#------------------------------------------------------------------------------
#$Date: 2016-02-21 02:03:34 +0200 (Sun, 21 Feb 2016) $
#$Revision: 176798 $
#$URL: svn://www.crystallography.net/cod/cif/2/23/49/2234934.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_2234934
loop_
_publ_author_name
'Yu, Gang'
'Zhan, Shu-Zhong'
'Ng, Seik Weng'
_publ_section_title
;
 Tris[(2E)-1,3-bis(4-chlorophenyl)triaz-2-en-1-ido-κ²N¹,N³]cobalt(III)
;
_journal_coeditor_code           BT5911
_journal_issue                   6
_journal_name_full               'Acta Crystallographica Section E'
_journal_page_first              m758
_journal_paper_doi               10.1107/S1600536812020569
_journal_volume                  68
_journal_year                    2012
_chemical_formula_iupac          '[Co (C12 H8 Cl2 N3)3]'
_chemical_formula_moiety         'C36 H24 Cl6 Co N9'
_chemical_formula_sum            'C36 H24 Cl6 Co N9'
_chemical_formula_weight         854.27
_chemical_name_systematic
;
Tris[(2E)-1,3-bis(4-chlorophenyl)triaz-2-en-1-ido-
κ²N¹,N³]cobalt(III)
;
_space_group_IT_number           148
_symmetry_cell_setting           trigonal
_symmetry_space_group_name_Hall  '-R 3'
_symmetry_space_group_name_H-M   'R -3 :H'
_atom_sites_solution_hydrogens   difmap
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                120.00
_cell_formula_units_Z            6
_cell_length_a                   19.383(3)
_cell_length_b                   19.383
_cell_length_c                   17.546(2)
_cell_measurement_reflns_used    1211
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      22.09
_cell_measurement_theta_min      2.62
_cell_volume                     5708.9(11)
_computing_cell_refinement       'SAINT (Bruker, 2005)'
_computing_data_collection       'APEX2 (Bruker, 2005)'
_computing_data_reduction        'SAINT (Bruker, 2005)'
_computing_molecular_graphics    'X-SEED (Barbour, 2001)'
_computing_publication_material  'publCIF (Westrip, 2010)'
_computing_structure_refinement  'SHELXL97 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 0.993
_diffrn_measured_fraction_theta_max 0.993
_diffrn_measurement_device_type  'Bruker SMART APEX'
_diffrn_measurement_method       '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  0.0531
_diffrn_reflns_av_sigmaI/netI    0.0728
_diffrn_reflns_limit_h_max       20
_diffrn_reflns_limit_h_min       -24
_diffrn_reflns_limit_k_max       22
_diffrn_reflns_limit_k_min       -24
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_number            8131
