#------------------------------------------------------------------------------
#$Date: 2016-02-13 14:50:18 +0200 (Sat, 13 Feb 2016) $
#$Revision: 176428 $
#$URL: svn://www.crystallography.net/cod/cif/4/08/58/4085855.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_4085855
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            'C32 H47 N2 Ta'
_chemical_formula_weight         640.67
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_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
_audit_creation_method           SHELXL-97
_cell_angle_alpha                76.545(5)
_cell_angle_beta                 83.679(5)
_cell_angle_gamma                80.275(5)
_cell_formula_units_Z            2
_cell_length_a                   9.566(4)
_cell_length_b                   10.824(4)
_cell_length_c                   15.350(6)
_cell_measurement_reflns_used    9962
_cell_measurement_temperature    200(2)
_cell_measurement_theta_max      32.05
_cell_measurement_theta_min      2.47
_cell_volume                     1519.4(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      200(2)
_diffrn_measured_fraction_theta_full 0.988
_diffrn_measured_fraction_theta_max 0.988
_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  0.0310
_diffrn_reflns_av_sigmaI/netI    0.0401
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_number            25861
_diffrn_reflns_theta_full        31.51
_diffrn_reflns_theta_max         31.51
_diffrn_reflns_theta_min         1.96
_exptl_absorpt_coefficient_mu    3.638
_exptl_absorpt_correction_T_max  0.8681
_exptl_absorpt_correction_T_min  0.4514
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_process_details   sadabs
_exptl_crystal_colour            YELLOW
_exptl_crystal_density_diffrn    1.400
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       PLATE
_exptl_crystal_F_000             652
_exptl_crystal_size_max          0.26
_exptl_crystal_size_mid          0.26
_exptl_crystal_size_min          0.04
_refine_diff_density_max         1.226
_refine_diff_density_min         -1.018
_refine_diff_density_rms         0.092
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.025
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     360
_refine_ls_number_reflns         9993
_refine_ls_number_restraints     6
_refine_ls_restrained_S_all      1.025
_refine_ls_R_factor_all          0.0387
_refine_ls_R_factor_gt           0.0279
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[σ²(Fo²)+(0.0254P)²+0.0000P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0550
_refine_ls_wR_factor_ref         0.0586
_reflns_number_gt                8411
_reflns_number_total             9993
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            om5b00158_si_002.cif
_cod_data_source_block           tabu2s10
_cod_depositor_comments
;
The following automatic conversions were performed:

'_symmetry_cell_setting' value 'Triclinic' changed to 'triclinic'
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.

'_exptl_absorpt_correction_type' value 'EMPIRICAL' changed to
'empirical' 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        1519.3(10)
_cod_original_sg_symbol_H-M      P-1
_cod_database_code               4085855
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
Ta Ta 0.234900(10) 0.541219(9) 0.272237(6) 0.03070(3) Uani 1 1 d D . .
N1 N 0.0894(2) 0.6575(2) 0.32958(15) 0.0374(5) Uani 1 1 d . A .
N2 N 0.3284(2) 0.4549(2) 0.17570(14) 0.0362(5) Uani 1 1 d . A .
C1 C 0.2093(3) 0.3649(2) 0.36953(17) 0.0405(6) Uani 1 1 d . A .
H1A H 0.2885 0.3476 0.4091 0.049 Uiso 1 1 calc R . .
H1B H 0.1208 0.3832 0.4073 0.049 Uiso 1 1 calc R . .
C2 C 0.2027(3) 0.2392(2) 0.34194(18) 0.0415(6) Uani 1 1 d . . .
H2A H 0.1299 0.2550 0.2979 0.050 Uiso 1 1 calc R A .
H2B H 0.2956 0.2112 0.3118 0.050 Uiso 1 1 calc R . .
C3 C 0.1675(4) 0.1318(3) 0.4200(2) 0.0616(9) Uani 1 1 d . A .
H3A H 0.2439 0.1116 0.4620 0.074 Uiso 1 1 calc R . .
H3B H 0.0779 0.1618 0.4528 0.074 Uiso 1 1 calc R . .
C4 C 0.1512(4) 0.0107(3) 0.3916(2) 0.0652(9) Uani 1 1 d . . .
H4A H 0.1178 -0.0513 0.4438 0.098 Uiso 1 1 calc R A .
