#------------------------------------------------------------------------------
#$Date: 2016-02-13 14:50:18 +0200 (Sat, 13 Feb 2016) $
#$Revision: 176428 $
#$URL: svn://www.crystallography.net/cod/cif/4/08/58/4085845.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_4085845
loop_
_publ_author_name
'Sattler, Aaron'
'Parkin, Gerard'
_publ_section_title
;
 Synthesis, Structural Characterization, and Cyclometalation Chemistry of
 Tantalum Terphenyl Compounds
;
_journal_issue                   10
_journal_name_full               Organometallics
_journal_page_first              1828
_journal_paper_doi               10.1021/acs.organomet.5b00158
_journal_volume                  34
_journal_year                    2015
_chemical_formula_sum            'C28 H40 N3 Ta'
_chemical_formula_weight         599.58
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/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                 92.520(3)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   8.2335(16)
_cell_length_b                   14.005(3)
_cell_length_c                   22.975(5)
_cell_measurement_reflns_used    9997
_cell_measurement_temperature    125(2)
_cell_measurement_theta_max      29.91
_cell_measurement_theta_min      2.29
_cell_volume                     2646.7(10)
_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, 2008)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      125(2)
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_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  0.0750
_diffrn_reflns_av_sigmaI/netI    0.0590
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       32
_diffrn_reflns_limit_l_min       -32
_diffrn_reflns_number            41984
_diffrn_reflns_theta_full        30.58
_diffrn_reflns_theta_max         30.58
_diffrn_reflns_theta_min         1.70
_exptl_absorpt_coefficient_mu    4.172
_exptl_absorpt_correction_T_max  0.8851
_exptl_absorpt_correction_T_min  0.5734
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_process_details   sadabs
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.505
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             1208
_exptl_crystal_size_max          0.15
_exptl_crystal_size_mid          0.08
_exptl_crystal_size_min          0.03
_refine_diff_density_max         3.749
_refine_diff_density_min         -1.198
_refine_diff_density_rms         0.155
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.008
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     298
_refine_ls_number_reflns         8119
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.008
_refine_ls_R_factor_all          0.0651
_refine_ls_R_factor_gt           0.0372
_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)+(0.0224P)²+4.0471P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0673
_refine_ls_wR_factor_ref         0.0760
_reflns_number_gt                5821
_reflns_number_total             8119
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            om5b00158_si_002.cif
_cod_data_source_block           taets10
_cod_depositor_comments
;
The following automatic conversions were performed:

'_symmetry_cell_setting' value 'Monoclinic' changed to 'monoclinic'
according to
/usr/data/users/saulius/crontab/automatic-downloads/rss-feeds/ACS/lib/dictionaries/cif_core.dic
dictionary named 'cif_core.dic' version 2.4.2 from 2011-04-26.

Automatic conversion script
Id: cif_fix_values 3271 2015-04-21 07:52:19Z andrius 

 Adding full bibliography for 4085842--4085857.cif.
;
_cod_original_cell_volume        2646.7(9)
_cod_original_sg_symbol_H-M      P2(1)/n
_cod_database_code               4085845
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x+1/2, y+1/2, -z+1/2'
'-x, -y, -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
Ta Ta 0.961248(19) 0.194385(12) 0.116014(7) 0.02122(5) Uani 1 1 d .
N4 N 1.1048(4) 0.1488(3) 0.18073(15) 0.0282(8) Uani 1 1 d .
N5 N 1.0609(4) 0.3260(3) 0.11718(18) 0.0350(9) Uani 1 1 d .
N6 N 0.8232(4) 0.0752(2) 0.11534(13) 0.0215(7) Uani 1 1 d .
C1 C 1.0709(5) 0.1598(3) 0.03319(18) 0.0305(10) Uani 1 1 d .
H1A H 1.0281 0.0972 0.0197 0.037 Uiso 1 1 calc R
H1B H 1.0340 0.2080 0.0040 0.037 Uiso 1 1 calc R
C2 C 1.2558(5) 0.1556(4) 0.0341(2) 0.0363(11) Uani 1 1 d .
H2A H 1.2912 0.1404 -0.0050 0.054 Uiso 1 1 calc R
H2B H 1.2946 0.1062 0.0615 0.054 Uiso 1 1 calc R
H2C H 1.3007 0.2176 0.0464 0.054 Uiso 1 1 calc R
C11 C 0.7295(5) 0.2760(3) 0.12438(17) 0.0206(8) Uani 1 1 d .
C12 C 0.6602(5) 0.3217(3) 0.07374(17) 0.0225(8) Uani 1 1 d .
C13 C 0.5530(5) 0.3989(3) 0.07798(19) 0.0299(9) Uani 1 1 d .
