#------------------------------------------------------------------------------
#$Date: 2025-08-19 17:49:58 +0300 (Tue, 19 Aug 2025) $
#$Revision: 301806 $
#$URL: file:///home/coder/svn-repositories/cod/cif/2/23/96/2239641.cif $
#------------------------------------------------------------------------------
#
# This file is available in the Crystallography Open Database (COD),
# http://www.crystallography.net/. The original data for this entry
# were provided by IUCr Journals, http://journals.iucr.org/.
#
# The file may be used within the scientific community so long as
# proper attribution is given to the journal article from which the
# data were obtained.
#
data_2239641
loop_
_publ_author_name
'Verma, Pratik'
'Sussman, Victor J.'
'Brennessel, William W.'
'Ellis, John E.'
_publ_section_title
;
 (η⁴-Cyclooctatetraene)(η⁸-cyclooctatetraene)iodidotantalum(V)
;
_journal_coeditor_code           LH5707
_journal_issue                   7
_journal_name_full               'Acta Crystallographica Section E'
_journal_page_first              m245
_journal_page_last               m246
_journal_paper_doi               10.1107/S1600536814012379
_journal_volume                  70
_journal_year                    2014
_chemical_formula_iupac          '[Ta (C8 H8)2 I]'
_chemical_formula_moiety         'C16 H16 I Ta'
_chemical_formula_sum            'C16 H16 I Ta'
_chemical_formula_weight         516.14
_chemical_name_common            3149
_chemical_name_systematic
;
(η⁴-Cyclooctatetraene)(η⁸-cyclooctatetraene)iodidotantalum(V)
;
_space_group_crystal_system      monoclinic
_space_group_IT_number           12
_space_group_name_Hall           '-C 2y'
_space_group_name_H-M_alt        'C 1 2/m 1'
_symmetry_space_group_name_Hall  '-C 2y'
_symmetry_space_group_name_H-M   'C 1 2/m 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-2014
_cell_angle_alpha                90
_cell_angle_beta                 113.522(2)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   14.3626(14)
_cell_length_b                   11.0200(11)
_cell_length_c                   9.3467(9)
_cell_measurement_reflns_used    937
_cell_measurement_temperature    173(2)
_cell_measurement_theta_max      27.47
_cell_measurement_theta_min      2.41
_cell_volume                     1356.4(2)
_computing_cell_refinement       'SAINT (Bruker, 2003)'
_computing_data_collection       'SMART (Bruker, 2003)'
_computing_data_reduction        'SAINT (Bruker, 2003)'
_computing_molecular_graphics    'SHELXTL (Sheldrick, 2008)'
_computing_publication_material  'SHELXTL (Sheldrick, 2008)'
_computing_structure_refinement  'SHELXL-2014 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      173(2)
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 1.000
_diffrn_measurement_device_type  'Siemens SMART CCD platform'
_diffrn_measurement_method       'ω scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0196
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_h_min       -18
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       12
_diffrn_reflns_limit_l_min       -12
_diffrn_reflns_number            8110
_diffrn_reflns_theta_full        27.485
_diffrn_reflns_theta_max         27.471
_diffrn_reflns_theta_min         2.377
_exptl_absorpt_coefficient_mu    10.358
_exptl_absorpt_correction_T_max  0.4305
_exptl_absorpt_correction_T_min  0.3177
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   '(SADABS; Sheldrick, 2012)'
_exptl_crystal_colour            red-purple
_exptl_crystal_density_diffrn    2.527
_exptl_crystal_description       block
_exptl_crystal_F_000             952
_exptl_crystal_size_max          0.10
_exptl_crystal_size_mid          0.10
_exptl_crystal_size_min          0.10
_refine_diff_density_max         1.038
_refine_diff_density_min         -0.717
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.079
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     97
_refine_ls_number_reflns         1636
_refine_ls_number_restraints     96
_refine_ls_restrained_S_all      1.079
_refine_ls_R_factor_all          0.0200
_refine_ls_R_factor_gt           0.0173
_refine_ls_shift/su_max          0.003
_refine_ls_shift/su_mean         0.001
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[σ²(Fo²)+(0.0180P)²+5.3173P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0394
_refine_ls_wR_factor_ref         0.0400
_reflns_number_gt                1520
_reflns_number_total             1636
_reflns_threshold_expression     I>2σ(I)
_cod_data_source_file            lh5707sup1.cf
_cod_data_source_block           I
_cod_database_code               2239641
_cod_database_fobs_code          2239641
#BEGIN Tags that were not found in dictionaries:
_shelx_space_group_comment
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;
_shelx_estimated_absorpt_t_min   0.424
_shelx_estimated_absorpt_t_max   0.424
_shelxl_version_number           2.014
#END Tags that were not found in dictionaries
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, y, -z'
'x+1/2, y+1/2, z'
'-x+1/2, y+1/2, -z'
'-x, -y, -z'
'x, -y, z'
'-x+1/2, -y+1/2, -z'
'x+1/2, -y+1/2, z'
loop_
_atom_site_type_symbol
_atom_site_label
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_calc_flag
_atom_site_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
Ta Ta1 0.28337(2) 0.5000 0.16766(2) 0.01915(6) Uani d 1 . .
