#------------------------------------------------------------------------------
#$Date: 2025-08-20 15:06:16 +0200 (Wed 20 de Aug de 2025) $
#$Revision: 301830 $
#$URL: svn://www.crystallography.net/cod/cif/4/07/73/4077395.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_4077395
loop_
_publ_author_name
'Bazinet, Patrick'
'Yap, Glenn P. A.'
'Richeson, Darrin S.'
_publ_section_title
;
 Metallaaziridine Complexes of Tantalum Derived from
 1,8-Bis(isopropylamino)naphthalene via β-H Activation
;
_journal_issue                   20
_journal_name_full               Organometallics
_journal_page_first              4129
_journal_paper_doi               10.1021/om0105167
_journal_volume                  20
_journal_year                    2001
_chemical_formula_sum            'C44 H50 Cl4 N4 Ta2'
_chemical_formula_weight         1138.58
_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                110.555(2)
_cell_angle_beta                 95.041(2)
_cell_angle_gamma                95.855(2)
_cell_formula_units_Z            1
_cell_length_a                   9.085(1)
_cell_length_b                   9.529(1)
_cell_length_c                   13.481(2)
_cell_measurement_reflns_used    'reflections from 60 data frames'
_cell_measurement_temperature    203(2)
_cell_measurement_theta_max      28.29
_cell_measurement_theta_min      1.47
_cell_volume                     1077.4(2)
_computing_cell_refinement       'Bruker SMART'
_computing_data_collection       'Bruker SMART'
_computing_data_reduction        'Bruker SHELXTL'
_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      203(2)
_diffrn_measured_fraction_theta_full 0.871
_diffrn_measured_fraction_theta_max 0.871
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       'phi and omega 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  0.0328
_diffrn_reflns_av_sigmaI/netI    0.0596
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_number            8474
_diffrn_reflns_theta_full        28.78
_diffrn_reflns_theta_max         28.78
_diffrn_reflns_theta_min         1.63
_diffrn_standards_decay_%        <1
_diffrn_standards_number         '50 standard frames at start and end'
_exptl_absorpt_coefficient_mu    5.358
_exptl_absorpt_correction_T_max  0.928076
_exptl_absorpt_correction_T_min  0.619401
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'Blessing,R., Acta Cryst. (1995) A51 33-38.'
_exptl_crystal_colour            orange
_exptl_crystal_density_diffrn    1.755
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             556
_exptl_crystal_size_max          0.20
_exptl_crystal_size_mid          0.15
_exptl_crystal_size_min          0.10
_refine_diff_density_max         0.876
_refine_diff_density_min         -1.187
_refine_diff_density_rms         0.114
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.005
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     262
_refine_ls_number_reflns         4897
_refine_ls_number_restraints     4
_refine_ls_restrained_S_all      1.006
_refine_ls_R_factor_all          0.0453
_refine_ls_R_factor_gt           0.0355
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[σ²(Fo²)+(0.0200P)²+0.0000P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0650
_refine_ls_wR_factor_ref         0.0662
_reflns_number_gt                4023
_reflns_number_total             4897
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            om0105167.cif
_cod_data_source_block           dr229
_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 2.4.2 from 2011-04-26.

Automatic conversion script
Id: cif_fix_values 1715 2011-07-08 13:25:40Z adriana 
;
_cod_original_sg_symbol_H-M      P-1
_cod_database_code               4077395
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 0.03417(2) 0.17764(2) 0.138395(14) 0.03947(7) Uani 1 1 d D . .
Cl1 Cl 0.2361(11) 0.3649(12) 0.1601(9) 0.077(3) Uani 0.50 1 d PD A 1
Cl2 Cl -0.0928(5) -0.0833(3) 0.0591(3) 0.0672(11) Uani 0.50 1 d PD . 1
Cl1' Cl 0.2000(12) 0.3834(12) 0.1381(10) 0.078(3) Uani 0.50 1 d PD A 2
Cl2' Cl -0.1535(3) -0.0411(3) 0.0351(2) 0.0470(8) Uani 0.50 1 d PD . 2
N1 N 0.0705(4) 0.1610(5) 0.2753(3) 0.0542(11) Uani 1 1 d D A .