H13A H 0.5112 0.4293 0.0435 0.036 Uiso 1 1 calc R
C14 C 0.5076(5) 0.4312(3) 0.13158(19) 0.0305(9) Uani 1 1 d .
H14A H 0.4357 0.4839 0.1342 0.037 Uiso 1 1 calc R
C15 C 0.5673(5) 0.3863(3) 0.18111(19) 0.0295(9) Uani 1 1 d .
H15A H 0.5343 0.4079 0.2180 0.035 Uiso 1 1 calc R
C16 C 0.6758(4) 0.3096(3) 0.17864(17) 0.0222(8) Uani 1 1 d .
C21 C 0.7017(5) 0.2902(3) 0.01385(17) 0.0246(9) Uani 1 1 d .
C22 C 0.6784(4) 0.1963(3) -0.00399(16) 0.0245(8) Uani 1 1 d .
H22A H 0.6401 0.1507 0.0228 0.029 Uiso 1 1 calc R
C23 C 0.7105(5) 0.1676(3) -0.06060(18) 0.0304(10) Uani 1 1 d .
H23A H 0.6936 0.1030 -0.0718 0.037 Uiso 1 1 calc R
C24 C 0.7677(5) 0.2335(4) -0.10127(18) 0.0327(10) Uani 1 1 d .
C25 C 0.7887(6) 0.3267(3) -0.08317(19) 0.0353(11) Uani 1 1 d .
H25A H 0.8275 0.3723 -0.1098 0.042 Uiso 1 1 calc R
C26 C 0.7550(5) 0.3558(3) -0.02719(19) 0.0326(10) Uani 1 1 d .
H26A H 0.7683 0.4210 -0.0166 0.039 Uiso 1 1 calc R
C27 C 0.8004(7) 0.2019(4) -0.16253(19) 0.0476(13) Uani 1 1 d .
H27A H 0.7211 0.2316 -0.1900 0.071 Uiso 1 1 calc R
H27B H 0.7910 0.1322 -0.1652 0.071 Uiso 1 1 calc R
H27C H 0.9104 0.2213 -0.1721 0.071 Uiso 1 1 calc R
C31 C 0.7257(5) 0.2657(3) 0.23597(17) 0.0221(8) Uani 1 1 d .
C32 C 0.6852(5) 0.1721(3) 0.24975(17) 0.0258(9) Uani 1 1 d .
H32A H 0.6385 0.1319 0.2202 0.031 Uiso 1 1 calc R
C33 C 0.7117(5) 0.1362(3) 0.30569(18) 0.0295(9) Uani 1 1 d .
H33A H 0.6812 0.0723 0.3137 0.035 Uiso 1 1 calc R
C34 C 0.7817(5) 0.1918(3) 0.35024(17) 0.0268(8) Uani 1 1 d .
C35 C 0.8282(5) 0.2837(3) 0.33613(18) 0.0309(10) Uani 1 1 d .
H35A H 0.8812 0.3224 0.3651 0.037 Uiso 1 1 calc R
C36 C 0.7990(5) 0.3206(3) 0.28068(18) 0.0298(9) Uani 1 1 d .
H36A H 0.8296 0.3846 0.2729 0.036 Uiso 1 1 calc R
C37 C 0.8031(6) 0.1551(3) 0.41202(18) 0.0364(11) Uani 1 1 d .
H37A H 0.9129 0.1703 0.4275 0.055 Uiso 1 1 calc R
H37B H 0.7873 0.0857 0.4123 0.055 Uiso 1 1 calc R
H37C H 0.7229 0.1854 0.4363 0.055 Uiso 1 1 calc R
C41 C 1.2785(5) 0.1737(4) 0.1856(2) 0.0373(12) Uani 1 1 d .
H41A H 1.3033 0.2037 0.2235 0.056 Uiso 1 1 calc R
H41B H 1.3038 0.2183 0.1544 0.056 Uiso 1 1 calc R
H41C H 1.3439 0.1157 0.1821 0.056 Uiso 1 1 calc R
C42 C 1.0650(5) 0.0857(4) 0.22788(19) 0.0381(11) Uani 1 1 d .
H42A H 1.1412 0.0319 0.2296 0.057 Uiso 1 1 calc R
H42B H 0.9540 0.0616 0.2212 0.057 Uiso 1 1 calc R
H42C H 1.0729 0.1208 0.2648 0.057 Uiso 1 1 calc R
C51 C 1.0788(6) 0.3785(3) 0.1728(2) 0.0437(13) Uani 1 1 d .