H4B H 0.2432 -0.0265 0.3668 0.098 Uiso 1 1 calc R . .
H4C H 0.0821 0.0313 0.3459 0.098 Uiso 1 1 calc R . .
C5 C 0.4099(5) 0.6334(5) 0.2946(4) 0.0352(11) Uani 0.695(6) 1 d PD A 1
H5A H 0.4786 0.6359 0.2413 0.042 Uiso 0.695(6) 1 calc PR A 1
H5B H 0.3710 0.7236 0.2965 0.042 Uiso 0.695(6) 1 calc PR A 1
C6 C 0.4934(4) 0.5765(4) 0.3777(3) 0.0463(11) Uani 0.695(6) 1 d PD A 1
H6A H 0.5407 0.4888 0.3744 0.056 Uiso 0.695(6) 1 calc PR A 1
H6B H 0.4262 0.5692 0.4319 0.056 Uiso 0.695(6) 1 calc PR A 1
C7 C 0.6063(5) 0.6572(6) 0.3871(4) 0.0515(12) Uani 0.695(6) 1 d PD A 1
H7A H 0.6681 0.6077 0.4349 0.062 Uiso 0.695(6) 1 calc PR A 1
H7B H 0.6667 0.6730 0.3302 0.062 Uiso 0.695(6) 1 calc PR A 1
C8 C 0.5428(6) 0.7850(7) 0.4096(5) 0.083(2) Uani 0.695(6) 1 d PD A 1
H8A H 0.6194 0.8326 0.4139 0.125 Uiso 0.695(6) 1 calc PR A 1
H8B H 0.4859 0.7702 0.4672 0.125 Uiso 0.695(6) 1 calc PR A 1
H8C H 0.4820 0.8349 0.3624 0.125 Uiso 0.695(6) 1 calc PR A 1
C5A C 0.4319(10) 0.5847(9) 0.3105(10) 0.036(3) Uani 0.305(6) 1 d PD A 2
H5AA H 0.4692 0.5119 0.3583 0.043 Uiso 0.305(6) 1 calc PR A 2
H5AB H 0.5021 0.5873 0.2579 0.043 Uiso 0.305(6) 1 calc PR A 2
C6A C 0.4272(8) 0.7076(8) 0.3434(6) 0.042(2) Uani 0.305(6) 1 d PD A 2
H6AA H 0.3581 0.7060 0.3965 0.050 Uiso 0.305(6) 1 calc PR A 2
H6AB H 0.3916 0.7814 0.2957 0.050 Uiso 0.305(6) 1 calc PR A 2
C7A C 0.5702(10) 0.7296(13) 0.3688(9) 0.051(3) Uani 0.305(6) 1 d PD A 2
H7AA H 0.6092 0.6533 0.4135 0.061 Uiso 0.305(6) 1 calc PR A 2
H7AB H 0.6375 0.7377 0.3147 0.061 Uiso 0.305(6) 1 calc PR A 2
C8A C 0.5607(14) 0.8475(13) 0.4072(11) 0.073(4) Uani 0.305(6) 1 d PD A 2
H8AA H 0.6553 0.8555 0.4222 0.109 Uiso 0.305(6) 1 calc PR A 2
H8AB H 0.4958 0.8396 0.4616 0.109 Uiso 0.305(6) 1 calc PR A 2
H8AC H 0.5249 0.9239 0.3628 0.109 Uiso 0.305(6) 1 calc PR A 2
C11 C 0.0954(2) 0.6342(2) 0.16152(16) 0.0315(5) Uani 1 1 d . A .
C12 C -0.0266(2) 0.5875(2) 0.14646(16) 0.0318(5) Uani 1 1 d . . .
C13 C -0.1129(3) 0.6541(3) 0.07761(18) 0.0411(6) Uani 1 1 d . A .
H13A H -0.1945 0.6207 0.0686 0.049 Uiso 1 1 calc R . .
C14 C -0.0809(3) 0.7684(3) 0.0223(2) 0.0466(6) Uani 1 1 d . . .
H14A H -0.1407 0.8136 -0.0239 0.056 Uiso 1 1 calc R A .
C15 C 0.0383(3) 0.8153(3) 0.03508(19) 0.0437(6) Uani 1 1 d . A .
H15A H 0.0615 0.8928 -0.0032 0.052 Uiso 1 1 calc R . .
