#------------------------------------------------------------------------------
#$Date: 2016-02-16 03:10:39 +0200 (Tue, 16 Feb 2016) $
#$Revision: 176453 $
#$URL: svn://www.crystallography.net/cod/cif/7/01/53/7015322.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_7015322
loop_
_publ_author_name
'Tandon, Santokh S.'
'Dul, Marie-Claire'
'Lee, John L.'
'Dawe, Louise N.'
'Anwar, Muhammad U.'
'Thompson, Laurence K.'
_publ_section_title
;
 Complexes of ditopic carbo- and thio-carbohydrazone
 ligands--mononuclear, 1D chain, dinuclear and tetranuclear examples.
;
_journal_issue                   14
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              3466
_journal_page_last               3475
_journal_paper_doi               10.1039/c0dt01487g
_journal_volume                  40
_journal_year                    2011
_chemical_formula_moiety         'C9 H15 Br2 Co N6 O3, 0.7(C2 H3 N)'
_chemical_formula_sum            'C10.4 H17.1 Br2 Co N6.7 O3'
_chemical_formula_weight         502.73
_chemical_name_systematic
;
?
;
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_symmetry_Int_Tables_number      2
_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                82.511(7)
_cell_angle_beta                 71.639(6)
_cell_angle_gamma                82.963(7)
_cell_formula_units_Z            2
_cell_length_a                   8.5454(10)
_cell_length_b                   10.1776(13)
_cell_length_c                   10.7934(13)
_cell_measurement_reflns_used    5250
_cell_measurement_temperature    153(2)
_cell_measurement_theta_max      29.72
_cell_measurement_theta_min      3.06
_cell_volume                     880.02(19)
_computing_cell_refinement       'TwinSolve (Rigaku/MSC Inc., 2005)'
_computing_data_collection       'CrystalClear (Rigaku/MSC Inc., 2005)'
_computing_data_reduction        'TwinSolve (Rigaku/MSC Inc., 2005)'
_computing_molecular_graphics    'CrystalStructure3.7.0(Rigaku/MSC Inc.,2005)'
_computing_publication_material  'CrystalStructure3.7.0(Rigaku/MSC Inc.,2005)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      153(2)
_diffrn_detector_area_resol_mean 14.63
_diffrn_measured_fraction_theta_full 0.967
_diffrn_measured_fraction_theta_max 0.967
_diffrn_measurement_device_type  'Rigaku Saturn'
_diffrn_measurement_method       ω
_diffrn_radiation_monochromator  'graphite - Rigaku SHINE'
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71069
_diffrn_reflns_av_R_equivalents  0.0613
_diffrn_reflns_av_sigmaI/netI    0.0503
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       13
_diffrn_reflns_limit_l_min       -12
_diffrn_reflns_number            5789
_diffrn_reflns_theta_full        26.50
_diffrn_reflns_theta_max         26.50
_diffrn_reflns_theta_min         3.09
_exptl_absorpt_coefficient_mu    5.552
_exptl_absorpt_correction_T_max  1.0000
_exptl_absorpt_correction_T_min  0.1807
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
; Shape and scale corrections using equivalent reflections.
Shape function based on spherical harmonics.
Highest even and odd order for spherical harmonics: 4 and 1
Laue group: -1
Friedel opposites are equivalent.
;
_exptl_crystal_colour            Brown
_exptl_crystal_density_diffrn    1.897
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       Prism
_exptl_crystal_F_000             494.80
_exptl_crystal_size_max          0.32
_exptl_crystal_size_mid          0.19
_exptl_crystal_size_min          0.10
_refine_diff_density_max         2.151
_refine_diff_density_min         -1.791
_refine_diff_density_rms         0.254
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.119
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     218
_refine_ls_number_reflns         3538
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.119
_refine_ls_R_factor_all          0.0853
_refine_ls_R_factor_gt           0.0789
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[σ²(Fo²)+(0.1290P)²+6.7771P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2190
_refine_ls_wR_factor_ref         0.2263
_reflns_number_gt                3202
_reflns_number_total             3538
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c0dt01487g.txt
_cod_data_source_block           7
_cod_original_formula_sum        'C10.40 H17.10 Br2 Co N6.70 O3 '
_cod_database_code               7015322
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
Br1 Br 0.38141(9) 0.93238(7) 0.32653(7) 0.0238(3) Uani 1 1 d . . .
Br2 Br 0.27437(9) 0.55764(7) 0.15469(7) 0.0252(3) Uani 1 1 d . . .
Co1 Co 0.32686(10) 0.74238(8) 0.24272(8) 0.0147(3) Uani 1 1 d . . .
O1 O 0.2544(7) 0.5983(6) 0.4934(5) 0.0269(12) Uani 1 1 d . . .
O2 O 0.1969(7) 1.0104(7) -0.0783(6) 0.0419(17) Uani 1 1 d . . .