I I1 0.26793(2) 0.5000 -0.16320(4) 0.02953(8) Uani d 1 A .
C C1 0.1203(2) 0.4365(4) 0.0278(4) 0.0312(8) Uani d 1 . .
H H1 0.1043 0.4003 -0.0715 0.037 Uiso calc 1 . .
C C2 0.1398(3) 0.3549(3) 0.1493(5) 0.0356(9) Uani d 1 . .
H H2 0.1770 0.2859 0.1413 0.043 Uiso calc 1 . .
C C3 0.1160(3) 0.3522(4) 0.2844(5) 0.0455(11) Uani d 1 . .
H H3 0.1214 0.2729 0.3271 0.055 Uiso calc 1 . .
C C4 0.0875(3) 0.4358(5) 0.3660(5) 0.0531(13) Uani d 1 . .
H H4 0.0626 0.4012 0.4371 0.064 Uiso calc 1 . .
C C5 0.4245(10) 0.3628(8) 0.2362(15) 0.039(3) Uani d 0.5 A -1
H H5 0.4396 0.2896 0.1962 0.047 Uiso calc 0.5 A -1
C C6 0.3753(8) 0.3428(9) 0.3361(12) 0.038(4) Uani d 0.5 A -1
H H6 0.3574 0.2602 0.3398 0.046 Uiso calc 0.5 A -1
C C7 0.3473(7) 0.4163(9) 0.4297(10) 0.042(2) Uani d 0.5 A -1
H H7 0.3298 0.3703 0.5013 0.050 Uiso calc 0.5 A -1
C C8 0.3375(6) 0.5382(8) 0.4486(9) 0.042(3) Uani d 0.5 A -1
H H8 0.3127 0.5560 0.5266 0.051 Uiso calc 0.5 A -1
C C9 0.3558(12) 0.6407(8) 0.3790(17) 0.039(3) Uani d 0.5 A -1
H H9 0.3318 0.7123 0.4097 0.047 Uiso calc 0.5 A -1
C C10 0.4007(7) 0.6649(8) 0.2747(12) 0.038(4) Uani d 0.5 A -1
H H10 0.4011 0.7488 0.2518 0.046 Uiso calc 0.5 A -1
C C11 0.4453(7) 0.5925(8) 0.1965(11) 0.042(2) Uani d 0.5 A -1
H H11 0.4749 0.6393 0.1400 0.050 Uiso calc 0.5 A -1
C C12 0.4570(5) 0.4667(6) 0.1811(8) 0.042(3) Uani d 0.5 A -1
H H12 0.4949 0.4481 0.1208 0.051 Uiso calc 0.5 A -1
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'
I I -0.4742 1.8119 '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_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle
C1 Ta1 C1 . 6_565 35.6(2)
C1 Ta1 C6 . . 109.2(3)
C1 Ta1 C6 6_565 . 141.1(2)
C1 Ta1 C9 . . 132.6(3)
C1 Ta1 C9 6_565 . 106.3(3)
C6 Ta1 C9 . . 89.0(3)
C1 Ta1 C5 . . 121.5(3)
C1 Ta1 C5 6_565 . 155.1(3)
C6 Ta1 C5 . . 34.1(2)
C9 Ta1 C5 . . 98.3(3)
C1 Ta1 C10 . . 148.7(2)
C1 Ta1 C10 6_565 . 113.2(2)
C6 Ta1 C10 . . 99.5(3)
C9 Ta1 C10 . . 33.7(2)
C5 Ta1 C10 . . 89.3(3)
C1 Ta1 C7 . . 110.4(3)
C1 Ta1 C7 6_565 . 125.5(2)
C6 Ta1 C7 . . 33.1(2)
C9 Ta1 C7 . . 63.2(3)
C5 Ta1 C7 . . 63.4(3)
C10 Ta1 C7 . . 87.0(3)
C1 Ta1 C11 . . 154.0(2)
C1 Ta1 C11 6_565 . 130.1(2)
C6 Ta1 C11 . . 88.8(3)
C9 Ta1 C11 . . 63.9(3)
C5 Ta1 C11 . . 64.5(3)
C10 Ta1 C11 . . 33.4(2)