_diffrn_reflns_theta_full        27.48
_diffrn_reflns_theta_max         27.48
_diffrn_reflns_theta_min         1.68
_diffrn_standards_decay_%        0
_diffrn_standards_interval_count 0
_diffrn_standards_interval_time  0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.913
_exptl_absorpt_correction_T_max  0.8385
_exptl_absorpt_correction_T_min  0.7714
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   '(SADABS; Sheldrick, 1996)'
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    1.491
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             2592
_exptl_crystal_size_max          0.30
_exptl_crystal_size_mid          0.25
_exptl_crystal_size_min          0.20
_refine_diff_density_max         0.349
_refine_diff_density_min         -0.339
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.040
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     157
_refine_ls_number_reflns         2891
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.040
_refine_ls_R_factor_all          0.1085
_refine_ls_R_factor_gt           0.0531
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.001
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[σ²(Fo²)+(0.0758P)²+0.3669P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1276
_refine_ls_wR_factor_ref         0.1590
_reflns_number_gt                1714
_reflns_number_total             2891
_reflns_threshold_expression     I>2σ(I)
_cod_data_source_file            bt5911.cif
_cod_data_source_block           I
_cod_original_cell_volume        5708.5(10)
_cod_original_sg_symbol_H-M      'R -3'
_cod_database_code               2234934
_cod_database_fobs_code          2234934
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-y, x-y, z'
'-x+y, -x, z'
'x+2/3, y+1/3, z+1/3'
'-y+2/3, x-y+1/3, z+1/3'
'-x+y+2/3, -x+1/3, z+1/3'
'x+1/3, y+2/3, z+2/3'
'-y+1/3, x-y+2/3, z+2/3'
'-x+y+1/3, -x+2/3, z+2/3'
'-x, -y, -z'
'y, -x+y, -z'
'x-y, x, -z'
'-x+2/3, -y+1/3, -z+1/3'
'y+2/3, -x+y+1/3, -z+1/3'
'x-y+2/3, x+1/3, -z+1/3'
'-x+1/3, -y+2/3, -z+2/3'
'y+1/3, -x+y+2/3, -z+2/3'
'x-y+1/3, x+2/3, -z+2/3'
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_refinement_flags
_atom_site_occupancy
_atom_site_symmetry_multiplicity
Co Co1 0.0000 0.0000 0.25642(4) 0.0361(3) Uani d S 1 3
Cl Cl1 -0.04587(9) 0.28231(8) 0.51099(7) 0.0835(5) Uani d . 1 1
Cl Cl2 0.34023(9) 0.12548(9) -0.01594(8) 0.0937(5) Uani d . 1 1
C C1 0.0269(2) 0.1483(2) 0.35169(17) 0.0349(8) Uani d . 1 1
C C2 -0.0262(2) 0.1092(2) 0.41122(18) 0.0402(8) Uani d . 1 1
H H2 -0.0473 0.0547 0.4178 0.048 Uiso calc R 1 1
