#------------------------------------------------------------------------------
#$Date: 2016-03-23 16:29:29 +0200 (Wed, 23 Mar 2016) $
#$Revision: 179380 $
#$URL: svn://www.crystallography.net/cod/cif/4/32/77/4327706.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_4327706
loop_
_publ_author_name
'Kurt S. Heinselman'
'Vincent M. Miskowski'
'Steven J. Geib'
'Louis C. Wang'
'Michael D. Hopkins'
_publ_section_title
;
 Molecular Structures and FT-Raman Spectroscopy of Luminescent Niobium and
 Tantalum Arylimido Compounds
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              5530
_journal_page_last               5538
_journal_paper_doi               10.1021/ic970494+
_journal_volume                  36
_journal_year                    1997
_chemical_formula_sum            'C18 H33 Br3 N3 Ta'
_chemical_formula_weight         712.15
_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
_cell_angle_alpha                90.00
_cell_angle_beta                 91.95(3)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   10.111(2)
_cell_length_b                   14.700(3)
_cell_length_c                   15.931(3)
_cell_measurement_reflns_used    25
_cell_measurement_temperature    208(2)
_cell_measurement_theta_max      15.0
_cell_measurement_theta_min      10.0
_cell_volume                     2366.5(8)
_computing_structure_refinement  'SHELXL-93 (Sheldrick, 1993)'
_computing_structure_solution    'SHELXS-86 (Sheldrick, 1990)'
_diffrn_ambient_temperature      208(2)
_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  0.0961
_diffrn_reflns_av_sigmaI/netI    0.0776
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -8
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -7
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            3952
_diffrn_reflns_theta_max         24.00
_diffrn_reflns_theta_min         2.35
_exptl_absorpt_coefficient_mu    9.717
_exptl_absorpt_correction_T_max  0.89
_exptl_absorpt_correction_T_min  0.42
_exptl_absorpt_correction_type   psi-scan
_exptl_crystal_density_diffrn    1.999
_exptl_crystal_F_000             1360
_exptl_crystal_size_max          0.37
_exptl_crystal_size_mid          0.26
_exptl_crystal_size_min          0.17
_refine_diff_density_max         2.280
_refine_diff_density_min         -1.217
_refine_diff_density_rms         0.172
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_all   1.033
_refine_ls_goodness_of_fit_obs   1.093
_refine_ls_matrix_type           full
_refine_ls_number_parameters     226
_refine_ls_number_reflns         3726
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.046
_refine_ls_restrained_S_obs      1.093
_refine_ls_R_factor_all          0.0908
_refine_ls_R_factor_obs          0.0521
_refine_ls_shift/esd_max         -0.124
_refine_ls_shift/esd_mean        0.003
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[σ²(Fo²)+(0.0607P)²+0.0000P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.1290
_refine_ls_wR_factor_obs         0.1104
_reflns_number_observed          2562
_reflns_number_total             3726
_reflns_observed_criterion       >2sigma(I)
_cod_data_source_file            ic9704942B_3.cif
_cod_data_source_block           compound6
_cod_depositor_comments
;
The following automatic conversions were performed:

'_refine_ls_weighting_scheme' value 'calc
w=1/[\s^2^(Fo^2^)+(0.0607P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' was
changed to 'calc'. New tag '_refine_ls_weighting_details' was
created. The value of the new tag was set to
'w=1/[\s^2^(Fo^2^)+(0.0607P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'.

Automatic conversion script
Id: cif_fix_values 3143 2015-03-26 13:38:13Z robertas 
;
_cod_database_code               4327706
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_thermal_displace_type
_atom_site_occupancy
_atom_site_calc_flag
_atom_site_refinement_flags
Ta Ta 0.12531(5) 0.07369(4) 0.27494(3) 0.0366(2) Uani 1 d .
Br1 Br -0.12275(14) 0.04218(10) 0.27048(11) 0.0579(4) Uani 1 d .
Br2 Br 0.37469(13) 0.08030(11) 0.26015(9) 0.0536(4) Uani 1 d .
