#------------------------------------------------------------------------------
#$Date: 2016-03-25 12:14:32 +0200 (Fri, 25 Mar 2016) $
#$Revision: 179805 $
#$URL: svn://www.crystallography.net/cod/cif/7/01/01/7010143.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_7010143
loop_
_publ_author_name
'Nielson, Alastair J.'
'Glenny, Mark W.'
'Rickard, Clifton E. F.'
'Waters, Joyce M.'
_publ_section_title
;
 Regiospecific influences of phenyl ring substituents in monoimido
 complexes of tantalum and tungsten and bis imido complexes of
 molybdenum
;
_journal_issue                   24
_journal_name_full
'Journal of the Chemical Society, Dalton Transactions'
_journal_page_first              4569
_journal_paper_doi               10.1039/b006420n
_journal_year                    2000
_chemical_formula_moiety         '[Ta Cl4 (N C6 H4 CMe3-2)(py)].pyH.C H2 Cl2'
_chemical_formula_sum            'C21 H26 Cl6 N3 Ta'
_chemical_formula_weight         714.10
_chemical_name_systematic
;
[Ta Cl4 (N C6 H4 CMe3-2)(py)].pyH.C H2 Cl2
;
_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                100.66
_cell_angle_beta                 93.2530(10)
_cell_angle_gamma                93.4750(10)
_cell_formula_units_Z            2
_cell_length_a                   8.34720(10)
_cell_length_b                   10.0506(2)
_cell_length_c                   16.8679(2)
_cell_measurement_temperature    203(2)
_cell_measurement_theta_max      26
_cell_measurement_theta_min      2
_cell_volume                     1384.81(4)
_computing_cell_refinement       'Siemens SMART'
_computing_data_collection       'Siemens SMART (Siemens 1995)'
_computing_data_reduction        'Siemens SMART (Siemens 1995)'
_computing_molecular_graphics    ORTEP3
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      203(2)
_diffrn_measured_fraction_theta_full 0.950
_diffrn_measured_fraction_theta_max 0.950
_diffrn_measurement_device_type  'Siemens SMART'
_diffrn_measurement_method       'area detectorω 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  0.0000
_diffrn_reflns_av_sigmaI/netI    0.0469
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_number            6022
_diffrn_reflns_theta_full        27.47
_diffrn_reflns_theta_max         27.47
_diffrn_reflns_theta_min         2.07
_diffrn_standards_decay_%        0
_exptl_absorpt_coefficient_mu    4.562
_exptl_absorpt_correction_T_max  0.7714
_exptl_absorpt_correction_T_min  0.3616
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'Blessing, 1995'
_exptl_crystal_colour            orange
_exptl_crystal_density_diffrn    1.713
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    .
_exptl_crystal_description       tablet
_exptl_crystal_F_000             696
_exptl_crystal_size_max          0.28
_exptl_crystal_size_mid          0.24
_exptl_crystal_size_min          0.06
_refine_diff_density_max         3.214
_refine_diff_density_min         -2.118
_refine_diff_density_rms         0.176
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.069
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     283
_refine_ls_number_reflns         6022
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.069
_refine_ls_R_factor_all          0.0507
_refine_ls_R_factor_gt           0.0427
_refine_ls_shift/su_max          0.025
_refine_ls_shift/su_mean         0.001
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[σ²(Fo²)+(0.0643P)²+3.2773P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1107
_refine_ls_wR_factor_ref         0.1157
_reflns_number_gt                5279
_reflns_number_total             6022
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            b006420n.txt
_cod_data_source_block           mg448
_cod_depositor_comments
;
The following automatic conversions were performed:
'_symmetry_cell_setting' value 'Triclinic' changed to 'triclinic'
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 

The following automatic conversions were performed:

'_refine_ls_weighting_scheme' value 'calc
w=1/[\s^2^(Fo^2^)+(0.0643P)^2^+3.2773P] 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^)+(0.0643P)^2^+3.2773P] where P=(Fo^2^+2Fc^2^)/3'.

Automatic conversion script
Id: cif_fix_values 3143 2015-03-26 13:38:13Z robertas 
;
_cod_original_cell_volume        1384.82(4)
_cod_original_sg_symbol_H-M      P(1-bar)
_cod_database_code               7010143
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_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
Ta Ta 0.71483(3) 0.81613(2) 0.634168(14) 0.02823(10) Uani 1 d . . .
Cl1 Cl 0.98851(18) 0.81420(17) 0.68392(10) 0.0383(3) Uani 1 d . . .
Cl2 Cl 0.7814(2) 1.00856(16) 0.57151(10) 0.0397(3) Uani 1 d . . .
Cl3 Cl 0.6519(2) 0.59362(16) 0.66479(10) 0.0395(3) Uani 1 d . . .
