#------------------------------------------------------------------------------
#$Date: 2016-02-13 14:50:18 +0200 (Sat, 13 Feb 2016) $
#$Revision: 176428 $
#$URL: svn://www.crystallography.net/cod/cif/1/10/07/1100799.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_1100799
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_sum            'C33 H49 N3 Si2 Zr'
_chemical_formula_weight         635.15
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_cell_angle_alpha                90.00
_cell_angle_beta                 106.355(11)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   11.119(2)
_cell_length_b                   19.430(4)
_cell_length_c                   15.805(2)
_cell_measurement_reflns_used    40
_cell_measurement_temperature    200(2)
_cell_measurement_theta_max      17.209
_cell_measurement_theta_min      3.96
_cell_volume                     3276.4(10)
_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  0.1751
_diffrn_reflns_av_sigmaI/netI    0.1321
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       25
_diffrn_reflns_limit_k_min       -25
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            27467
_diffrn_reflns_theta_max         27.53
_diffrn_reflns_theta_min         3.01
_diffrn_source                   'Enraf Nonius FR590'
_exptl_absorpt_coefficient_mu    0.434
_exptl_absorpt_correction_T_max  0.954
_exptl_absorpt_correction_T_min  0.794
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
 R.H. Blessing, Acta Cryst. (1995), A51, 33-38
;
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.288
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             1344
_exptl_crystal_size_max          0.561
_exptl_crystal_size_mid          0.443
_exptl_crystal_size_min          0.108
_refine_ls_extinction_coef       ?
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.020
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     350
_refine_ls_number_reflns         7529
_refine_ls_number_restraints     3
_refine_ls_restrained_S_all      1.021
_refine_ls_R_factor_all          0.1359
_refine_ls_R_factor_gt           0.0636
_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)+(0.0414P)²+5.5411P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1210
_refine_ls_wR_factor_ref         0.1446
_reflns_number_gt                4388
_reflns_number_total             7529
_reflns_threshold_expression     >2sigma(I)
_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_enum 1527 2010-12-29 10:47:43Z saulius 
;
_cod_original_sg_symbol_H-M      P21/c
_cod_database_code               1100799
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, y+1/2, -z+1/2'
'-x, -y, -z'
'x, -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
_atom_site_disorder_assembly
_atom_site_disorder_group
Zr1 Zr 0.16570(4) 0.11245(2) 0.23597(3) 0.01799(12) Uani 1 1 d . . .
C1 C 0.2279(5) 0.0594(2) 0.1091(3) 0.0248(11) Uani 1 1 d . . .
C2 C 0.1012(5) 0.0810(3) 0.0764(3) 0.0279(11) Uani 1 1 d . . .
H2 H 0.0328 0.0519 0.0556 0.034 Uiso 1 1 calc R . .
C3 C 0.0951(5) 0.1535(3) 0.0803(3) 0.0240(10) Uani 1 1 d . . .
H3 H 0.0223 0.1797 0.0622 0.029 Uiso 1 1 calc R . .
C4 C 0.2186(5) 0.1803(2) 0.1164(3) 0.0230(10) Uani 1 1 d . . .
C5 C 0.2979(5) 0.1214(3) 0.1314(3) 0.0253(11) Uani 1 1 d . . .
H5 H 0.3847 0.1232 0.1532 0.030 Uiso 1 1 calc R . .
Si1 Si 0.28551(13) -0.01848(7) 0.17817(9) 0.0267(3) Uani 1 1 d . . .
N1 N 0.2559(4) 0.0136(2) 0.2723(2) 0.0240(9) Uani 1 1 d . . .
C11 C 0.1969(6) -0.0980(3) 0.1282(4) 0.0401(14) Uani 1 1 d . . .
H11A H 0.2289 -0.1370 0.1649 0.060 Uiso 1 1 calc R . .
H11B H 0.2070 -0.1054 0.0705 0.060 Uiso 1 1 calc R . .
H11C H 0.1096 -0.0922 0.1237 0.060 Uiso 1 1 calc R . .
C12 C 0.4537(5) -0.0323(3) 0.1829(4) 0.0422(15) Uani 1 1 d . . .
H12A H 0.4848 -0.0723 0.2180 0.063 Uiso 1 1 calc R . .