N2 N -0.1166(4) 0.2905(5) 0.2052(3) 0.0472(10) Uani 1 1 d D A .
C1 C 0.0185(5) 0.2084(6) 0.3754(4) 0.0514(13) Uani 1 1 d . . .
C2 C 0.0763(7) 0.1713(11) 0.4575(5) 0.104(3) Uani 1 1 d . A .
H2A H 0.1526 0.1100 0.4477 0.124 Uiso 1 1 calc R . .
C3 C 0.0237(8) 0.2234(11) 0.5569(5) 0.106(3) Uani 1 1 d . . .
H3A H 0.0655 0.1969 0.6130 0.127 Uiso 1 1 calc R A .
C4 C -0.0859(6) 0.3108(7) 0.5731(4) 0.0614(15) Uani 1 1 d . A .
H4A H -0.1194 0.3455 0.6404 0.074 Uiso 1 1 calc R . .
C5 C -0.1493(5) 0.3495(5) 0.4910(3) 0.0433(11) Uani 1 1 d . . .
C6 C -0.0987(4) 0.2986(5) 0.3884(3) 0.0369(10) Uani 1 1 d . A .
C7 C -0.1693(6) 0.3386(6) 0.3055(4) 0.0496(12) Uani 1 1 d . . .
C8 C -0.2815(9) 0.4256(9) 0.3261(5) 0.098(3) Uani 1 1 d . A .
H8A H -0.3282 0.4518 0.2713 0.117 Uiso 1 1 calc R . .
C9 C -0.3280(10) 0.4761(10) 0.4268(6) 0.114(3) Uani 1 1 d . . .
H9A H -0.4057 0.5356 0.4391 0.137 Uiso 1 1 calc R A .
C10 C -0.2628(7) 0.4404(7) 0.5075(5) 0.0666(16) Uani 1 1 d . A .
H10A H -0.2943 0.4773 0.5754 0.080 Uiso 1 1 calc R . .
C11 C 0.1867(9) 0.0679(11) 0.2398(6) 0.112(3) Uani 1 1 d D A .
H11A H 0.1842 0.0604 0.1645 0.134 Uiso 0.50 1 calc PR B 1
C12 C 0.1481(13) -0.0962(12) 0.2272(9) 0.174(6) Uani 1 1 d . . .
H12A H 0.0455 -0.1326 0.1939 0.261 Uiso 1 1 calc R A .
H12B H 0.1597 -0.1048 0.2970 0.261 Uiso 1 1 calc R . .
H12C H 0.2142 -0.1563 0.1828 0.261 Uiso 1 1 calc R . .
C13 C 0.3439(9) 0.1484(17) 0.2876(9) 0.183(6) Uani 1 1 d . . .
H13A H 0.3520 0.2517 0.2896 0.275 Uiso 1 1 calc R A .
H13B H 0.4151 0.0958 0.2440 0.275 Uiso 1 1 calc R . .
H13C H 0.3649 0.1491 0.3595 0.275 Uiso 1 1 calc R . .
C14 C -0.1705(8) 0.3113(11) 0.1105(5) 0.103(3) Uani 1 1 d D A .
H14A H -0.1086 0.2556 0.0571 0.123 Uiso 0.50 1 calc PR C 2
C15 C -0.3297(10) 0.2374(17) 0.0629(7) 0.187(7) Uani 1 1 d . . .
H15A H -0.3427 0.1337 0.0602 0.281 Uiso 1 1 calc R A .
H15B H -0.3493 0.2380 -0.0089 0.281 Uiso 1 1 calc R . .
