_theta_full 0.951
_diffrn_measured_fraction_theta_max 0.951
_diffrn_measurement_device_type  'Bruker X8 APEX II diffractometer'
_diffrn_measurement_method       'phi and omega 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  0.0659
_diffrn_reflns_av_sigmaI/netI    0.0677
_diffrn_reflns_limit_h_max       19
_diffrn_reflns_limit_h_min       -19
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -10
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            28280
_diffrn_reflns_theta_full        24.71
_diffrn_reflns_theta_max         24.71
_diffrn_reflns_theta_min         1.48
_exptl_absorpt_coefficient_mu    0.400
_exptl_absorpt_correction_T_max  0.9424
_exptl_absorpt_correction_T_min  0.9066
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   SADABS
_exptl_crystal_colour            blue
_exptl_crystal_density_diffrn    1.069
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             1092
_exptl_crystal_size_max          0.25
_exptl_crystal_size_mid          0.20
_exptl_crystal_size_min          0.15
_platon_squeeze_details          ' ?'
_refine_diff_density_max         0.254
_refine_diff_density_min         -0.209
_refine_diff_density_rms         0.052
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.910
_refine_ls_hydrogen_treatment    riding
_refine_ls_matrix_type           full
_refine_ls_number_parameters     294
_refine_ls_number_reflns         5102
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.910
_refine_ls_R_factor_all          0.0600
_refine_ls_R_factor_gt           0.0363
_refine_ls_shift/su_max          0.031
_refine_ls_shift/su_mean         0.001
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[σ²(Fo²)+(0.0440P)²+0.0000P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0802
_refine_ls_wR_factor_ref         0.0841
_reflns_number_gt                3259
_reflns_number_total             5102
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            om0611913si20061230_110032.cif
_cod_data_source_block           th30
_cod_depositor_comments
;
The following automatic conversions were performed:

'_symmetry_cell_setting' value 'Monoclinic' changed to 'monoclinic'
according to /home/saulius/struct/CIF-dictionaries/cif_core.dic
dictionary named 'cif_core.dic' version 2.4.1 from 2010-06-29.

Automatic conversion script
Id: cif_fix_values 1715 2011-07-08 13:25:40Z adriana 
;
_cod_original_sg_symbol_H-M      P2/n
_cod_database_code               4072992
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x+1/2, y, -z+1/2'
'-x, -y, -z'
'x-1/2, -y, 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
Ti1 Ti 0.87594(2) 0.14632(3) 0.191802(18) 0.01824(9) Uani 1 1 d .
Si1 Si 0.83135(4) 0.33889(5) 0.00210(3) 0.02553(15) Uani 1 1 d .
Si2 Si 1.05891(3) -0.04858(5) 0.31435(3) 0.02537(15) Uani 1 1 d .
Si3 Si 1.02770(3) 0.14931(5) 0.11915(3) 0.02281(14) Uani 1 1 d .
N1 N 0.77851(8) 0.15025(12) 0.23690(8) 0.0189(4) Uani 1 1 d .
C1 C 0.91838(11) 0.10853(17) 0.08051(10) 0.0205(5) Uani 1 1 d .
C2 C 0.89173(11) -0.00974(16) 0.10413(10) 0.0195(5) Uani 1 1 d .
H2A H 0.9269 -0.0864 0.1174 0.023 Uiso 1 1 calc R
C3 C 0.80689(11) -0.00842(16) 0.09630(10) 0.0184(5) Uani 1 1 d .
C4 C 0.78093(11) 0.11399(16) 0.07041(10) 0.0201(5) Uani 1 1 d .
H4A H 0.7230 0.1428 0.0580 0.024 Uiso 1 1 calc R
C5 C 0.84745(11) 0.18858(16) 0.05938(10) 0.0201(5) Uani 1 1 d .
C6 C 1.01537(11) 0.18422(16) 0.21702(10) 0.0205(5) Uani 1 1 d .
C7 C 1.00225(11) 0.09943(17) 0.27588(10) 0.0209(5) Uani 1 1 d .
C8 C 0.95850(11) 0.17042(16) 0.31986(10) 0.0204(5) Uani 1 1 d .
H8A H 0.9433 0.1379 0.3665 0.024 Uiso 1 1 calc R
C9 C 0.94430(11) 0.29543(17) 0.29204(10) 0.0213(5) Uani 1 1 d .
C10 C 0.97726(11) 0.30120(17) 0.22713(10) 0.0225(5) Uani 1 1 d .
H10A H 0.9806 0.3799 0.1973 0.027 Uiso 1 1 calc R
C11 C 0.72158(12) 0.34898(18) -0.04836(11) 0.0356(6) Uani 1 1 d .