H12B H 0.5019 0.0072 0.2088 0.063 Uiso 1 1 calc R . .
H12C H 0.4607 -0.0391 0.1243 0.063 Uiso 1 1 calc R . .
C13 C 0.2745(5) -0.0289(3) 0.3543(3) 0.0296(12) Uani 1 1 d . . .
C14 C 0.1581(5) -0.0720(3) 0.3497(4) 0.0383(13) Uani 1 1 d . . .
H14A H 0.1409 -0.1014 0.2989 0.057 Uiso 1 1 calc R . .
H14B H 0.0879 -0.0421 0.3453 0.057 Uiso 1 1 calc R . .
H14C H 0.1723 -0.0995 0.4020 0.057 Uiso 1 1 calc R . .
C15 C 0.3029(6) 0.0182(3) 0.4354(3) 0.0407(14) Uani 1 1 d . . .
H15A H 0.3761 0.0452 0.4379 0.061 Uiso 1 1 calc R . .
H15B H 0.3176 -0.0093 0.4878 0.061 Uiso 1 1 calc R . .
H15C H 0.2329 0.0482 0.4314 0.061 Uiso 1 1 calc R . .
C16 C 0.3861(5) -0.0785(3) 0.3674(4) 0.0422(14) Uani 1 1 d . . .
H16A H 0.4609 -0.0527 0.3706 0.063 Uiso 1 1 calc R . .
H16B H 0.3704 -0.1099 0.3186 0.063 Uiso 1 1 calc R . .
H16C H 0.3966 -0.1039 0.4211 0.063 Uiso 1 1 calc R . .
Si2 Si 0.26229(13) 0.25520(7) 0.19222(9) 0.0240(3) Uani 1 1 d . . .
N2 N 0.2358(4) 0.2134(2) 0.2827(2) 0.0224(9) Uani 1 1 d . . .
C21 C 0.1616(5) 0.3317(3) 0.1502(3) 0.0369(13) Uani 1 1 d . . .
H21A H 0.1868 0.3692 0.1909 0.055 Uiso 1 1 calc R . .
H21B H 0.0756 0.3203 0.1443 0.055 Uiso 1 1 calc R . .
H21C H 0.1707 0.3448 0.0937 0.055 Uiso 1 1 calc R . .
C22 C 0.4266(5) 0.2800(3) 0.2007(4) 0.0393(14) Uani 1 1 d . . .
H22A H 0.4502 0.3186 0.2397 0.059 Uiso 1 1 calc R . .
H22B H 0.4334 0.2922 0.1433 0.059 Uiso 1 1 calc R . .
H22C H 0.4813 0.2419 0.2233 0.059 Uiso 1 1 calc R . .
C23 C 0.2395(5) 0.2498(2) 0.3666(3) 0.0250(11) Uani 1 1 d . . .
C24 C 0.1099(5) 0.2803(3) 0.3601(4) 0.0348(13) Uani 1 1 d . . .
H24A H 0.0869 0.3118 0.3114 0.052 Uiso 1 1 calc R . .
H24B H 0.1126 0.3043 0.4137 0.052 Uiso 1 1 calc R . .
H24C H 0.0492 0.2439 0.3511 0.052 Uiso 1 1 calc R . .
C25 C 0.3357(5) 0.3094(3) 0.3856(4) 0.0371(13) Uani 1 1 d . . .
H25A H 0.3147 0.3416 0.3376 0.056 Uiso 1 1 calc R . .
H25B H 0.4181 0.2914 0.3919 0.056 Uiso 1 1 calc R . .
H25C H 0.3339 0.3323 0.4391 0.056 Uiso 1 1 calc R . .
C26 C 0.2767(6) 0.2002(3) 0.4437(3) 0.0422(15) Uani 1 1 d . . .
H26A H 0.3579 0.1814 0.4477 0.063 Uiso 1 1 calc R . .
H26B H 0.2164 0.1636 0.4349 0.063 Uiso 1 1 calc R . .
H26C H 0.2792 0.2242 0.4972 0.063 Uiso 1 1 calc R . .
N3 N -0.0325(3) 0.1080(2) 0.2283(2) 0.0220(8) Uani 1 1 d . . .
C30 C 0.0205(5) 0.0982(2) 0.3108(3) 0.0268(11) Uani 1 1 d . . .