H15C H -0.3988 0.2933 0.1069 0.281 Uiso 1 1 calc R . .
C16 C -0.1386(14) 0.4788(15) 0.1162(9) 0.187(6) Uani 1 1 d . . .
H16A H -0.0356 0.5198 0.1463 0.281 Uiso 1 1 calc R A .
H16B H -0.2043 0.5392 0.1610 0.281 Uiso 1 1 calc R . .
H16C H -0.1562 0.4813 0.0449 0.281 Uiso 1 1 calc R . .
C17 C -0.4526(7) -0.1646(7) 0.3820(5) 0.0660(16) Uani 1 1 d . . .
H17A H -0.4735 -0.1509 0.4516 0.079 Uiso 1 1 calc R . .
C18 C -0.5222(6) -0.2885(7) 0.2970(4) 0.0594(14) Uani 1 1 d . . .
H18A H -0.5916 -0.3599 0.3080 0.071 Uiso 1 1 calc R . .
C19 C -0.4905(6) -0.3081(6) 0.1956(4) 0.0582(14) Uani 1 1 d . . .
H19A H -0.5381 -0.3932 0.1373 0.070 Uiso 1 1 calc R . .
C20 C -0.3902(6) -0.2045(6) 0.1797(5) 0.0617(15) Uani 1 1 d . . .
H20A H -0.3685 -0.2188 0.1102 0.074 Uiso 1 1 calc R . .
C21 C -0.3210(5) -0.0806(6) 0.2632(4) 0.0576(14) Uani 1 1 d . . .
H21A H -0.2526 -0.0092 0.2513 0.069 Uiso 1 1 calc R . .
C22 C -0.3511(6) -0.0599(6) 0.3644(5) 0.0605(14) Uani 1 1 d . . .
H22A H -0.3029 0.0255 0.4223 0.073 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'
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
N1 Ta N2 81.64(16) . .
N1 Ta Cl1 97.9(3) . .
N2 Ta Cl1 103.7(4) . .
N1 Ta Cl1' 107.9(3) . .
N2 Ta Cl1' 97.5(4) . .
Cl1 Ta Cl1' 12.4(5) . .
N1 Ta C11 36.96(17) . .
N2 Ta C11 118.57(18) . .
Cl1 Ta C11 89.9(4) . .
Cl1' Ta C11 102.3(4) . .
N1 Ta C14 117.07(18) . .
N2 Ta C14 35.49(18) . .
Cl1 Ta C14 99.4(4) . .
Cl1' Ta C14 88.2(4) . .
C11 Ta C14 153.9(2) . .
N1 Ta Cl2 91.53(17) . .
N2 Ta Cl2 103.87(16) . .
Cl1 Ta Cl2 151.9(4) . .
Cl1' Ta Cl2 153.0(4) . .
C11 Ta Cl2 81.8(3) . .
C14 Ta Cl2 99.7(3) . .
N1 Ta Cl2' 104.46(16) . .
N2 Ta Cl2' 91.37(14) . .
Cl1 Ta Cl2' 154.7(3) . .
Cl1' Ta Cl2' 147.4(3) . .
C11 Ta Cl2' 100.8(3) . .
C14 Ta Cl2' 81.0(2) . .
Cl2 Ta Cl2' 19.32(10) . .
N1 Ta Cl2 145.77(16) . 2
N2 Ta Cl2 131.89(16) . 2
Cl1 Ta Cl2 82.1(3) . 2
Cl1' Ta Cl2 78.1(3) . 2
C11 Ta Cl2 109.03(17) . 2
C14 Ta Cl2 96.48(18) . 2
Cl2 Ta Cl2 75.39(11) . 2
Cl2' Ta Cl2 72.69(8) . 2
N1 Ta Cl2' 127.87(14) . 2
N2 Ta Cl2' 149.75(14) . 2
Cl1 Ta Cl2' 80.9(3) . 2
Cl1' Ta Cl2' 80.8(4) . 2
C11 Ta Cl2' 91.04(16) . 2
C14 Ta Cl2' 114.46(17) . 2
Cl2 Ta Cl2' 72.47(8) . 2
Cl2' Ta Cl2' 76.02(10) . 2
Cl2 Ta Cl2' 18.01(9) 2 2
Ta Cl2 Ta 104.61(11) . 2
Ta Cl2' Ta 103.98(10) . 2
C1 N1 C11 129.0(4) . .
