#------------------------------------------------------------------------------
#$Date: 2016-03-21 14:01:21 +0200 (Mon, 21 Mar 2016) $
#$Revision: 178709 $
#$URL: svn://www.crystallography.net/cod/cif/4/08/20/4082063.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_4082063
loop_
_publ_author_name
'Sattler, Aaron'
'Labinger, Jay A.'
'Bercaw, John E.'
_publ_section_title
;
 Highly Selective Olefin Trimerization Catalysis by a Borane-Activated
 Titanium Trimethyl Complex
;
_journal_issue                   23
_journal_name_full               Organometallics
_journal_page_first              6899
_journal_paper_doi               10.1021/om401098m
_journal_volume                  32
_journal_year                    2013
_chemical_formula_sum            'C34 H41 N O2 Ti'
_chemical_formula_weight         543.58
_chemical_name_systematic
; 
 ? 
;
_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
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 108.341(2)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   12.6220(4)
_cell_length_b                   18.3101(7)
_cell_length_c                   13.1507(5)
_cell_measurement_reflns_used    9328
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      38.32
_cell_measurement_theta_min      2.76
_cell_volume                     2884.87(18)
_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      100(2)
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 1.000
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       'φ and ω 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  0.0959
_diffrn_reflns_av_sigmaI/netI    0.0498
_diffrn_reflns_limit_h_max       21
_diffrn_reflns_limit_h_min       -21
_diffrn_reflns_limit_k_max       31
_diffrn_reflns_limit_k_min       -31
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            188107
_diffrn_reflns_theta_full        37.78
_diffrn_reflns_theta_max         37.78
_diffrn_reflns_theta_min         1.70
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.327
_exptl_absorpt_correction_T_max  0.9680
_exptl_absorpt_correction_T_min  0.8885
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_process_details   sadabs
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.252
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             1160
_exptl_crystal_size_max          0.37
_exptl_crystal_size_mid          0.27
_exptl_crystal_size_min          0.10
_refine_diff_density_max         1.114
_refine_diff_density_min         -0.518
_refine_diff_density_rms         0.089
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.037
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     348
_refine_ls_number_reflns         15474
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.037
_refine_ls_R_factor_all          0.0803
_refine_ls_R_factor_gt           0.0489
_refine_ls_shift/su_max          0.003
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[σ²(Fo²)+(0.0643P)²+1.0466P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1178
_refine_ls_wR_factor_ref         0.1351
_reflns_number_gt                11124
_reflns_number_total             15474
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            om401098m_si_002.cif
_cod_data_source_block           ftme3s10
_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 2.4.2 from 2011-04-26.

Automatic conversion script
Id: cif_fix_values 1891 2012-01-12 08:04:46Z andrius 
;
_cod_original_sg_symbol_H-M      P2(1)/c
_cod_database_code               4082063
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
Ti Ti 0.589176(15) 0.647276(10) 0.685788(16) 0.01303(5) Uani 1 1 d .
N N 0.62183(7) 0.52827(5) 0.69287(7) 0.01057(14) Uani 1 1 d .
O1 O 0.45081(6) 0.61192(4) 0.69172(6) 0.01275(13) Uani 1 1 d .
O2 O 0.66126(7) 0.43113(5) 0.88764(7) 0.01755(15) Uani 1 1 d .
C1 C 0.75048(10) 0.65959(7) 0.66920(12) 0.0240(2) Uani 1 1 d .
H1A H 0.8071 0.6430 0.7349 0.036 Uiso 1 1 calc R
H1B H 0.7633 0.7111 0.6566 0.036 Uiso 1 1 calc R
H1C H 0.7554 0.6303 0.6085 0.036 Uiso 1 1 calc R
C2 C 0.60944(12) 0.72352(10) 0.80629(16) 0.0395(4) Uani 1 1 d .