C C3 -0.0476(2) 0.1507(2) 0.46038(19) 0.0441(9) Uani d . 1 1
H H3 -0.0830 0.1245 0.5001 0.053 Uiso calc R 1 1
C C4 -0.0162(2) 0.2313(2) 0.4501(2) 0.0477(10) Uani d . 1 1
C C5 0.0370(3) 0.2714(2) 0.3925(2) 0.0581(11) Uani d . 1 1
H H5 0.0586 0.3261 0.3871 0.070 Uiso calc R 1 1
C C6 0.0582(2) 0.2301(2) 0.3430(2) 0.0486(10) Uani d . 1 1
H H6 0.0935 0.2569 0.3034 0.058 Uiso calc R 1 1
C C7 0.1553(2) 0.0949(2) 0.15565(17) 0.0368(8) Uani d . 1 1
C C8 0.1422(3) 0.0343(3) 0.1071(2) 0.0630(12) Uani d . 1 1
H H8 0.0949 -0.0142 0.1102 0.076 Uiso calc R 1 1
C C9 0.1988(3) 0.0447(3) 0.0536(3) 0.0725(14) Uani d . 1 1
H H9 0.1893 0.0033 0.0205 0.087 Uiso calc R 1 1
C C10 0.2671(3) 0.1136(3) 0.0490(2) 0.0547(11) Uani d . 1 1
C C11 0.2815(2) 0.1764(3) 0.0959(2) 0.0561(11) Uani d . 1 1
H H11 0.3288 0.2247 0.0914 0.067 Uiso calc R 1 1
C C12 0.2254(2) 0.1673(2) 0.1496(2) 0.0485(10) Uani d . 1 1
H H12 0.2347 0.2094 0.1815 0.058 Uiso calc R 1 1
N N1 0.04549(18) 0.10269(17) 0.30269(15) 0.0398(7) Uani d . 1 1
N N2 0.10592(17) 0.13926(18) 0.25527(15) 0.0407(7) Uani d . 1 1
N N3 0.09691(17) 0.08162(18) 0.21030(15) 0.0387(7) Uani d . 1 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'
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'
Co Co 0.3494 0.9721 '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
N1 Co1 N1 . 3 103.22(10)
N1 Co1 N1 . 2 103.22(10)
N1 Co1 N1 3 2 103.22(10)
N1 Co1 N3 . 3 163.88(12)
N1 Co1 N3 3 3 64.54(12)
N1 Co1 N3 2 3 90.28(12)
N1 Co1 N3 . . 64.54(12)
N1 Co1 N3 3 . 90.28(12)
N1 Co1 N3 2 . 163.88(12)
N3 Co1 N3 3 . 103.63(10)
N1 Co1 N3 . 2 90.28(12)
N1 Co1 N3 3 2 163.88(12)
N1 Co1 N3 2 2 64.54(12)
N3 Co1 N3 3 2 103.63(10)
N3 Co1 N3 . 2 103.63(10)
N1 Co1 N2 . 2 98.78(11)
N1 Co1 N2 3 2 134.58(11)
N1 Co1 N2 2 2 32.42(10)
N3 Co1 N2 3 2 97.33(11)
N3 Co1 N2 . 2 135.13(11)
N3 Co1 N2 2 2 32.14(10)
N1 Co1 N2 . 3 134.58(11)
N1 Co1 N2 3 3 32.42(10)
N1 Co1 N2 2 3 98.78(11)
N3 Co1 N2 3 3 32.14(10)
N3 Co1 N2 . 3 97.33(11)
N3 Co1 N2 2 3 135.13(11)
N2 Co1 N2 2 3 119.993(4)
C2 C1 C6 . . 118.9(3)
C2 C1 N1 . . 118.0(3)
C6 C1 N1 . . 123.1(3)
C3 C2 C1 . . 120.5(3)
C3 C2 H2 . . 119.7
C1 C2 H2 . . 119.7
C4 C3 C2 . . 119.3(3)
C4 C3 H3 . . 120.3
C2 C3 H3 . . 120.3
C5 C4 C3 . . 121.3(3)
C5 C4 Cl1 . . 120.0(3)
C3 C4 Cl1 . . 118.7(3)
C4 C5 C6 . . 119.6(4)
C4 C5 H5 . . 120.2
C6 C5 H5 . . 120.2
C5 C6 C1 . . 120.3(3)
C5 C6 H6 . . 119.8
C1 C6 H6 . . 119.8
C8 C7 C12 . . 119.3(3)
C8 C7 N3 . . 118.7(3)
C12 C7 N3 . . 122.0(3)
C7 C8 C9 . . 120.3(4)
C7 C8 H8 . . 119.8
C9 C8 H8 . . 119.8
C10 C9 C8 . . 120.4(4)
C10 C9 H9 . . 119.8