O3 O 0.5465(7) 0.5841(6) 0.3580(5) 0.0323(13) Uani 1 1 d . . .
N1 N 0.1954(7) 0.6816(6) 0.4097(6) 0.0210(12) Uani 1 1 d . . .
N2 N 0.1206(7) 0.8287(6) 0.2328(5) 0.0162(11) Uani 1 1 d . . .
N3 N 0.1057(7) 0.9056(6) 0.1225(6) 0.0196(12) Uani 1 1 d . . .
H7 H 0.0058 0.9416 0.1251 0.024 Uiso 1 1 calc R . .
N4 N 0.3897(8) 0.8813(7) -0.0136(6) 0.0290(15) Uani 1 1 d . . .
H8 H 0.4581 0.9023 -0.0919 0.035 Uiso 1 1 calc R . .
N5 N 0.4555(7) 0.8004(6) 0.0735(6) 0.0196(12) Uani 1 1 d . . .
N6 N 0.5309(7) 0.6570(6) 0.2524(6) 0.0202(12) Uani 1 1 d . . .
N7 N 0.1377(17) 0.766(2) 0.806(2) 0.090(7) Uani 0.70 1 d P . .
C1 C -0.0817(10) 0.6861(10) 0.5699(7) 0.035(2) Uani 1 1 d . . .
H1 H -0.0268 0.6698 0.6384 0.042 Uiso 1 1 calc R . .
H2 H -0.1297 0.6052 0.5645 0.042 Uiso 1 1 calc R . .
H3 H -0.1696 0.7585 0.5914 0.042 Uiso 1 1 calc R . .
C2 C 0.0413(9) 0.7236(8) 0.4417(7) 0.0224(14) Uani 1 1 d . . .
C3 C -0.0036(9) 0.8102(7) 0.3373(7) 0.0201(14) Uani 1 1 d . . .
C4 C -0.1764(10) 0.8685(10) 0.3547(8) 0.036(2) Uani 1 1 d . . .
H4 H -0.1922 0.9542 0.3912 0.043 Uiso 1 1 calc R . .
H5 H -0.2533 0.8079 0.4149 0.043 Uiso 1 1 calc R . .
H6 H -0.1975 0.8818 0.2697 0.043 Uiso 1 1 calc R . .
C5 C 0.2291(9) 0.9319(8) 0.0095(7) 0.0266(16) Uani 1 1 d . . .
C6 C 0.7300(9) 0.7786(8) -0.0904(8) 0.0257(16) Uani 1 1 d . . .
H9 H 0.7299 0.7076 -0.1436 0.031 Uiso 1 1 calc R . .
H10 H 0.8408 0.7792 -0.0820 0.031 Uiso 1 1 calc R . .
H11 H 0.6990 0.8646 -0.1329 0.031 Uiso 1 1 calc R . .
C7 C 0.6094(8) 0.7554(7) 0.0413(7) 0.0197(13) Uani 1 1 d . . .
C8 C 0.6563(8) 0.6731(7) 0.1447(8) 0.0218(14) Uani 1 1 d . . .
C9 C 0.8237(10) 0.6071(9) 0.1349(9) 0.0336(19) Uani 1 1 d . . .
H12 H 0.8809 0.5890 0.0439 0.040 Uiso 1 1 calc R . .
H13 H 0.8140 0.5233 0.1917 0.040 Uiso 1 1 calc R . .
H14 H 0.8869 0.6655 0.1626 0.040 Uiso 1 1 calc R . .
C10 C 0.2703(19) 0.7464(13) 0.7487(16) 0.044(3) Uani 0.70 1 d P . .
C11 C 0.4400(14) 0.7375(13) 0.6714(14) 0.039(3) Uani 0.70 1 d P . .
H15 H 0.4934 0.6504 0.6929 0.047 Uiso 0.70 1 calc PR . .
H16 H 0.4957 0.8078 0.6900 0.047 Uiso 0.70 1 calc PR . .
H17 H 0.4476 0.7480 0.5782 0.047 Uiso 0.70 1 calc PR . .
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'
Br Br -0.2901 2.4595 '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'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 '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 Co1 N5 178.5(2) . . ?
N1 Co1 N6 98.3(3) . . ?
N5 Co1 N6 82.3(3) . . ?
N1 Co1 N2 81.8(2) . . ?
N5 Co1 N2 97.7(2) . . ?
N6 Co1 N2 180.0(3) . . ?
N1 Co1 Br2 90.5(2) . . ?
N5 Co1 Br2 88.07(19) . . ?
N6 Co1 Br2 90.71(19) . . ?
N2 Co1 Br2 89.28(18) . . ?
N1 Co1 Br1 90.8(2) . . ?
N5 Co1 Br1 90.62(19) . . ?
N6 Co1 Br1 89.67(19) . . ?