C31 C -0.0474(6) 0.0769(4) 0.3775(4) 0.061(2) Uani 1 1 d . . .
H31A H -0.0707 0.0289 0.3665 0.073 Uiso 1 1 calc R . .
H31B H 0.0125 0.0792 0.4354 0.073 Uiso 1 1 calc R . .
C32 C -0.1616(4) 0.1151(3) 0.3818(3) 0.0284(11) Uani 1 1 d D B .
C33 C -0.1512(9) 0.1766(4) 0.4271(5) 0.073(3) Uani 1 1 d D . .
H33 H -0.0689 0.1923 0.4459 0.088 Uiso 1 1 calc R A 1
C34 C -0.2224(15) 0.2144(7) 0.4479(9) 0.047(4) Uiso 0.511(18) 1 d PD B 1
H34 H -0.1978 0.2521 0.4850 0.057 Uiso 0.511(18) 1 calc PR B 1
C35 C -0.3460(19) 0.1957(10) 0.4106(11) 0.056(5) Uiso 0.511(18) 1 d PD B 1
H35 H -0.4083 0.2242 0.4196 0.068 Uiso 0.511(18) 1 calc PR B 1
C36 C -0.3816(15) 0.1376(11) 0.3613(10) 0.052(4) Uiso 0.511(18) 1 d PD B 1
H36 H -0.4660 0.1276 0.3367 0.063 Uiso 0.511(18) 1 calc PR B 1
C34' C -0.2932(19) 0.2087(8) 0.4202(10) 0.047(4) Uiso 0.489(18) 1 d P B 2
H34' H -0.3044 0.2520 0.4419 0.056 Uiso 0.489(18) 1 calc PR B 2
C35' C -0.3911(14) 0.1671(9) 0.3806(10) 0.043(4) Uiso 0.489(18) 1 d P B 2
H35' H -0.4701 0.1857 0.3746 0.052 Uiso 0.489(18) 1 calc PR B 2
C36' C -0.3905(11) 0.1003(8) 0.3475(8) 0.036(4) Uiso 0.489(18) 1 d P B 2
H36' H -0.4587 0.0708 0.3296 0.044 Uiso 0.489(18) 1 calc PR B 2
C37 C -0.2772(6) 0.0877(4) 0.3466(4) 0.060(2) Uani 1 1 d D . .
H37 H -0.2928 0.0454 0.3180 0.072 Uiso 1 1 calc R B 1
C38 C -0.1591(4) 0.1046(3) 0.1727(3) 0.0255(11) Uani 1 1 d . . .
C39 C -0.2299(5) 0.1651(3) 0.1521(3) 0.0267(11) Uani 1 1 d . . .
C40 C -0.3494(5) 0.1600(3) 0.0939(3) 0.0330(12) Uani 1 1 d . . .
H40 H -0.3982 0.1994 0.0796 0.040 Uiso 1 1 calc R . .
C41 C -0.3970(5) 0.0986(3) 0.0572(4) 0.0395(14) Uani 1 1 d . . .
H41 H -0.4777 0.0963 0.0191 0.047 Uiso 1 1 calc R . .
C42 C -0.3240(5) 0.0398(3) 0.0772(4) 0.0375(13) Uani 1 1 d . . .
H42 H -0.3555 -0.0016 0.0506 0.045 Uiso 1 1 calc R . .
C43 C -0.2057(5) 0.0414(3) 0.1357(4) 0.0291(12) Uani 1 1 d . . .
C44 C -0.1299(5) -0.0242(3) 0.1565(4) 0.0394(13) Uani 1 1 d . . .
H44A H -0.0504 -0.0146 0.1981 0.059 Uiso 1 1 calc R . .
H44B H -0.1168 -0.0424 0.1033 0.059 Uiso 1 1 calc R . .
H44C H -0.1745 -0.0573 0.1813 0.059 Uiso 1 1 calc R . .
C45 C -0.1787(5) 0.2334(3) 0.1903(4) 0.0386(13) Uani 1 1 d . . .
H45A H -0.0956 0.2273 0.2289 0.058 Uiso 1 1 calc R . .
H45B H -0.2317 0.2524 0.2230 0.058 Uiso 1 1 calc R . .
H45C H -0.1758 0.2643 0.1435 0.058 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'
Zr Zr -2.9673 0.5597 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
