#------------------------------------------------------------------------------
#$Date: 2016-03-25 13:30:56 +0200 (Fri, 25 Mar 2016) $
#$Revision: 179848 $
#$URL: svn://www.crystallography.net/cod/cif/7/01/44/7014436.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_7014436
loop_
_publ_author_name
'Boonmak, Jaursup'
'Nakano, Motohiro'
'Youngme, Sujittra'
_publ_section_title
;
 Structural diversity and magnetic properties in 1D and 2D
 azido-bridged cobalt(II) complexes with 1,2-bis(2-pyridyl)ethylene.
;
_journal_issue                   6
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              1254
_journal_page_last               1260
_journal_paper_doi               10.1039/c0dt00853b
_journal_volume                  40
_journal_year                    2011
_chemical_formula_sum            'C36 H34 Co3 N24 O2'
_chemical_formula_weight         1011.66
_chemical_name_common
;
diaqua hexaazido bis(1,2-bis(2-pyridyl)ethylene)
tricobalt(ii)(1,2-bis(2-pyridyl)ethylene)
;
_chemical_name_systematic
;
diaqua hexaazido bis(1,2-bis(2-pyridyl)ethylene)
tricobalt(II)(1,2-bis(2-pyridyl)ethylene)
;
_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                117.61(3)
_cell_angle_beta                 100.91(3)
_cell_angle_gamma                96.17(3)
_cell_formula_units_Z            1
_cell_length_a                   8.8038(18)
_cell_length_b                   11.541(2)
_cell_length_c                   12.422(3)
_cell_measurement_reflns_used    7187
_cell_measurement_temperature    123(2)
_cell_measurement_theta_max      27.47
_cell_measurement_theta_min      3.09
_cell_volume                     1070.2(6)
_computing_cell_refinement       process-auto
_computing_data_collection       'process-auto(Rigaku, 1998)'
_computing_data_reduction        'CRYSTAL STRUCTURE (Rigaku/MSC, 2006)'
_computing_molecular_graphics    SHELXTL
_computing_publication_material  SHELXTL
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      123(2)
_diffrn_measured_fraction_theta_full 0.989
_diffrn_measured_fraction_theta_max 0.989
_diffrn_measurement_device_type
;
Rigaku RAXIS-RAPID
;
_diffrn_measurement_method       '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  0.0501
_diffrn_reflns_av_sigmaI/netI    0.0651
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_number            10327
_diffrn_reflns_theta_full        27.47
_diffrn_reflns_theta_max         27.47
_diffrn_reflns_theta_min         3.09
_exptl_absorpt_coefficient_mu    1.215
_exptl_absorpt_correction_T_max  1.0000
_exptl_absorpt_correction_T_min  0.687670
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
Higashi, T. (1995). Program for Absorption Correction.
Rigaku Corporation, Tokyo, Japan.
;
_exptl_crystal_colour            blue
_exptl_crystal_density_diffrn    1.570
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       rod
_exptl_crystal_F_000             515
_exptl_crystal_size_max          0.60
_exptl_crystal_size_mid          0.15
_exptl_crystal_size_min          0.10
_refine_diff_density_max         0.920
_refine_diff_density_min         -1.743
_refine_diff_density_rms         0.144
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.184
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     303
_refine_ls_number_reflns         4790
_refine_ls_number_restraints     3
_refine_ls_restrained_S_all      1.184
_refine_ls_R_factor_all          0.0651
_refine_ls_R_factor_gt           0.0479
_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)+(0.0609P)²+1.6407P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1153
_refine_ls_wR_factor_ref         0.1560
_reflns_number_gt                3817
_reflns_number_total             4790
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            C0DT00853B.TXT
_cod_data_source_block           Cpd_1
_cod_original_cell_volume        1070.1(6)
_cod_original_sg_symbol_H-M      P-1
_cod_database_code               7014436
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
Co1 Co 0.37667(5) 0.08731(4) 0.55308(4) 0.01578(16) Uani 1 1 d . . .
Co2 Co 0.0000 0.0000 0.5000 0.01469(18) Uani 1 2 d S . .
N1 N 0.1654(3) 0.1390(3) 0.4869(3) 0.0164(6) Uani 1 1 d . . .
N2 N 0.1504(4) 0.1700(3) 0.4057(3) 0.0216(7) Uani 1 1 d . . .