H2A H 0.5363 0.7369 0.8117 0.059 Uiso 1 1 calc R
H2B H 0.6461 0.7671 0.7898 0.059 Uiso 1 1 calc R
H2C H 0.6556 0.7027 0.8745 0.059 Uiso 1 1 calc R
C3 C 0.51450(13) 0.69982(9) 0.53937(13) 0.0323(3) Uani 1 1 d .
H3A H 0.4827 0.6633 0.4837 0.048 Uiso 1 1 calc R
H3B H 0.5707 0.7286 0.5200 0.048 Uiso 1 1 calc R
H3C H 0.4551 0.7322 0.5459 0.048 Uiso 1 1 calc R
C11 C 0.38319(8) 0.55512(5) 0.67176(8) 0.01048(15) Uani 1 1 d .
C12 C 0.42792(8) 0.48654(5) 0.65765(8) 0.01082(15) Uani 1 1 d .
C13 C 0.35873(8) 0.42429(6) 0.63485(8) 0.01283(16) Uani 1 1 d .
H13A H 0.3893 0.3783 0.6257 0.015 Uiso 1 1 calc R
C14 C 0.24666(8) 0.42966(6) 0.62560(8) 0.01303(16) Uani 1 1 d .
C15 C 0.20484(8) 0.49853(6) 0.64048(8) 0.01196(16) Uani 1 1 d .
H15A H 0.1280 0.5020 0.6343 0.014 Uiso 1 1 calc R
C16 C 0.26848(8) 0.56199(5) 0.66363(8) 0.01042(15) Uani 1 1 d .
C17 C 0.54539(8) 0.47775(5) 0.67207(8) 0.01134(15) Uani 1 1 d .
H17A H 0.5698 0.4294 0.6656 0.014 Uiso 1 1 calc R
C18 C 0.17021(9) 0.36433(6) 0.60217(11) 0.0203(2) Uani 1 1 d .
H18A H 0.1961 0.3290 0.5592 0.030 Uiso 1 1 calc R
H18B H 0.0942 0.3800 0.5624 0.030 Uiso 1 1 calc R
H18C H 0.1706 0.3415 0.6697 0.030 Uiso 1 1 calc R
C21 C 0.73362(8) 0.50131(5) 0.71029(8) 0.01065(15) Uani 1 1 d .
C22 C 0.81092(8) 0.50522(6) 0.81349(8) 0.01199(16) Uani 1 1 d .
C23 C 0.92038(8) 0.48289(6) 0.82790(9) 0.01474(18) Uani 1 1 d .
H23A H 0.9739 0.4854 0.8972 0.018 Uiso 1 1 calc R
C24 C 0.95248(8) 0.45709(6) 0.74256(9) 0.01520(18) Uani 1 1 d .
H24A H 1.0274 0.4423 0.7536 0.018 Uiso 1 1 calc R
C25 C 0.87476(9) 0.45307(6) 0.64133(9) 0.01481(17) Uani 1 1 d .
H25A H 0.8963 0.4352 0.5829 0.018 Uiso 1 1 calc R
C26 C 0.76508(8) 0.47516(6) 0.62491(8) 0.01328(17) Uani 1 1 d .
H26A H 0.7119 0.4723 0.5554 0.016 Uiso 1 1 calc R
C31 C 0.77851(8) 0.53282(6) 0.90589(8) 0.01385(17) Uani 1 1 d .
C32 C 0.70074(9) 0.49402(6) 0.94208(8) 0.01505(18) Uani 1 1 d .
C33 C 0.67195(10) 0.51886(8) 1.02988(9) 0.0203(2) Uani 1 1 d .
H33A H 0.6195 0.4925 1.0540 0.024 Uiso 1 1 calc R
C34 C 0.72035(10) 0.58252(8) 1.08226(10) 0.0233(2) Uani 1 1 d .
H34A H 0.7000 0.5998 1.1416 0.028 Uiso 1 1 calc R
C35 C 0.79805(10) 0.62094(8) 1.04861(10) 0.0227(2) Uani 1 1 d .