Br3 Br 0.0904(2) 0.18923(10) 0.16008(10) 0.0633(5) Uani 1 d .
N1 N 0.1237(10) 0.1444(7) 0.3651(6) 0.038(2) Uani 1 d .
N2 N 0.1465(10) -0.0669(7) 0.3422(6) 0.041(2) Uani 1 d .
N3 N 0.1356(12) -0.0413(8) 0.1560(6) 0.049(3) Uani 1 d .
C1 C 0.1185(12) 0.2049(8) 0.4327(8) 0.039(3) Uani 1 d .
C2 C 0.2164(12) 0.2010(8) 0.4988(8) 0.040(3) Uani 1 d .
C3 C 0.2083(13) 0.2602(10) 0.5653(9) 0.049(3) Uani 1 d .
H3A H 0.2730(13) 0.2589(10) 0.6082(9) 0.059 Uiso 1 calc R
C4 C 0.1069(17) 0.3205(11) 0.5692(10) 0.065(4) Uani 1 d .
H4A H 0.1027(17) 0.3594(11) 0.6151(10) 0.078 Uiso 1 calc R
C5 C 0.0105(16) 0.3249(10) 0.5066(10) 0.061(4) Uani 1 d .
H5A H -0.0590(16) 0.3658(10) 0.5112(10) 0.073 Uiso 1 calc R
C6 C 0.0152(12) 0.2697(9) 0.4370(8) 0.043(3) Uani 1 d .
C7 C 0.3303(11) 0.1333(8) 0.4936(7) 0.036(3) Uani 1 d .
H7A H 0.3064(11) 0.0888(8) 0.4499(7) 0.043 Uiso 1 calc R
C8 C 0.3551(15) 0.0818(11) 0.5749(10) 0.066(4) Uani 1 d .
H8A H 0.4273(15) 0.0402(11) 0.5686(10) 0.098 Uiso 1 calc R
H8B H 0.2770(15) 0.0485(11) 0.5885(10) 0.098 Uiso 1 calc R
H8C H 0.3768(15) 0.1240(11) 0.6193(10) 0.098 Uiso 1 calc R
C9 C 0.4583(13) 0.1802(9) 0.4686(9) 0.050(3) Uani 1 d .
H9A H 0.4428(13) 0.2129(9) 0.4171(9) 0.075 Uiso 1 calc R
H9B H 0.5258(13) 0.1353(9) 0.4611(9) 0.075 Uiso 1 calc R
H9C H 0.4866(13) 0.2218(9) 0.5120(9) 0.075 Uiso 1 calc R
C10 C -0.0943(14) 0.2761(9) 0.3687(9) 0.054(4) Uani 1 d .
H10A H -0.0689(14) 0.2365(9) 0.3225(9) 0.065 Uiso 1 calc R
C11 C -0.2268(14) 0.2425(13) 0.3979(10) 0.076(5) Uani 1 d .
H11A H -0.2919(14) 0.2480(13) 0.3529(10) 0.114 Uiso 1 calc R
H11B H -0.2533(14) 0.2784(13) 0.4449(10) 0.114 Uiso 1 calc R
H11C H -0.2191(14) 0.1799(13) 0.4145(10) 0.114 Uiso 1 calc R
C12 C -0.1071(15) 0.3731(10) 0.3331(10) 0.063(4) Uani 1 d .
H12A H -0.0225(15) 0.3933(10) 0.3149(10) 0.094 Uiso 1 calc R
H12B H -0.1374(15) 0.4133(10) 0.3759(10) 0.094 Uiso 1 calc R
H12C H -0.1695(15) 0.3733(10) 0.2863(10) 0.094 Uiso 1 calc R
C13 C 0.2808(13) -0.0881(9) 0.3788(8) 0.050(3) Uani 1 d .
H13A H 0.3059(13) -0.0423(9) 0.4193(8) 0.074 Uiso 1 calc R
H13B H 0.3436(13) -0.0890(9) 0.3349(8) 0.074 Uiso 1 calc R
H13C H 0.2794(13) -0.1465(9) 0.4058(8) 0.074 Uiso 1 calc R
C14 C 0.1098(14) -0.1376(9) 0.2804(9) 0.054(4) Uani 1 d .