C7 Ta1 C11 . . 95.0(3)
C1 Ta1 C8 . . 118.50(19)
C1 Ta1 C8 6_565 . 111.9(2)
C6 Ta1 C8 . . 63.8(3)
C9 Ta1 C8 . . 33.0(2)
C5 Ta1 C8 . . 87.1(3)
C10 Ta1 C8 . . 63.7(3)
C7 Ta1 C8 . . 32.5(2)
C11 Ta1 C8 . . 86.0(3)
C1 Ta1 C12 . . 139.89(19)
C1 Ta1 C12 6_565 . 148.81(18)
C6 Ta1 C12 . . 64.7(2)
C9 Ta1 C12 . . 87.5(4)
C5 Ta1 C12 . . 33.6(2)
C10 Ta1 C12 . . 64.3(3)
C7 Ta1 C12 . . 85.7(3)
C11 Ta1 C12 . . 33.2(2)
C8 Ta1 C12 . . 95.1(2)
C1 Ta1 C2 . . 32.60(13)
C1 Ta1 C2 6_565 . 62.58(13)
C6 Ta1 C2 . . 78.9(2)
C9 Ta1 C2 . . 122.1(2)
C5 Ta1 C2 . . 101.3(2)
C10 Ta1 C2 . . 155.6(2)
C7 Ta1 C2 . . 78.5(3)
C11 Ta1 C2 . . 165.8(2)
C8 Ta1 C2 . . 94.66(19)
C12 Ta1 C2 . . 132.81(18)
C1 Ta1 C2 . 6_565 62.58(13)
C1 Ta1 C2 6_565 6_565 32.60(13)
C6 Ta1 C2 . 6_565 136.4(2)
C9 Ta1 C2 . 6_565 74.0(3)
C5 Ta1 C2 . 6_565 169.2(3)
C10 Ta1 C2 . 6_565 88.2(2)
C7 Ta1 C2 . 6_565 106.0(2)
C11 Ta1 C2 . 6_565 116.8(2)
C8 Ta1 C2 . 6_565 82.4(2)
C12 Ta1 C2 . 6_565 149.84(18)
C2 Ta1 C2 . 6_565 77.28(17)
C1 Ta1 I1 . . 76.97(9)
C1 Ta1 I1 6_565 . 76.97(9)
C6 Ta1 I1 . . 118.5(2)
C9 Ta1 I1 . . 132.5(2)
C5 Ta1 I1 . . 89.0(3)
C10 Ta1 I1 . . 100.3(2)
C7 Ta1 I1 . . 151.54(19)
C11 Ta1 I1 . . 77.9(2)
C8 Ta1 I1 . . 163.56(16)
C12 Ta1 I1 . . 73.25(16)
C2 Ta1 I1 . . 101.77(9)
C2 Ta1 I1 6_565 . 101.77(9)
C2 C1 C1 . 6_565 130.4(2)
C2 C1 Ta1 . . 84.5(2)
C1 C1 Ta1 6_565 . 72.20(10)
C2 C1 H1 . . 114.8
C1 C1 H1 6_565 . 114.8
Ta1 C1 H1 . . 118.6
C1 C2 C3 . . 133.9(4)
C1 C2 Ta1 . . 62.89(19)
C3 C2 Ta1 . . 115.0(2)
C1 C2 H2 . . 113.0
C3 C2 H2 . . 113.0
Ta1 C2 H2 . . 92.4
C4 C3 C2 . . 135.3(4)
C4 C3 H3 . . 112.4
C2 C3 H3 . . 112.4
C3 C4 C4 . 6_565 132.7(3)
C3 C4 H4 . . 113.7
C4 C4 H4 6_565 . 113.7
C6 C5 C12 . . 134.7(8)
C6 C5 Ta1 . . 71.3(5)
C12 C5 Ta1 . . 76.0(6)
C6 C5 H5 . . 112.7
C12 C5 H5 . . 112.7
Ta1 C5 H5 . . 136.9
C7 C6 C5 . . 133.8(8)
C7 C6 Ta1 . . 76.2(6)
C5 C6 Ta1 . . 74.6(6)
C7 C6 H6 . . 113.1
C5 C6 H6 . . 113.1
Ta1 C6 H6 . . 129.8
C6 C7 C8 . . 137.5(9)
C6 C7 Ta1 . . 70.7(6)
C8 C7 Ta1 . . 75.0(6)
C6 C7 H7 . . 111.3
C8 C7 H7 . . 111.3
Ta1 C7 H7 . . 144.5
C7 C8 C9 . . 133.9(9)
C7 C8 Ta1 . . 72.5(6)
C9 C8 Ta1 . . 71.0(6)
C7 C8 H8 . . 113.1
C9 C8 H8 . . 113.1
Ta1 C8 H8 . . 143.0
C8 C9 C10 . . 135.7(8)
C8 C9 Ta1 . . 76.0(6)
C10 C9 Ta1 . . 73.6(6)