C8 C9 H9 . . 119.8
C9 C10 C11 . . 120.7(4)
C9 C10 Cl2 . . 120.5(4)
C11 C10 Cl2 . . 118.8(3)
C10 C11 C12 . . 119.7(4)
C10 C11 H11 . . 120.1
C12 C11 H11 . . 120.1
C11 C12 C7 . . 119.5(4)
C11 C12 H12 . . 120.3
C7 C12 H12 . . 120.3
N2 N1 C1 . . 119.2(3)
N2 N1 Co1 . . 96.6(2)
C1 N1 Co1 . . 141.9(2)
N3 N2 N1 . . 102.6(3)
N2 N3 C7 . . 120.3(3)
N2 N3 Co1 . . 96.14(19)
C7 N3 Co1 . . 143.3(3)
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_site_symmetry_2
_geom_bond_distance
Co1 N1 . 1.909(3)
Co1 N1 3 1.909(3)
Co1 N1 2 1.909(3)
Co1 N3 3 1.927(3)
Co1 N3 . 1.927(3)
Co1 N3 2 1.927(3)
Co1 N2 2 2.441(3)
Co1 N2 3 2.441(3)
Cl1 C4 . 1.737(4)
Cl2 C10 . 1.741(4)
C1 C2 . 1.394(4)
C1 C6 . 1.395(5)
C1 N1 . 1.403(4)
C2 C3 . 1.378(5)
C2 H2 . 0.9300
C3 C4 . 1.376(5)
C3 H3 . 0.9300
C4 C5 . 1.373(5)
C5 C6 . 1.376(5)
C5 H5 . 0.9300
C6 H6 . 0.9300
C7 C8 . 1.368(5)
C7 C12 . 1.386(5)
C7 N3 . 1.406(4)
C8 C9 . 1.381(6)
C8 H8 . 0.9300
C9 C10 . 1.332(6)
C9 H9 . 0.9300
C10 C11 . 1.377(6)
C11 C12 . 1.382(5)
C11 H11 . 0.9300
C12 H12 . 0.9300
N1 N2 . 1.318(4)
N2 N3 . 1.306(4)
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
C6 C1 C2 C3 . 0.3(5)
N1 C1 C2 C3 . -179.0(3)
C1 C2 C3 C4 . 0.1(5)
C2 C3 C4 C5 . -1.0(6)
C2 C3 C4 Cl1 . 178.3(3)
C3 C4 C5 C6 . 1.4(6)
Cl1 C4 C5 C6 . -177.8(3)
C4 C5 C6 C1 . -1.0(6)
C2 C1 C6 C5 . 0.2(6)
N1 C1 C6 C5 . 179.4(4)
C12 C7 C8 C9 . 1.1(6)
N3 C7 C8 C9 . -178.9(4)
C7 C8 C9 C10 . 0.5(8)
C8 C9 C10 C11 . -1.9(8)
C8 C9 C10 Cl2 . 177.4(4)
C9 C10 C11 C12 . 1.6(7)
Cl2 C10 C11 C12 . -177.7(3)
C10 C11 C12 C7 . 0.1(6)
C8 C7 C12 C11 . -1.4(6)
N3 C7 C12 C11 . 178.6(3)
C2 C1 N1 N2 . -167.4(3)
C6 C1 N1 N2 . 13.3(5)
C2 C1 N1 Co1 . 34.7(5)
C6 C1 N1 Co1 . -144.5(3)
N1 Co1 N1 N2 3 85.6(3)
N1 Co1 N1 N2 2 -167.2(2)
N3 Co1 N1 N2 3 46.6(5)
N3 Co1 N1 N2 . 1.67(19)
N3 Co1 N1 N2 2 -103.3(2)
N2 Co1 N1 N2 2 -134.4(2)
N2 Co1 N1 N2 3 75.96(18)
N1 Co1 N1 C1 3 -113.8(3)
N1 Co1 N1 C1 2 -6.5(4)
N3 Co1 N1 C1 3 -152.7(4)
N3 Co1 N1 C1 . 162.3(4)
N3 Co1 N1 C1 2 57.4(4)
N2 Co1 N1 C1 2 26.2(4)
N2 Co1 N1 C1 3 -123.4(3)
C1 N1 N2 N3 . -168.8(3)
Co1 N1 N2 N3 . -2.3(3)
N1 N2 N3 C7 . -173.3(3)
N1 N2 N3 Co1 . 2.3(3)
C8 C7 N3 N2 . -176.9(3)
C12 C7 N3 N2 . 3.0(5)
C8 C7 N3 Co1 . 10.5(6)
C12 C7 N3 Co1 . -169.6(3)
N1 Co1 N3 N2 . -1.69(19)
N1 Co1 N3 N2 3 -106.2(2)
N1 Co1 N3 N2 2 41.0(5)
N3 Co1 N3 N2 3 -170.04(19)
N3 Co1 N3 N2 2 82.0(3)
N2 Co1 N3 N2 2 74.52(18)
N2 Co1 N3 N2 3 -138.0(2)
N1 Co1 N3 C7 . 171.9(4)
N1 Co1 N3 C7 3 67.4(4)
N1 Co1 N3 C7 2 -145.5(4)
N3 Co1 N3 C7 3 3.5(4)
N3 Co1 N3 C7 2 -104.4(3)
N2 Co1 N3 C7 2 -111.9(4)
N2 Co1 N3 C7 3 35.6(4)