C16 C 0.1258(3) 0.7504(2) 0.10378(17) 0.0346(5) Uani 1 1 d . . .
C21 C -0.0742(2) 0.4658(2) 0.20084(17) 0.0329(5) Uani 1 1 d . A .
C22 C -0.0881(3) 0.3681(3) 0.15847(19) 0.0434(6) Uani 1 1 d . . .
H22A H -0.0584 0.3761 0.0965 0.052 Uiso 1 1 calc R A .
C23 C -0.1442(3) 0.2598(3) 0.2051(2) 0.0474(7) Uani 1 1 d . A .
H23A H -0.1509 0.1941 0.1748 0.057 Uiso 1 1 calc R . .
C24 C -0.1905(3) 0.2451(3) 0.29453(19) 0.0426(6) Uani 1 1 d . . .
C25 C -0.1764(3) 0.3409(3) 0.33700(19) 0.0439(6) Uani 1 1 d . A .
H25A H -0.2062 0.3321 0.3990 0.053 Uiso 1 1 calc R . .
C26 C -0.1198(3) 0.4502(3) 0.29130(18) 0.0393(6) Uani 1 1 d . . .
H26A H -0.1122 0.5150 0.3223 0.047 Uiso 1 1 calc R A .
C27 C -0.2567(4) 0.1283(3) 0.3444(2) 0.0612(8) Uani 1 1 d . A .
H27A H -0.2281 0.0585 0.3123 0.092 Uiso 1 1 calc R . .
H27B H -0.3605 0.1502 0.3478 0.092 Uiso 1 1 calc R . .
H27C H -0.2242 0.1006 0.4052 0.092 Uiso 1 1 calc R . .
C31 C 0.2516(3) 0.8104(2) 0.11271(17) 0.0365(5) Uani 1 1 d . A .
C32 C 0.3875(3) 0.7650(3) 0.0816(2) 0.0556(8) Uani 1 1 d . . .
H32A H 0.4021 0.6918 0.0558 0.067 Uiso 1 1 calc R A .
C33 C 0.5019(3) 0.8242(3) 0.0874(3) 0.0631(9) Uani 1 1 d . A .
H33A H 0.5938 0.7905 0.0654 0.076 Uiso 1 1 calc R . .
C34 C 0.4867(3) 0.9310(3) 0.1241(2) 0.0499(7) Uani 1 1 d . . .
C35 C 0.3508(3) 0.9790(3) 0.1529(2) 0.0515(7) Uani 1 1 d . A .
H35A H 0.3363 1.0536 0.1773 0.062 Uiso 1 1 calc R . .
C36 C 0.2346(3) 0.9199(3) 0.14691(19) 0.0436(6) Uani 1 1 d . . .
H36A H 0.1421 0.9554 0.1667 0.052 Uiso 1 1 calc R A .
C37 C 0.6145(4) 0.9924(4) 0.1320(3) 0.0694(10) Uani 1 1 d . A .
H37A H 0.5822 1.0747 0.1494 0.104 Uiso 1 1 calc R . .
H37B H 0.6702 1.0069 0.0740 0.104 Uiso 1 1 calc R . .
H37C H 0.6736 0.9353 0.1776 0.104 Uiso 1 1 calc R . .
C41 C 0.1231(3) 0.6374(3) 0.4226(2) 0.0535(8) Uani 1 1 d . . .
H41A H 0.0406 0.6128 0.4628 0.080 Uiso 1 1 calc R A .
H41B H 0.1471 0.7170 0.4332 0.080 Uiso 1 1 calc R . .
H41C H 0.2043 0.5688 0.4345 0.080 Uiso 1 1 calc R . .
C42 C -0.0321(3) 0.7585(3) 0.3119(2) 0.0498(7) Uani 1 1 d . . .
H42A H -0.1104 0.7388 0.3572 0.075 Uiso 1 1 calc R A .
H42B H -0.0626 0.7637 0.2521 0.075 Uiso 1 1 calc R . .
H42C H -0.0049 0.8408 0.3144 0.075 Uiso 1 1 calc R . .
C51 C 0.4667(3) 0.3836(3) 0.2040(2) 0.0545(8) Uani 1 1 d . . .
H51A H 0.4734 0.2942 0.1987 0.082 Uiso 1 1 calc R A .
H51B H 0.4755 0.3857 0.2667 0.082 Uiso 1 1 calc R . .