H14A H 0.0149(14) -0.1358(9) 0.2693(9) 0.065 Uiso 1 calc R
H14B H 0.1317(14) -0.1969(9) 0.3038(9) 0.065 Uiso 1 calc R
C15 C 0.1778(16) -0.1260(11) 0.2008(10) 0.064(4) Uani 1 d .
H15A H 0.1591(16) -0.1780(11) 0.1649(10) 0.077 Uiso 1 calc R
H15B H 0.2726(16) -0.1239(11) 0.2123(10) 0.077 Uiso 1 calc R
C16 C 0.0041(15) -0.0583(11) 0.1105(10) 0.067(5) Uani 1 d .
H16A H -0.0619(15) -0.0715(11) 0.1506(10) 0.101 Uiso 1 calc R
H16B H 0.0123(15) -0.1090(11) 0.0730(10) 0.101 Uiso 1 calc R
H16C H -0.0214(15) -0.0052(11) 0.0789(10) 0.101 Uiso 1 calc R
C17 C 0.0595(15) -0.0740(11) 0.4149(9) 0.063(4) Uani 1 d .
H17A H 0.0832(15) -0.0280(11) 0.4554(9) 0.094 Uiso 1 calc R
H17C H 0.0698(15) -0.1330(11) 0.4403(9) 0.094 Uiso 1 calc R
H17D H -0.0310(15) -0.0658(11) 0.3962(9) 0.094 Uiso 1 calc R
C18 C 0.2312(17) -0.0217(13) 0.0912(9) 0.077(5) Uani 1 d .
H18C H 0.2053(17) 0.0328(13) 0.0617(9) 0.115 Uiso 1 calc R
H18D H 0.2333(17) -0.0715(13) 0.0523(9) 0.115 Uiso 1 calc R
H18A H 0.3175(17) -0.0135(13) 0.1171(9) 0.115 Uiso 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'
Br Br -0.2901 2.4595 '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
N1 Ta N2 98.7(4)
N1 Ta Br3 100.9(3)
N2 Ta Br3 160.2(3)
N1 Ta Br2 95.1(3)
N2 Ta Br2 90.0(3)
Br3 Ta Br2 91.24(6)
N1 Ta N3 173.9(4)
N2 Ta N3 75.4(4)
Br3 Ta N3 85.1(3)
Br2 Ta N3 83.7(3)
N1 Ta Br1 95.3(3)
N2 Ta Br1 85.8(3)
Br3 Ta Br1 89.37(6)
Br2 Ta Br1 169.23(6)
N3 Ta Br1 85.6(3)
C1 N1 Ta 176.1(9)
C14 N2 C17 109.3(11)
C14 N2 C13 108.7(10)
C17 N2 C13 103.7(10)
C14 N2 Ta 107.5(7)
C17 N2 Ta 111.9(8)
C13 N2 Ta 115.6(7)
C18 N3 C15 108.5(13)
C18 N3 C16 106.5(11)
C15 N3 C16 108.9(12)
C18 N3 Ta 116.0(9)
C15 N3 Ta 102.5(7)
C16 N3 Ta 114.2(9)
N1 C1 C6 120.7(11)
N1 C1 C2 120.1(11)
C6 C1 C2 119.2(11)
C3 C2 C1 119.1(12)
C3 C2 C7 121.3(11)
C1 C2 C7 119.6(11)
C4 C3 C2 120.9(14)
C3 C4 C5 121.0(15)
C4 C5 C6 121.0(14)
C5 C6 C1 118.7(13)
C5 C6 C10 119.5(12)
C1 C6 C10 121.7(12)
C8 C7 C2 112.6(11)
C8 C7 C9 109.3(11)
C2 C7 C9 111.5(10)
C11 C10 C6 112.8(12)
C11 C10 C12 110.6(13)
C6 C10 C12 111.7(12)