H35A H 0.8310 0.6642 1.0848 0.027 Uiso 1 1 calc R
C36 C 0.82720(9) 0.59535(7) 0.96111(9) 0.0185(2) Uani 1 1 d .
H36A H 0.8814 0.6211 0.9388 0.022 Uiso 1 1 calc R
C37 C 0.57344(11) 0.39362(8) 0.91189(10) 0.0239(2) Uani 1 1 d .
H37A H 0.5497 0.3518 0.8636 0.036 Uiso 1 1 calc R
H37B H 0.5102 0.4269 0.9026 0.036 Uiso 1 1 calc R
H37C H 0.5999 0.3764 0.9862 0.036 Uiso 1 1 calc R
C41 C 0.21906(8) 0.63563(5) 0.67999(8) 0.01070(15) Uani 1 1 d .
C42 C 0.09274(8) 0.63094(6) 0.66341(9) 0.01466(18) Uani 1 1 d .
H42A H 0.0536 0.6135 0.5899 0.018 Uiso 1 1 calc R
H42B H 0.0792 0.5953 0.7145 0.018 Uiso 1 1 calc R
C43 C 0.27555(9) 0.66243(6) 0.79592(9) 0.01456(17) Uani 1 1 d .
H43A H 0.2620 0.6267 0.8469 0.017 Uiso 1 1 calc R
H43B H 0.3572 0.6660 0.8099 0.017 Uiso 1 1 calc R
C44 C 0.23583(8) 0.69298(6) 0.59980(8) 0.01285(16) Uani 1 1 d .
H44A H 0.3163 0.6971 0.6080 0.015 Uiso 1 1 calc R
H44B H 0.1964 0.6768 0.5257 0.015 Uiso 1 1 calc R
C45 C 0.04575(9) 0.70592(6) 0.68034(10) 0.0177(2) Uani 1 1 d .
H45A H -0.0362 0.7014 0.6684 0.021 Uiso 1 1 calc R
C46 C 0.22958(9) 0.73743(6) 0.81370(9) 0.01735(19) Uani 1 1 d .
H46A H 0.2680 0.7541 0.8887 0.021 Uiso 1 1 calc R
C47 C 0.19092(9) 0.76783(6) 0.61917(9) 0.01517(18) Uani 1 1 d .
H47A H 0.2044 0.8042 0.5679 0.018 Uiso 1 1 calc R
C48 C 0.10390(10) 0.73142(7) 0.79545(10) 0.0207(2) Uani 1 1 d .
H48A H 0.0739 0.7795 0.8074 0.025 Uiso 1 1 calc R
H48B H 0.0898 0.6961 0.8467 0.025 Uiso 1 1 calc R
C49 C 0.25084(9) 0.79260(6) 0.73434(10) 0.01761(19) Uani 1 1 d .
H49A H 0.2231 0.8414 0.7465 0.021 Uiso 1 1 calc R
H49B H 0.3320 0.7965 0.7458 0.021 Uiso 1 1 calc R
C50 C 0.06564(9) 0.76186(6) 0.60167(10) 0.0181(2) Uani 1 1 d .