Cl4 Cl 0.46214(18) 0.78730(17) 0.55009(9) 0.0377(3) Uani 1 d . . .
N1 N 0.6373(6) 0.9045(6) 0.7236(3) 0.0327(11) Uani 1 d . . .
N2 N 0.8140(6) 0.6853(5) 0.5128(3) 0.0292(10) Uani 1 d . . .
C1 C 0.5442(7) 0.9475(7) 0.7886(4) 0.0329(13) Uani 1 d . . .
C2 C 0.3974(8) 0.8696(8) 0.7890(4) 0.0419(16) Uani 1 d . . .
H2A H 0.3696 0.7948 0.7471 0.050 Uiso 1 calc R . .
C3 C 0.2945(8) 0.9008(10) 0.8494(4) 0.053(2) Uani 1 d . . .
H3A H 0.1983 0.8471 0.8494 0.064 Uiso 1 calc R . .
C4 C 0.3342(9) 1.0112(10) 0.9095(4) 0.058(2) Uani 1 d . . .
H4A H 0.2629 1.0357 0.9500 0.069 Uiso 1 calc R . .
C5 C 0.4780(9) 1.0868(9) 0.9111(4) 0.051(2) Uani 1 d . . .
H5A H 0.5026 1.1606 0.9540 0.061 Uiso 1 calc R . .
C6 C 0.5894(7) 1.0598(8) 0.8525(4) 0.0382(15) Uani 1 d . . .
C7 C 0.7513(8) 1.1422(7) 0.8596(4) 0.0392(15) Uani 1 d . . .
C8 C 0.8857(8) 1.0484(8) 0.8699(4) 0.0447(17) Uani 1 d . . .
H8A H 0.8770 0.9724 0.8247 0.067 Uiso 1 calc R . .
H8B H 0.8759 1.0150 0.9199 0.067 Uiso 1 calc R . .
H8C H 0.9893 1.0984 0.8716 0.067 Uiso 1 calc R . .
C9 C 0.7675(10) 1.2600(9) 0.9337(5) 0.057(2) Uani 1 d . . .
H9A H 0.7575 1.2234 0.9827 0.085 Uiso 1 calc R . .
H9B H 0.6833 1.3210 0.9289 0.085 Uiso 1 calc R . .
H9C H 0.8718 1.3092 0.9361 0.085 Uiso 1 calc R . .
C10 C 0.7741(10) 1.2055(8) 0.7844(5) 0.0517(18) Uani 1 d . . .
H10A H 0.7633 1.1346 0.7365 0.077 Uiso 1 calc R . .
H10B H 0.8803 1.2523 0.7889 0.077 Uiso 1 calc R . .
H10C H 0.6931 1.2697 0.7804 0.077 Uiso 1 calc R . .
C11 C 0.7497(7) 0.5618(7) 0.4771(4) 0.0343(13) Uani 1 d . . .
H11A H 0.6567 0.5270 0.4975 0.041 Uiso 1 calc R . .
C12 C 0.8135(8) 0.4828(7) 0.4118(4) 0.0396(15) Uani 1 d . . .
H12A H 0.7650 0.3964 0.3888 0.048 Uiso 1 calc R . .
C13 C 0.9498(8) 0.5334(7) 0.3810(4) 0.0396(15) Uani 1 d . . .
H13A H 0.9960 0.4819 0.3370 0.048 Uiso 1 calc R . .
C14 C 1.0161(8) 0.6607(7) 0.4163(4) 0.0389(15) Uani 1 d . . .
H14A H 1.1077 0.6983 0.3962 0.047 Uiso 1 calc R . .
C15 C 0.9460(8) 0.7323(7) 0.4815(4) 0.0351(13) Uani 1 d . . .
H15A H 0.9931 0.8188 0.5054 0.042 Uiso 1 calc R . .
N3 N 0.6141(8) 0.8613(7) 0.3806(4) 0.0546(17) Uani 1 d . . .
H3B H 0.5764 0.9011 0.4252 0.066 Uiso 1 calc R . .
C16 C 0.7243(10) 0.9304(8) 0.3474(5) 0.0503(18) Uani 1 d . . .
H16A H 0.7599 1.0200 0.3717 0.060 Uiso 1 calc R . .
C17 C 0.7851(10) 0.8694(8) 0.2773(5) 0.0527(19) Uani 1 d . . .
H17A H 0.8634 0.9163 0.2529 0.063 Uiso 1 calc R . .
C18 C 0.7310(10) 0.7400(9) 0.2434(5) 0.058(2) Uani 1 d . . .
H18A H 0.7707 0.6974 0.1948 0.069 Uiso 1 calc R . .