N3 N 0.1386(5) 0.2025(4) 0.3304(4) 0.0400(9) Uani 1 1 d . . .
N4 N 0.2201(4) -0.0235(3) 0.5884(3) 0.0182(6) Uani 1 1 d . . .
N5 N 0.2545(4) -0.0873(3) 0.6402(3) 0.0206(7) Uani 1 1 d . . .
N6 N 0.2876(4) -0.1479(4) 0.6894(4) 0.0336(8) Uani 1 1 d . . .
N7 N 0.4248(3) -0.0207(3) 0.3848(3) 0.0164(6) Uani 1 1 d . . .
N8 N 0.3390(4) -0.0611(3) 0.2804(3) 0.0193(6) Uani 1 1 d . . .
N9 N 0.2610(4) -0.1004(3) 0.1800(3) 0.0295(8) Uani 1 1 d . . .
N10 N 0.5058(4) 0.2837(3) 0.6259(3) 0.0195(6) Uani 1 1 d . . .
N11 N 0.1961(4) 0.1655(3) 0.8840(3) 0.0216(7) Uani 1 1 d . . .
N12 N 0.0345(5) 0.4111(3) 0.7387(3) 0.0299(8) Uani 1 1 d . . .
C1 C 0.5373(4) 0.3155(4) 0.5393(4) 0.0225(8) Uani 1 1 d . . .
H1 H 0.4966 0.2523 0.4542 0.027 Uiso 1 1 calc R . .
C2 C 0.6279(5) 0.4389(4) 0.5729(4) 0.0249(8) Uani 1 1 d . . .
H2 H 0.6479 0.4577 0.5111 0.030 Uiso 1 1 calc R . .
C3 C 0.6882(5) 0.5338(4) 0.6991(4) 0.0282(9) Uani 1 1 d . . .
H3 H 0.7480 0.6177 0.7236 0.034 Uiso 1 1 calc R . .
C4 C 0.6581(5) 0.5016(4) 0.7882(4) 0.0252(8) Uani 1 1 d . . .
H4 H 0.6989 0.5637 0.8737 0.030 Uiso 1 1 calc R . .
C5 C 0.5666(4) 0.3759(4) 0.7501(3) 0.0208(7) Uani 1 1 d . . .
C6 C 0.5317(5) 0.3384(4) 0.8422(3) 0.0225(8) Uani 1 1 d . . .
H6 H 0.6112 0.3662 0.9157 0.027 Uiso 1 1 calc R . .
C7 C 0.3922(5) 0.2668(4) 0.8257(3) 0.0209(8) Uani 1 1 d . . .
H7 H 0.3116 0.2486 0.7560 0.025 Uiso 1 1 calc R . .
C8 C 0.3513(5) 0.2130(4) 0.9058(3) 0.0218(8) Uani 1 1 d . . .
C9 C 0.4673(5) 0.2061(4) 0.9965(4) 0.0295(9) Uani 1 1 d . . .
H9 H 0.5744 0.2371 1.0086 0.035 Uiso 1 1 calc R . .
C10 C 0.4204(6) 0.1530(4) 1.0671(4) 0.0336(10) Uani 1 1 d . . .
H10 H 0.4951 0.1490 1.1285 0.040 Uiso 1 1 calc R . .
C11 C 0.2597(5) 0.1055(4) 1.0451(4) 0.0326(10) Uani 1 1 d . . .
H11 H 0.2248 0.0698 1.0919 0.039 Uiso 1 1 calc R . .
C12 C 0.1522(5) 0.1123(4) 0.9524(4) 0.0261(8) Uani 1 1 d . . .
H12 H 0.0448 0.0786 0.9368 0.031 Uiso 1 1 calc R . .
C13 C 0.0658(6) 0.4475(4) 0.6553(4) 0.0357(10) Uani 1 1 d . . .
H13 H 0.0576 0.3804 0.5738 0.043 Uiso 1 1 calc R . .
C14 C 0.1093(5) 0.5793(4) 0.6847(4) 0.0307(9) Uani 1 1 d . . .
H14 H 0.1327 0.6005 0.6251 0.037 Uiso 1 1 calc R . .
C15 C 0.0841(5) 0.6437(4) 0.8914(4) 0.0236(8) Uani 1 1 d . . .