N2 Co1 Br1 90.34(18) . . ?
Br2 Co1 Br1 178.57(4) . . ?
C2 N1 O1 120.1(6) . . ?
C2 N1 Co1 116.8(5) . . ?
O1 N1 Co1 123.1(5) . . ?
C3 N2 N3 122.7(6) . . ?
C3 N2 Co1 115.4(5) . . ?
N3 N2 Co1 121.9(4) . . ?
C5 N3 N2 126.7(6) . . ?
C5 N3 H7 116.7 . . ?
N2 N3 H7 116.7 . . ?
C5 N4 N5 126.4(6) . . ?
C5 N4 H8 116.8 . . ?
N5 N4 H8 116.8 . . ?
C7 N5 N4 121.7(6) . . ?
C7 N5 Co1 115.7(5) . . ?
N4 N5 Co1 122.5(5) . . ?
O3 N6 C8 122.4(6) . . ?
O3 N6 Co1 122.3(5) . . ?
C8 N6 Co1 115.3(5) . . ?
C2 C1 H1 109.5 . . ?
C2 C1 H2 109.5 . . ?
H1 C1 H2 109.5 . . ?
C2 C1 H3 109.5 . . ?
H1 C1 H3 109.5 . . ?
H2 C1 H3 109.5 . . ?
N1 C2 C3 113.0(6) . . ?
N1 C2 C1 124.3(7) . . ?
C3 C2 C1 122.6(6) . . ?
N2 C3 C2 113.1(6) . . ?
N2 C3 C4 125.7(6) . . ?
C2 C3 C4 121.3(6) . . ?
C3 C4 H4 109.5 . . ?
C3 C4 H5 109.5 . . ?
H4 C4 H5 109.5 . . ?
C3 C4 H6 109.5 . . ?
H4 C4 H6 109.5 . . ?
H5 C4 H6 109.5 . . ?
O2 C5 N3 118.6(7) . . ?
O2 C5 N4 116.6(7) . . ?
N3 C5 N4 124.7(6) . . ?
C7 C6 H9 109.5 . . ?
C7 C6 H10 109.5 . . ?
H9 C6 H10 109.5 . . ?
C7 C6 H11 109.5 . . ?
H9 C6 H11 109.5 . . ?
H10 C6 H11 109.5 . . ?
N5 C7 C8 114.0(6) . . ?
N5 C7 C6 124.9(7) . . ?
C8 C7 C6 121.0(6) . . ?
N6 C8 C7 112.6(6) . . ?
N6 C8 C9 121.7(7) . . ?
C7 C8 C9 125.6(7) . . ?
C8 C9 H12 109.5 . . ?
C8 C9 H13 109.5 . . ?
H12 C9 H13 109.5 . . ?
C8 C9 H14 109.5 . . ?
H12 C9 H14 109.5 . . ?
H13 C9 H14 109.5 . . ?
N7 C10 C11 173.5(18) . . ?
C10 C11 H15 109.5 . . ?
C10 C11 H16 109.5 . . ?
H15 C11 H16 109.5 . . ?
C10 C11 H17 109.5 . . ?
H15 C11 H17 109.5 . . ?
H16 C11 H17 109.5 . . ?
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
Br1 Co1 2.3911(11) . ?
Br2 Co1 2.3622(11) . ?
Co1 N1 1.870(6) . ?
Co1 N5 1.872(6) . ?
Co1 N6 1.878(6) . ?
Co1 N2 1.898(5) . ?
O1 N1 1.331(7) . ?
O2 C5 1.235(9) . ?
O3 N6 1.311(8) . ?
N1 C2 1.285(9) . ?
N2 C3 1.293(9) . ?
N2 N3 1.369(8) . ?
N3 C5 1.359(9) . ?
N3 H7 0.8800 . ?
N4 C5 1.363(9) . ?
N4 N5 1.377(9) . ?
N4 H8 0.8800 . ?
N5 C7 1.290(9) . ?
N6 C8 1.317(10) . ?
N7 C10 1.12(2) . ?
C1 C2 1.486(10) . ?
C1 H1 0.9800 . ?
C1 H2 0.9800 . ?
C1 H3 0.9800 . ?
C2 C3 1.458(9) . ?
C3 C4 1.486(10) . ?
C4 H4 0.9800 . ?
C4 H5 0.9800 . ?
C4 H6 0.9800 . ?
C6 C7 1.479(10) . ?
C6 H9 0.9800 . ?
C6 H10 0.9800 . ?
C6 H11 0.9800 . ?
C7 C8 1.436(10) . ?
C8 C9 1.482(9) . ?
C9 H12 0.9800 . ?
C9 H13 0.9800 . ?
C9 H14 0.9800 . ?
C10 C11 1.425(18) . ?
C11 H15 0.9800 . ?
C11 H16 0.9800 . ?
C11 H17 0.9800 . ?