N2 C14 C15 112.3(11)
C14 C15 N3 112.0(12)
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
Ta N1 1.774(10)
Ta N2 2.335(10)
Ta Br3 2.513(2)
Ta Br2 2.5423(15)
Ta N3 2.544(11)
Ta Br1 2.549(2)
N1 C1 1.40(2)
N2 C14 1.47(2)
N2 C17 1.48(2)
N2 C13 1.49(2)
N3 C18 1.47(2)
N3 C15 1.49(2)
N3 C16 1.51(2)
C1 C6 1.42(2)
C1 C2 1.42(2)
C2 C3 1.38(2)
C2 C7 1.53(2)
C3 C4 1.36(2)
C4 C5 1.37(2)
C5 C6 1.38(2)
C6 C10 1.53(2)
C7 C8 1.51(2)
C7 C9 1.53(2)
C10 C11 1.52(2)
C10 C12 1.54(2)
C14 C15 1.47(2)
loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
N2 Ta N1 C1 -160.9(131)
Br3 Ta N1 C1 16.0(132)
Br2 Ta N1 C1 108.3(131)
N3 Ta N1 C1 -173.3(111)
Br1 Ta N1 C1 -74.4(131)
N1 Ta N2 C14 163.1(8)
Br3 Ta N2 C14 -7.9(13)
Br2 Ta N2 C14 -101.7(8)
N3 Ta N2 C14 -18.2(8)
Br1 Ta N2 C14 68.4(8)
N1 Ta N2 C17 43.1(10)
Br3 Ta N2 C17 -128.0(9)
Br2 Ta N2 C17 138.3(9)
N3 Ta N2 C17 -138.2(10)
Br1 Ta N2 C17 -51.7(9)
N1 Ta N2 C13 -75.3(9)
Br3 Ta N2 C13 113.6(9)
Br2 Ta N2 C13 19.9(8)
N3 Ta N2 C13 103.4(9)
Br1 Ta N2 C13 -170.1(8)
N1 Ta N3 C18 -117.1(38)
N2 Ta N3 C18 -129.7(11)
Br3 Ta N3 C18 53.8(11)
Br2 Ta N3 C18 -38.0(11)
Br1 Ta N3 C18 143.5(11)
N1 Ta N3 C15 0.9(42)
N2 Ta N3 C15 -11.7(8)
Br3 Ta N3 C15 171.8(9)
Br2 Ta N3 C15 80.0(9)
Br1 Ta N3 C15 -98.5(9)
N1 Ta N3 C16 118.5(38)
N2 Ta N3 C16 105.9(10)
Br3 Ta N3 C16 -70.6(9)
Br2 Ta N3 C16 -162.4(9)
Br1 Ta N3 C16 19.1(9)
Ta N1 C1 C6 32.5(138)
Ta N1 C1 C2 -148.5(125)
N1 C1 C2 C3 -179.0(12)
C6 C1 C2 C3 0.1(18)
N1 C1 C2 C7 2.6(18)
C6 C1 C2 C7 -178.3(11)
C1 C2 C3 C4 1.4(20)
C7 C2 C3 C4 179.8(13)
C2 C3 C4 C5 -0.7(23)
C3 C4 C5 C6 -1.4(24)
C4 C5 C6 C1 2.8(21)
C4 C5 C6 C10 179.7(14)
N1 C1 C6 C5 176.9(12)
C2 C1 C6 C5 -2.1(19)
N1 C1 C6 C10 0.1(19)
C2 C1 C6 C10 -179.0(12)
C3 C2 C7 C8 47.9(17)
C1 C2 C7 C8 -133.8(13)
C3 C2 C7 C9 -75.4(15)
C1 C2 C7 C9 103.0(13)
C5 C6 C10 C11 -68.0(18)
C1 C6 C10 C11 108.9(15)
C5 C6 C10 C12 57.3(18)
C1 C6 C10 C12 -125.9(14)
C17 N2 C14 C15 171.1(12)
C13 N2 C14 C15 -76.4(14)
Ta N2 C14 C15 49.4(13)
N2 C14 C15 N3 -65.9(16)
C18 N3 C15 C14 164.8(12)
C16 N3 C15 C14 -79.7(14)
Ta N3 C15 C14 41.5(13)