H51A H 1.1814 0.4141 0.1741 0.066 Uiso 1 1 calc R
H51B H 1.0790 0.3332 0.2053 0.066 Uiso 1 1 calc R
H51C H 0.9879 0.4231 0.1759 0.066 Uiso 1 1 calc R
C52 C 1.0708(6) 0.3935(4) 0.0694(2) 0.0497(14) Uani 1 1 d .
H52A H 0.9795 0.4382 0.0702 0.075 Uiso 1 1 calc R
H52B H 1.0663 0.3588 0.0323 0.075 Uiso 1 1 calc R
H52C H 1.1734 0.4288 0.0734 0.075 Uiso 1 1 calc R
C61 C 0.9158(5) -0.0142(3) 0.1102(2) 0.0336(10) Uani 1 1 d .
H61A H 0.8892 -0.0575 0.1419 0.050 Uiso 1 1 calc R
H61B H 1.0325 -0.0001 0.1126 0.050 Uiso 1 1 calc R
H61C H 0.8874 -0.0444 0.0726 0.050 Uiso 1 1 calc R
C62 C 0.6510(5) 0.0517(3) 0.11501(17) 0.0252(9) Uani 1 1 d .
H62A H 0.6212 0.0146 0.0800 0.038 Uiso 1 1 calc R
H62B H 0.5870 0.1107 0.1151 0.038 Uiso 1 1 calc R
H62C H 0.6290 0.0140 0.1497 0.038 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'
Ta Ta -0.7052 6.5227 '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
N4 Ta N5 93.23(15)
N4 Ta N6 93.25(14)
N5 Ta N6 169.72(14)
N4 Ta C1 109.12(15)
N5 Ta C1 91.74(17)
N6 Ta C1 93.66(15)
N4 Ta C11 125.97(14)
N5 Ta C11 83.11(14)
N6 Ta C11 86.63(13)
C1 Ta C11 124.83(15)
C42 N4 C41 109.9(3)
C42 N4 Ta 128.1(3)
C41 N4 Ta 122.0(3)
C52 N5 C51 108.8(4)
C52 N5 Ta 128.3(3)
C51 N5 Ta 119.5(3)
C62 N6 C61 108.3(3)
C62 N6 Ta 137.3(3)
C61 N6 Ta 114.2(2)
C2 C1 Ta 116.5(3)
C16 C11 C12 116.0(3)
C16 C11 Ta 122.9(3)
C12 C11 Ta 118.1(3)
C13 C12 C11 121.4(4)
C13 C12 C21 117.4(3)
C11 C12 C21 121.2(3)
C14 C13 C12 120.8(4)
C15 C14 C13 119.3(4)
C14 C15 C16 121.6(4)
C15 C16 C11 120.9(4)
C15 C16 C31 115.6(3)
C11 C16 C31 123.5(3)
C22 C21 C26 117.8(4)
C22 C21 C12 121.1(3)
C26 C21 C12 121.0(4)
C21 C22 C23 121.2(4)
C22 C23 C24 120.8(4)
C25 C24 C23 117.5(4)
C25 C24 C27 122.2(4)
C23 C24 C27 120.3(5)
C24 C25 C26 122.0(4)
C25 C26 C21 120.8(4)
C32 C31 C36 116.8(4)
C32 C31 C16 121.9(3)
C36 C31 C16 121.0(4)
C33 C32 C31 121.5(4)
C32 C33 C34 121.5(4)
C35 C34 C33 117.2(4)
C35 C34 C37 120.9(4)
C33 C34 C37 121.9(4)
C34 C35 C36 121.5(4)
C35 C36 C31 121.5(4)
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
Ta N4 1.965(3)
Ta N5 2.017(4)
Ta N6 2.019(3)
Ta C1 2.196(4)
Ta C11 2.240(4)
N4 C42 1.446(6)
N4 C41 1.471(5)
N5 C52 1.454(6)
N5 C51 1.476(6)
N6 C62 1.455(5)
N6 C61 1.474(5)
C1 C2 1.523(6)
C11 C16 1.421(5)
C11 C12 1.425(5)
C12 C13 1.401(6)
C12 C21 1.499(5)
C13 C14 1.379(6)
C14 C15 1.372(6)
C15 C16 1.400(5)
C16 C31 1.495(5)
C21 C22 1.389(6)
C21 C26 1.401(6)
C22 C23 1.397(6)
C23 C24 1.409(6)
C24 C25 1.378(7)
C24 C27 1.511(6)
C25 C26 1.389(6)
C31 C32 1.392(6)
C31 C36 1.398(5)
C32 C33 1.388(6)
C33 C34 1.390(6)
C34 C35 1.386(6)
C34 C37 1.512(6)
C35 C36 1.386(6)