C8 C9 H9 . . 112.2
C10 C9 H9 . . 112.2
Ta1 C9 H9 . . 134.1
C9 C10 C11 . . 133.9(9)
C9 C10 Ta1 . . 72.7(6)
C11 C10 Ta1 . . 75.1(6)
C9 C10 H10 . . 113.0
C11 C10 H10 . . 113.0
Ta1 C10 H10 . . 135.0
C10 C11 C12 . . 135.4(8)
C10 C11 Ta1 . . 71.5(5)
C12 C11 Ta1 . . 74.2(5)
C10 C11 H11 . . 112.3
C12 C11 H11 . . 112.3
Ta1 C11 H11 . . 141.1
C11 C12 C5 . . 133.7(8)
C11 C12 Ta1 . . 72.6(5)
C5 C12 Ta1 . . 70.4(6)
C11 C12 H12 . . 113.1
C5 C12 H12 . . 113.1
Ta1 C12 H12 . . 143.8
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_site_symmetry_2
_geom_bond_distance
Ta1 C1 . 2.290(3)
Ta1 C1 6_565 2.290(3)
Ta1 C6 . 2.359(10)
Ta1 C9 . 2.397(13)
Ta1 C5 . 2.402(12)
Ta1 C10 . 2.408(9)
Ta1 C7 . 2.429(9)
Ta1 C11 . 2.454(9)
Ta1 C8 . 2.459(8)
Ta1 C12 . 2.474(7)
Ta1 C2 . 2.560(4)
Ta1 C2 6_565 2.560(4)
Ta1 I1 . 3.0107(5)
C1 C2 . 1.386(5)
C1 C1 6_565 1.400(8)
C1 H1 . 0.9500
C2 C3 . 1.435(6)
C2 H2 . 0.9500
C3 C4 . 1.359(7)
C3 H3 . 0.9500
C4 C4 6_565 1.416(11)
C4 H4 . 0.9500
C5 C6 . 1.396(9)
C5 C12 . 1.410(9)
C5 H5 . 0.9500
C6 C7 . 1.365(9)
C6 H6 . 0.9500
C7 C8 . 1.369(9)
C7 H7 . 0.9500
C8 C9 . 1.381(9)
C8 H8 . 0.9500
C9 C10 . 1.392(9)
C9 H9 . 0.9500
C10 C11 . 1.399(9)
C10 H10 . 0.9500
C11 C12 . 1.410(9)
C11 H11 . 0.9500
C12 H12 . 0.9500
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_site_symmetry_1
_geom_torsion_site_symmetry_4
_geom_torsion
C1 C1 C2 C3 6_565 . 38.6(5)
Ta1 C1 C2 C3 . . 99.6(4)
C1 C1 C2 Ta1 6_565 . -60.97(17)
C1 C2 C3 C4 . . -18.5(8)
Ta1 C2 C3 C4 . . 57.1(5)
C2 C3 C4 C4 . 6_565 -13.5(6)
C12 C5 C6 C7 . . -7(2)
Ta1 C5 C6 C7 . . -52.8(12)
C12 C5 C6 Ta1 . . 46.1(13)
C5 C6 C7 C8 . . 14(2)
Ta1 C6 C7 C8 . . -37.9(15)
C5 C6 C7 Ta1 . . 52.2(12)
C6 C7 C8 C9 . . -2(3)
Ta1 C7 C8 C9 . . -39.1(15)
C6 C7 C8 Ta1 . . 36.9(15)
C7 C8 C9 C10 . . -8(3)
Ta1 C8 C9 C10 . . -47.7(16)
C7 C8 C9 Ta1 . . 39.5(14)
C8 C9 C10 C11 . . 1(2)
Ta1 C9 C10 C11 . . -47.7(12)
C8 C9 C10 Ta1 . . 48.4(16)
C9 C10 C11 C12 . . 6(2)
Ta1 C10 C11 C12 . . -41.4(14)
C9 C10 C11 Ta1 . . 47.0(12)
C10 C11 C12 C5 . . 3(2)
Ta1 C11 C12 C5 . . -38.2(13)
C10 C11 C12 Ta1 . . 40.7(14)
C6 C5 C12 C11 . . -6(2)
Ta1 C5 C12 C11 . . 38.8(13)
C6 C5 C12 Ta1 . . -44.7(13)
loop_
_cod_related_entry_id
_cod_related_entry_database
_cod_related_entry_code
1 PubChem 139086719