H50A H 0.0265 0.7463 0.5272 0.022 Uiso 1 1 calc R
H50B H 0.0357 0.8100 0.6133 0.022 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'
O O 0.0106 0.0060 '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
O1 Ti C2 95.33(5)
O1 Ti C3 92.35(5)
C2 Ti C3 107.83(8)
O1 Ti C1 165.68(4)
C2 Ti C1 96.63(6)
C3 Ti C1 91.46(6)
O1 Ti N 79.81(3)
C2 Ti N 131.00(7)
C3 Ti N 121.01(6)
C1 Ti N 86.39(4)
C17 N C21 114.40(9)
C17 N Ti 125.06(7)
C21 N Ti 120.20(6)
C11 O1 Ti 144.29(7)
C32 O2 C37 118.12(9)
O1 C11 C12 117.83(8)
O1 C11 C16 121.65(9)
C12 C11 C16 120.51(9)
C13 C12 C11 120.01(9)
C13 C12 C17 118.68(9)
C11 C12 C17 121.22(9)
C14 C13 C12 120.58(9)
C13 C14 C15 118.03(9)
C13 C14 C18 122.18(10)
C15 C14 C18 119.79(9)
C16 C15 C14 124.34(9)
C15 C16 C11 116.52(9)
C15 C16 C41 122.31(8)
C11 C16 C41 121.18(8)
N C17 C12 127.67(9)
C26 C21 C22 120.75(9)
C26 C21 N 120.23(9)
C22 C21 N 118.95(9)
C23 C22 C21 118.31(9)
C23 C22 C31 120.25(9)
C21 C22 C31 121.44(9)
C24 C23 C22 121.16(9)
C25 C24 C23 119.72(9)
C24 C25 C26 120.18(10)
C21 C26 C25 119.87(9)
C36 C31 C32 118.59(10)
C36 C31 C22 121.08(10)
C32 C31 C22 120.28(10)
O2 C32 C33 124.30(10)
O2 C32 C31 115.22(9)
C33 C32 C31 120.44(11)
C32 C33 C34 119.69(11)
C35 C34 C33 120.68(11)
C34 C35 C36 119.28(12)
C31 C36 C35 121.28(11)
C16 C41 C42 112.36(8)
C16 C41 C43 109.68(8)
C42 C41 C43 107.02(8)
C16 C41 C44 110.66(8)
C42 C41 C44 107.34(8)
C43 C41 C44 109.68(8)
C45 C42 C41 111.00(9)
C46 C43 C41 110.77(9)
C47 C44 C41 110.83(8)
C50 C45 C48 109.51(10)
C50 C45 C42 110.25(9)
C48 C45 C42 109.15(10)
C48 C46 C49 109.54(10)
C48 C46 C43 109.51(9)
C49 C46 C43 109.22(9)
C50 C47 C49 109.59(9)
C50 C47 C44 109.26(9)
C49 C47 C44 109.57(9)
C46 C48 C45 109.10(9)
C47 C49 C46 109.83(9)
C47 C50 C45 109.14(9)
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
Ti O1 1.8871(7)
Ti C2 2.0665(14)
Ti C3 2.0927(14)
Ti C1 2.1268(11)
Ti N 2.2142(9)
N C17 1.3020(13)
N C21 1.4434(12)
O1 C11 1.3184(12)
O2 C32 1.3647(14)
O2 C37 1.4228(14)
C11 C12 1.4127(14)
C11 C16 1.4234(13)
C12 C13 1.4095(14)
C12 C17 1.4434(13)
C13 C14 1.3846(14)
C14 C15 1.4044(15)
C14 C18 1.5066(15)
C15 C16 1.3906(14)
C16 C41 1.5290(14)
C21 C26 1.3886(14)
C21 C22 1.4020(14)
C22 C23 1.3953(14)
C22 C31 1.4874(14)
C23 C24 1.3903(15)
C24 C25 1.3848(15)
C25 C26 1.3923(14)
C31 C36 1.3911(16)
C31 C32 1.4102(15)
C32 C33 1.3915(15)
C33 C34 1.3934(19)
C34 C35 1.3878(19)
C35 C36 1.3948(16)
C41 C42 1.5421(14)
C41 C43 1.5458(15)
C41 C44 1.5493(14)
C42 C45 1.5392(16)
C43 C46 1.5370(16)
C44 C47 1.5347(15)
C45 C50 1.5317(17)
C45 C48 1.5326(18)
C46 C48 1.5318(16)
C46 C49 1.5357(17)
C47 C50 1.5285(15)
C47 C49 1.5332(16)