H51C H 0.5432 0.4232 0.1657 0.082 Uiso 1 1 calc R . .
C52 C 0.3064(3) 0.4370(3) 0.08736(19) 0.0463(7) Uani 1 1 d . . .
H52A H 0.3847 0.4650 0.0446 0.069 Uiso 1 1 calc R A .
H52B H 0.2163 0.4880 0.0673 0.069 Uiso 1 1 calc R . .
H52C H 0.3033 0.3460 0.0907 0.069 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
N2 Ta N1 156.84(9)
N2 Ta C1 95.07(10)
N1 Ta C1 97.42(10)
N2 Ta C5 99.49(18)
N1 Ta C5 93.13(17)
C1 Ta C5 114.01(15)
N2 Ta C5A 95.2(4)
N1 Ta C5A 101.4(3)
C1 Ta C5A 101.1(3)
C5 Ta C5A 14.3(2)
N2 Ta C11 79.28(9)
N1 Ta C11 77.59(9)
C1 Ta C11 125.83(9)
C5 Ta C11 120.09(14)
C5A Ta C11 132.9(3)
C42 N1 C41 109.7(2)
C42 N1 Ta 143.36(19)
C41 N1 Ta 106.84(18)
C52 N2 C51 109.6(2)
C52 N2 Ta 141.74(17)
C51 N2 Ta 108.66(17)
C2 C1 Ta 122.39(18)
C3 C2 C1 113.6(2)
C4 C3 C2 113.3(3)
C6 C5 Ta 119.3(3)
C5 C6 C7 113.0(4)
C8 C7 C6 113.1(5)
C6A C5A Ta 118.7(6)
C5A C6A C7A 114.8(7)
C8A C7A C6A 113.8(9)
C12 C11 C16 116.9(2)
C12 C11 Ta 124.11(17)
C16 C11 Ta 118.99(17)
C13 C12 C11 121.0(2)
C13 C12 C21 115.0(2)
C11 C12 C21 124.0(2)
C14 C13 C12 120.9(2)
C15 C14 C13 119.2(3)
C14 C15 C16 120.8(3)
C15 C16 C11 121.3(2)
C15 C16 C31 116.5(2)
C11 C16 C31 122.2(2)
C26 C21 C22 117.4(2)
C26 C21 C12 122.6(2)
C22 C21 C12 119.7(2)
C23 C22 C21 121.1(3)
C24 C23 C22 121.4(3)
C23 C24 C25 117.8(2)
C23 C24 C27 121.1(3)
C25 C24 C27 121.1(3)
C24 C25 C26 121.6(3)
C21 C26 C25 120.7(2)
C36 C31 C32 117.3(2)
C36 C31 C16 120.7(2)
C32 C31 C16 121.9(2)
C33 C32 C31 121.2(3)
C32 C33 C34 121.8(3)
C33 C34 C35 117.2(3)
C33 C34 C37 120.9(3)
C35 C34 C37 121.8(3)
C34 C35 C36 121.2(3)
C31 C36 C35 121.1(3)
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
Ta N2 1.984(2)
Ta N1 1.988(2)
Ta C1 2.164(3)
Ta C5 2.184(4)
Ta C5A 2.189(7)
Ta C11 2.221(2)
N1 C42 1.456(3)
N1 C41 1.458(4)
N2 C52 1.456(3)
N2 C51 1.470(3)
C1 C2 1.529(4)
C2 C3 1.515(4)
C3 C4 1.511(4)
C5 C6 1.528(6)
C6 C7 1.538(5)
C7 C8 1.514(7)
C5A C6A 1.521(11)
C6A C7A 1.533(10)
C7A C8A 1.512(12)
C11 C12 1.408(3)
C11 C16 1.413(3)
C12 C13 1.398(3)
C12 C21 1.499(3)
C13 C14 1.388(4)
C14 C15 1.374(4)
C15 C16 1.399(4)
C16 C31 1.494(3)
C21 C26 1.389(4)
C21 C22 1.394(3)
C22 C23 1.384(4)
C23 C24 1.376(4)
C24 C25 1.379(4)
C24 C27 1.516(4)
C25 C26 1.390(4)
C31 C36 1.383(4)
C31 C32 1.384(4)
C32 C33 1.379(4)
C33 C34 1.379(4)
C34 C35 1.381(4)
C34 C37 1.515(4)
C35 C36 1.395(4)