C1 N1 Ta 140.1(3) . .
C11 N1 Ta 90.9(3) . .
C14 N2 C7 128.9(4) . .
C14 N2 Ta 92.5(3) . .
C7 N2 Ta 138.6(3) . .
C2 C1 N1 122.4(5) . .
C2 C1 C6 120.3(5) . .
N1 C1 C6 117.4(4) . .
C1 C2 C3 120.8(6) . .
C4 C3 C2 120.9(6) . .
C3 C4 C5 120.2(5) . .
C4 C5 C10 120.4(4) . .
C4 C5 C6 120.6(5) . .
C10 C5 C6 119.0(5) . .
C1 C6 C7 124.0(4) . .
C1 C6 C5 117.3(4) . .
C7 C6 C5 118.7(4) . .
C8 C7 N2 122.2(5) . .
C8 C7 C6 119.5(4) . .
N2 C7 C6 118.3(4) . .
C7 C8 C9 121.1(6) . .
C10 C9 C8 120.8(6) . .
C9 C10 C5 120.8(5) . .
N1 C11 C12 114.7(7) . .
N1 C11 C13 113.9(8) . .
C12 C11 C13 119.0(8) . .
N1 C11 Ta 52.2(2) . .
C12 C11 Ta 120.4(7) . .
C13 C11 Ta 117.9(7) . .
N2 C14 C15 115.4(7) . .
N2 C14 C16 113.9(8) . .
C15 C14 C16 113.0(8) . .
N2 C14 Ta 52.0(2) . .
C15 C14 Ta 125.2(8) . .
C16 C14 Ta 120.4(6) . .
C18 C17 C22 119.3(5) . .
C19 C18 C17 120.0(5) . .
C18 C19 C20 120.0(5) . .
C21 C20 C19 120.7(5) . .
C20 C21 C22 119.9(5) . .
C17 C22 C21 120.1(5) . .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
Ta N1 1.911(3) .
Ta N2 1.918(3) .
Ta Cl1 2.347(3) .
Ta Cl1' 2.348(3) .
Ta C11 2.418(6) .
Ta C14 2.432(6) .
Ta Cl2 2.446(3) .
Ta Cl2' 2.451(2) .
Ta Cl2 2.617(3) 2
Ta Cl2' 2.634(3) 2
Cl2 Ta 2.617(3) 2
Cl2' Ta 2.634(3) 2
N1 C1 1.405(5) .
N1 C11 1.454(6) .
N2 C14 1.413(7) .
N2 C7 1.411(5) .
C1 C2 1.356(8) .
C1 C6 1.420(6) .
C2 C3 1.401(8) .
C3 C4 1.346(8) .
C4 C5 1.383(7) .
C5 C10 1.396(7) .
C5 C6 1.430(5) .
C6 C7 1.424(7) .
C7 C8 1.366(7) .
C8 C9 1.392(8) .
C9 C10 1.355(9) .
C11 C12 1.512(12) .
C11 C13 1.520(13) .
C14 C15 1.521(11) .
C14 C16 1.567(14) .
C17 C18 1.370(8) .
C17 C22 1.385(8) .
C18 C19 1.373(7) .
C19 C20 1.360(7) .
C20 C21 1.359(7) .
C21 C22 1.365(7) .
loop_
_cod_related_entry_id
_cod_related_entry_database
_cod_related_entry_code
1 PubChem 139106587