H11A H 0.6883 0.3482 -0.0108 0.053 Uiso 1 1 calc R
H11B H 0.7071 0.2764 -0.0828 0.053 Uiso 1 1 calc R
H11C H 0.7117 0.4276 -0.0780 0.053 Uiso 1 1 calc R
C12 C 0.85812(13) 0.48661(17) 0.05843(11) 0.0361(6) Uani 1 1 d .
H12A H 0.9168 0.4885 0.0809 0.054 Uiso 1 1 calc R
H12B H 0.8290 0.4892 0.0992 0.054 Uiso 1 1 calc R
H12C H 0.8426 0.5600 0.0249 0.054 Uiso 1 1 calc R
C13 C 0.88894(13) 0.33160(18) -0.07410(11) 0.0383(6) Uani 1 1 d .
H13A H 0.8870 0.4144 -0.0989 0.057 Uiso 1 1 calc R
H13B H 0.8644 0.2678 -0.1121 0.057 Uiso 1 1 calc R
H13C H 0.9457 0.3088 -0.0513 0.057 Uiso 1 1 calc R
C14 C 1.05000(12) -0.06970(19) 0.41471(11) 0.0356(6) Uani 1 1 d .
H14A H 1.0672 0.0081 0.4436 0.053 Uiso 1 1 calc R
H14B H 1.0848 -0.1400 0.4384 0.053 Uiso 1 1 calc R
H14C H 0.9934 -0.0883 0.4148 0.053 Uiso 1 1 calc R
C15 C 1.16884(12) -0.02272(19) 0.31684(12) 0.0366(6) Uani 1 1 d .
H15A H 1.1760 -0.0210 0.2646 0.055 Uiso 1 1 calc R
H15B H 1.2013 -0.0917 0.3452 0.055 Uiso 1 1 calc R
H15C H 1.1868 0.0581 0.3420 0.055 Uiso 1 1 calc R
C16 C 1.02438(13) -0.19957(17) 0.26357(12) 0.0370(6) Uani 1 1 d .
H16A H 0.9671 -0.2143 0.2631 0.056 Uiso 1 1 calc R
H16B H 1.0575 -0.2697 0.2899 0.056 Uiso 1 1 calc R
H16C H 1.0304 -0.1942 0.2110 0.056 Uiso 1 1 calc R
C17 C 0.75453(11) -0.12340(16) 0.10141(10) 0.0213(5) Uani 1 1 d .
C18 C 0.79988(12) -0.21924(17) 0.15981(11) 0.0285(6) Uani 1 1 d .
H18A H 0.8156 -0.1792 0.2102 0.043 Uiso 1 1 calc R
H18B H 0.8487 -0.2483 0.1447 0.043 Uiso 1 1 calc R
H18C H 0.7644 -0.2917 0.1619 0.043 Uiso 1 1 calc R
C19 C 0.73424(12) -0.18475(17) 0.02186(11) 0.0319(6) Uani 1 1 d .
H19A H 0.7010 -0.2605 0.0225 0.048 Uiso 1 1 calc R
H19B H 0.7847 -0.2085 0.0081 0.048 Uiso 1 1 calc R
H19C H 0.7041 -0.1244 -0.0157 0.048 Uiso 1 1 calc R
C20 C 0.67543(11) -0.08574(18) 0.12188(11) 0.0290(6) Uani 1 1 d .
H20A H 0.6411 -0.1608 0.1204 0.043 Uiso 1 1 calc R
H20B H 0.6467 -0.0231 0.0851 0.043 Uiso 1 1 calc R
H20C H 0.6877 -0.0492 0.1733 0.043 Uiso 1 1 calc R
C21 C 0.91615(12) 0.40830(17) 0.33082(11) 0.0258(5) Uani 1 1 d .
C22 C 0.86081(14) 0.36856(19) 0.38141(12) 0.0426(6) Uani 1 1 d .
H22A H 0.8110 0.3311 0.3499 0.064 Uiso 1 1 calc R
H22B H 0.8469 0.4428 0.4082 0.064 Uiso 1 1 calc R
H22C H 0.8888 0.3061 0.4188 0.064 Uiso 1 1 calc R
C23 C 0.87170(13) 0.50427(18) 0.27269(12) 0.0396(6) Uani 1 1 d .
H23A H 0.9074 0.5317 0.2404 0.059 Uiso 1 1 calc R
H23B H 0.8564 0.5776 0.2994 0.059 Uiso 1 1 calc R
H23C H 0.8227 0.4653 0.2408 0.059 Uiso 1 1 calc R
C24 C 0.99281(13) 0.4705(2) 0.37986(12) 0.0460(7) Uani 1 1 d .