H15 H 0.0892 0.7096 0.9728 0.028 Uiso 1 1 calc R . .
C16 C 0.0426(5) 0.5083(4) 0.8560(4) 0.0228(8) Uani 1 1 d . . .
C18 C 0.1174(5) 0.6795(4) 0.8052(4) 0.0266(8) Uani 1 1 d . . .
H18 H 0.1449 0.7694 0.8276 0.032 Uiso 1 1 calc R . .
C17 C 0.0020(5) 0.4612(4) 0.9405(4) 0.0244(8) Uani 1 1 d . . .
H17 H -0.0234 0.3689 0.9083 0.029 Uiso 1 1 calc R . .
O1 O -0.0169(3) 0.1446(2) 0.6730(2) 0.0190(5) Uani 1 1 d D . .
H1B H -0.009(6) 0.236(3) 0.694(4) 0.049(15) Uiso 1 1 d D . .
H1A H 0.046(5) 0.147(5) 0.743(4) 0.047(15) Uiso 1 1 d D . .
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'
O O 0.0106 0.0060 '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
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
N4 Co1 N7 112.86(13) . . ?
N4 Co1 N10 142.28(12) . . ?
N7 Co1 N10 104.78(12) . . ?
N4 Co1 N7 93.85(12) . 2_656 ?
N7 Co1 N7 80.94(13) . 2_656 ?
N10 Co1 N7 94.38(12) . 2_656 ?
N4 Co1 N1 82.00(12) . . ?
N7 Co1 N1 98.66(12) . . ?
N10 Co1 N1 90.22(12) . . ?
N7 Co1 N1 175.34(11) 2_656 . ?
O1 Co2 O1 180.000(1) 2_556 . ?
O1 Co2 N1 92.50(11) 2_556 2_556 ?
O1 Co2 N1 87.50(11) . 2_556 ?
O1 Co2 N1 87.50(11) 2_556 . ?
O1 Co2 N1 92.50(11) . . ?
N1 Co2 N1 180.000(1) 2_556 . ?
O1 Co2 N4 89.10(12) 2_556 . ?
O1 Co2 N4 90.90(12) . . ?
N1 Co2 N4 100.50(11) 2_556 . ?
N1 Co2 N4 79.50(11) . . ?
O1 Co2 N4 90.90(12) 2_556 2_556 ?
O1 Co2 N4 89.10(12) . 2_556 ?
N1 Co2 N4 79.50(11) 2_556 2_556 ?
N1 Co2 N4 100.50(11) . 2_556 ?
N4 Co2 N4 180.0 . 2_556 ?
N2 N1 Co2 127.4(2) . . ?
N2 N1 Co1 122.9(2) . . ?
Co2 N1 Co1 97.09(12) . . ?
N3 N2 N1 178.3(4) . . ?
N5 N4 Co1 125.3(3) . . ?
N5 N4 Co2 134.2(3) . . ?
Co1 N4 Co2 100.37(12) . . ?
N6 N5 N4 179.8(4) . . ?
N8 N7 Co1 127.5(2) . . ?
N8 N7 Co1 130.9(2) . 2_656 ?
Co1 N7 Co1 99.06(13) . 2_656 ?
N9 N8 N7 178.1(4) . . ?
C1 N10 C5 118.6(3) . . ?
C1 N10 Co1 115.5(2) . . ?
C5 N10 Co1 125.8(2) . . ?
C8 N11 C12 118.5(3) . . ?
C13 N12 C16 118.4(3) . . ?
N10 C1 C2 122.4(4) . . ?
N10 C1 H1 118.8 . . ?
C2 C1 H1 118.8 . . ?
C3 C2 C1 119.3(4) . . ?
C3 C2 H2 120.4 . . ?
C1 C2 H2 120.4 . . ?
C4 C3 C2 118.8(3) . . ?
C4 C3 H3 120.6 . . ?
C2 C3 H3 120.6 . . ?
C3 C4 C5 120.0(4) . . ?
C3 C4 H4 120.0 . . ?
C5 C4 H4 120.0 . . ?
N10 C5 C4 121.1(3) . . ?
N10 C5 C6 117.5(3) . . ?
C4 C5 C6 121.5(3) . . ?
C7 C6 C5 123.2(4) . . ?
C7 C6 H6 118.4 . . ?