C19 C 0.6176(10) 0.6709(9) 0.2802(5) 0.056(2) Uani 1 d . . .
H19A H 0.5819 0.5807 0.2575 0.067 Uiso 1 calc R . .
C20 C 0.5583(9) 0.7344(9) 0.3492(5) 0.0508(19) Uani 1 d . . .
H20A H 0.4792 0.6898 0.3744 0.061 Uiso 1 calc R . .
Cl5 Cl 0.1527(9) 0.3200(6) 0.0590(4) 0.207(3) Uani 1 d . . .
Cl6 Cl 0.4756(7) 0.4118(5) 0.0932(3) 0.1381(16) Uani 1 d . . .
C21 C 0.314(2) 0.3127(18) 0.1133(13) 0.146(7) Uani 1 d . . .
H21A H 0.3424 0.2182 0.1052 0.176 Uiso 1 calc R . .
H21B H 0.2929 0.3404 0.1703 0.176 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'
Cl Cl 0.1484 0.1585 '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
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
N1 Ta Cl1 98.79(16) . . ?
N1 Ta Cl2 98.56(18) . . ?
Cl1 Ta Cl2 91.15(6) . . ?
N1 Ta Cl3 94.33(18) . . ?
Cl1 Ta Cl3 91.06(6) . . ?
Cl2 Ta Cl3 166.44(6) . . ?
N1 Ta N2 177.3(2) . . ?
Cl1 Ta N2 82.07(12) . . ?
Cl2 Ta N2 83.98(12) . . ?
Cl3 Ta N2 83.07(12) . . ?
N1 Ta Cl4 96.43(16) . . ?
Cl1 Ta Cl4 164.77(5) . . ?
Cl2 Ta Cl4 86.20(6) . . ?
Cl3 Ta Cl4 88.18(6) . . ?
N2 Ta Cl4 82.74(12) . . ?
C1 N1 Ta 165.1(5) . . ?
C11 N2 C15 116.7(5) . . ?
C11 N2 Ta 123.2(4) . . ?
C15 N2 Ta 120.0(4) . . ?
N1 C1 C2 115.5(6) . . ?
N1 C1 C6 124.5(6) . . ?
C2 C1 C6 120.0(6) . . ?
C3 C2 C1 121.5(7) . . ?
C4 C3 C2 119.0(7) . . ?
C3 C4 C5 120.4(7) . . ?
C4 C5 C6 123.7(7) . . ?
C5 C6 C1 115.4(6) . . ?
C5 C6 C7 121.5(6) . . ?
C1 C6 C7 123.0(5) . . ?
C6 C7 C8 108.7(6) . . ?
C6 C7 C10 111.1(6) . . ?
C8 C7 C10 109.9(6) . . ?
C6 C7 C9 112.2(6) . . ?
C8 C7 C9 107.7(6) . . ?
C10 C7 C9 107.1(7) . . ?
N2 C11 C12 123.3(6) . . ?
C13 C12 C11 118.9(6) . . ?
C14 C13 C12 118.6(6) . . ?
C13 C14 C15 119.0(6) . . ?
N2 C15 C14 123.6(6) . . ?
C16 N3 C20 123.5(7) . . ?
N3 C16 C17 119.0(7) . . ?
C18 C17 C16 119.2(7) . . ?
C17 C18 C19 120.1(8) . . ?
C20 C19 C18 119.4(8) . . ?
N3 C20 C19 118.7(7) . . ?
Cl5 C21 Cl6 114.6(12) . . ?
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Ta N1 1.779(5) . ?
Ta Cl1 2.3910(15) . ?
Ta Cl2 2.4204(16) . ?
Ta Cl3 2.4205(16) . ?
Ta N2 2.437(5) . ?
Ta Cl4 2.4451(15) . ?
N1 C1 1.399(7) . ?
N2 C11 1.341(8) . ?
N2 C15 1.346(8) . ?
C1 C2 1.415(9) . ?
C1 C6 1.425(9) . ?
C2 C3 1.374(9) . ?
C3 C4 1.368(12) . ?
C4 C5 1.378(12) . ?
C5 C6 1.397(9) . ?
C6 C7 1.528(10) . ?
C7 C8 1.531(9) . ?
C7 C10 1.537(10) . ?
C7 C9 1.548(9) . ?
C11 C12 1.387(9) . ?
C12 C13 1.385(10) . ?
C13 C14 1.376(10) . ?
C14 C15 1.378(9) . ?
N3 C16 1.330(10) . ?
N3 C20 1.332(10) . ?
C16 C17 1.366(11) . ?
C17 C18 1.359(11) . ?
C18 C19 1.382(12) . ?
C19 C20 1.355(12) . ?
Cl5 C21 1.598(19) . ?
Cl6 C21 1.714(18) . ?