H24A H 1.0213 0.4101 0.4183 0.069 Uiso 1 1 calc R
H24B H 0.9775 0.5453 0.4054 0.069 Uiso 1 1 calc R
H24C H 1.0287 0.4960 0.3473 0.069 Uiso 1 1 calc R
C25 C 1.06500(12) 0.29101(18) 0.07681(12) 0.0341(6) Uani 1 1 d .
H25A H 1.0266 0.3610 0.0748 0.051 Uiso 1 1 calc R
H25B H 1.0697 0.2711 0.0250 0.051 Uiso 1 1 calc R
H25C H 1.1184 0.3156 0.1083 0.051 Uiso 1 1 calc R
C26 C 1.09452(12) 0.01422(18) 0.11086(11) 0.0328(6) Uani 1 1 d .
H26A H 1.1512 0.0369 0.1339 0.049 Uiso 1 1 calc R
H26B H 1.0884 -0.0065 0.0569 0.049 Uiso 1 1 calc R
H26C H 1.0793 -0.0593 0.1375 0.049 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'
Ti Ti 0.2776 0.4457 '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
N1 Ti1 C1 143.98(6) .
N1 Ti1 C6 144.15(6) .
C1 Ti1 C6 71.83(6) .
N1 Ti1 C2 121.77(6) .
C1 Ti1 C2 35.61(6) .
C6 Ti1 C2 88.70(6) .
N1 Ti1 C10 119.63(6) .
C1 Ti1 C10 89.77(6) .
C6 Ti1 C10 35.52(6) .
C2 Ti1 C10 118.60(7) .
N1 Ti1 C7 116.76(6) .
C1 Ti1 C7 95.63(6) .
C6 Ti1 C7 35.95(6) .
C2 Ti1 C7 93.04(6) .
C10 Ti1 C7 58.70(6) .
N1 Ti1 C5 114.73(6) .
C1 Ti1 C5 35.84(6) .
C6 Ti1 C5 96.62(6) .
C2 Ti1 C5 58.61(6) .
C10 Ti1 C5 95.78(6) .
C7 Ti1 C5 128.51(7) .
N1 Ti1 C4 86.41(6) .
C1 Ti1 C4 57.87(6) .
C6 Ti1 C4 128.71(7) .
C2 Ti1 C4 56.40(6) .
C10 Ti1 C4 129.09(6) .
C7 Ti1 C4 149.18(6) .
C5 Ti1 C4 34.79(6) .
N1 Ti1 C8 87.29(6) .
C1 Ti1 C8 128.16(6) .
C6 Ti1 C8 57.84(6) .
C2 Ti1 C8 125.97(6) .
C10 Ti1 C8 56.50(6) .
C7 Ti1 C8 34.72(6) .
C5 Ti1 C8 151.62(6) .
C4 Ti1 C8 173.32(6) .
N1 Ti1 C3 89.96(6) .
C1 Ti1 C3 58.26(6) .
C6 Ti1 C3 122.68(6) .
C2 Ti1 C3 34.05(6) .
C10 Ti1 C3 147.99(7) .
C7 Ti1 C3 121.08(6) .
C5 Ti1 C3 57.98(6) .
C4 Ti1 C3 33.63(5) .
C8 Ti1 C3 144.22(6) .
N1 Ti1 C9 88.62(6) .
C1 Ti1 C9 123.70(6) .
C6 Ti1 C9 58.16(6) .
C2 Ti1 C9 146.53(6) .
C10 Ti1 C9 34.10(6) .
C7 Ti1 C9 57.96(6) .
C5 Ti1 C9 124.49(6) .
C4 Ti1 C9 148.20(6) .
C8 Ti1 C9 33.65(6) .
C3 Ti1 C9 177.52(6) .
C12 Si1 C11 107.59(9) .
C12 Si1 C13 109.59(9) .
C11 Si1 C13 106.18(9) .
C12 Si1 C5 115.14(8) .
C11 Si1 C5 108.20(9) .
C13 Si1 C5 109.74(9) .
C16 Si2 C14 106.62(10) .
C16 Si2 C7 117.33(8) .
C14 Si2 C7 107.73(9) .
C16 Si2 C15 109.23(10) .
C14 Si2 C15 107.87(9) .
C7 Si2 C15 107.71(9) .
C26 Si3 C25 108.21(9) .
C26 Si3 C6 116.08(9) .
C25 Si3 C6 110.92(9) .
C26 Si3 C1 111.31(9) .
C25 Si3 C1 115.95(9) .
C6 Si3 C1 94.12(8) .
N1 N1 Ti1 178.81(5) 2_655
C2 C1 C5 106.76(16) .
C2 C1 Si3 116.57(13) .
C5 C1 Si3 130.68(13) .
C2 C1 Ti1 72.92(10) .
C5 C1 Ti1 73.53(10) .
Si3 C1 Ti1 97.09(7) .
C3 C2 C1 110.45(15) .
C3 C2 Ti1 77.36(10) .
C1 C2 Ti1 71.47(10) .
C4 C3 C2 105.76(16) .
C4 C3 C17 127.84(16) .
C2 C3 C17 125.58(15) .
C4 C3 Ti1 71.34(9) .
C2 C3 Ti1 68.59(10) .
C17 C3 Ti1 132.45(12) .
C3 C4 C5 111.03(16) .
C3 C4 Ti1 75.03(10) .
C5 C4 Ti1 70.85(10) .
C4 C5 C1 105.95(15) .
C4 C5 Si1 121.90(13) .
C1 C5 Si1 129.92(14) .
C4 C5 Ti1 74.36(10) .
C1 C5 Ti1 70.63(10) .
Si1 C5 Ti1 133.10(9) .
C10 C6 C7 106.73(16) .
C10 C6 Si3 116.75(13) .
C7 C6 Si3 130.18(13) .
C10 C6 Ti1 72.83(10) .
C7 C6 Ti1 73.09(10) .
Si3 C6 Ti1 96.94(7) .
C8 C7 C6 106.04(15) .
C8 C7 Si2 121.39(14) .
C6 C7 Si2 129.16(14) .
C8 C7 Ti1 74.60(10) .
C6 C7 Ti1 70.96(10) .
Si2 C7 Ti1 135.76(9) .
C9 C8 C7 111.18(17) .
C9 C8 Ti1 75.41(10) .
C7 C8 Ti1 70.68(10) .
C10 C9 C8 105.49(16) .
C10 C9 C21 125.38(16) .
C8 C9 C21 128.06(17) .
C10 C9 Ti1 68.26(10) .
C8 C9 Ti1 70.94(10) .
C21 C9 Ti1 134.12(12) .
C9 C10 C6 110.47(16) .
C9 C10 Ti1 77.65(11) .
C6 C10 Ti1 71.65(10) .
C3 C17 C18 111.56(15) .
C3 C17 C20 111.46(15) .
C18 C17 C20 109.30(16) .
C3 C17 C19 106.41(15) .
C18 C17 C19 109.09(15) .
C20 C17 C19 108.93(15) .
C22 C21 C9 111.66(15) .
C22 C21 C23 108.94(17) .
C9 C21 C23 111.35(15) .
C22 C21 C24 109.37(17) .
C9 C21 C24 106.66(16) .
C23 C21 C24 108.79(16) .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
Ti1 N1 2.0096(14) .
Ti1 C1 2.3259(19) .
Ti1 C6 2.3305(18) .
Ti1 C2 2.3450(18) .
Ti1 C10 2.3459(18) .
Ti1 C7 2.3587(18) .
Ti1 C5 2.3644(17) .
Ti1 C4 2.4104(17) .
Ti1 C8 2.4097(17) .
Ti1 C3 2.4578(17) .
Ti1 C9 2.4672(18) .
Si1 C12 1.8582(19) .
Si1 C11 1.866(2) .
Si1 C13 1.870(2) .
Si1 C5 1.8786(18) .
Si2 C16 1.862(2) .
Si2 C14 1.867(2) .
Si2 C7 1.8781(18) .
Si2 C15 1.873(2) .
Si3 C26 1.8501(19) .
Si3 C25 1.8595(19) .
Si3 C6 1.8653(19) .
Si3 C1 1.8656(19) .
N1 N1 1.174(3) 2_655
C1 C2 1.428(2) .
C1 C5 1.444(2) .
C2 C3 1.410(3) .
C3 C4 1.409(2) .
C3 C17 1.520(2) .
C4 C5 1.428(3) .
C6 C10 1.426(2) .
C6 C7 1.447(3) .
C7 C8 1.424(3) .
C8 C9 1.413(2) .
C9 C10 1.416(3) .
C9 C21 1.517(3) .
C17 C18 1.528(2) .
C17 C20 1.527(3) .
C17 C19 1.537(3) .
C21 C22 1.517(3) .
C21 C23 1.522(3) .
C21 C24 1.533(3) .
loop_
_platon_squeeze_void_nr
_platon_squeeze_void_average_x
_platon_squeeze_void_average_y
_platon_squeeze_void_average_z
_platon_squeeze_void_volume
_platon_squeeze_void_count_electrons
1 0.250 0.438 0.250 167.8 40.1
2 0.750 0.562 0.750 167.8 40.2