C5 C6 H6 118.4 . . ?
C6 C7 C8 127.1(4) . . ?
C6 C7 H7 116.5 . . ?
C8 C7 H7 116.5 . . ?
N11 C8 C9 121.5(3) . . ?
N11 C8 C7 116.0(3) . . ?
C9 C8 C7 122.5(4) . . ?
C10 C9 C8 119.3(4) . . ?
C10 C9 H9 120.3 . . ?
C8 C9 H9 120.3 . . ?
C9 C10 C11 118.8(4) . . ?
C9 C10 H10 120.6 . . ?
C11 C10 H10 120.6 . . ?
C12 C11 C10 118.9(4) . . ?
C12 C11 H11 120.6 . . ?
C10 C11 H11 120.6 . . ?
N11 C12 C11 122.9(4) . . ?
N11 C12 H12 118.5 . . ?
C11 C12 H12 118.5 . . ?
N12 C13 C14 123.3(4) . . ?
N12 C13 H13 118.3 . . ?
C14 C13 H13 118.3 . . ?
C13 C14 C18 118.4(4) . . ?
C13 C14 H14 120.8 . . ?
C18 C14 H14 120.8 . . ?
C18 C15 C16 119.8(4) . . ?
C18 C15 H15 120.1 . . ?
C16 C15 H15 120.1 . . ?
N12 C16 C15 121.2(3) . . ?
N12 C16 C17 115.4(3) . . ?
C15 C16 C17 123.4(3) . . ?
C15 C18 C14 118.9(4) . . ?
C15 C18 H18 120.6 . . ?
C14 C18 H18 120.6 . . ?
C17 C17 C16 126.0(5) 2_567 . ?
C17 C17 H17 117.0 2_567 . ?
C16 C17 H17 117.0 . . ?
Co2 O1 H1B 122(3) . . ?
Co2 O1 H1A 116(3) . . ?
H1B O1 H1A 105(3) . . ?
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
Co1 N4 2.025(3) . ?
Co1 N7 2.034(3) . ?
Co1 N10 2.098(3) . ?
Co1 N7 2.138(3) 2_656 ?
Co1 N1 2.146(3) . ?
Co2 O1 2.068(3) 2_556 ?
Co2 O1 2.068(3) . ?
Co2 N1 2.133(3) 2_556 ?
Co2 N1 2.133(3) . ?
Co2 N4 2.149(3) . ?
Co2 N4 2.149(3) 2_556 ?
N1 N2 1.207(4) . ?
N2 N3 1.151(5) . ?
N4 N5 1.208(4) . ?
N5 N6 1.149(5) . ?
N7 N8 1.209(4) . ?
N7 Co1 2.138(3) 2_656 ?
N8 N9 1.148(4) . ?
N10 C1 1.351(5) . ?
N10 C5 1.357(5) . ?
N11 C8 1.342(5) . ?
N11 C12 1.344(5) . ?
N12 C13 1.346(5) . ?
N12 C16 1.346(5) . ?
C1 C2 1.385(5) . ?
C1 H1 0.9300 . ?
C2 C3 1.382(6) . ?
C2 H2 0.9300 . ?
C3 C4 1.380(6) . ?
C3 H3 0.9300 . ?
C4 C5 1.395(5) . ?
C4 H4 0.9300 . ?
C5 C6 1.467(5) . ?
C6 C7 1.328(5) . ?
C6 H6 0.9300 . ?
C7 C8 1.471(5) . ?
C7 H7 0.9300 . ?
C8 C9 1.408(6) . ?
C9 C10 1.377(6) . ?
C9 H9 0.9300 . ?
C10 C11 1.387(6) . ?
C10 H10 0.9300 . ?
C11 C12 1.383(6) . ?
C11 H11 0.9300 . ?
C12 H12 0.9300 . ?
C13 C14 1.379(6) . ?
C13 H13 0.9300 . ?
C14 C18 1.385(6) . ?
C14 H14 0.9300 . ?
C15 C18 1.382(5) . ?
C15 C16 1.395(5) . ?
C15 H15 0.9300 . ?
C16 C17 1.468(5) . ?
C18 H18 0.9300 . ?
C17 C17 1.338(7) 2_567 ?
C17 H17 0.9300 . ?
O1 H1B 0.95(3) . ?
O1 H1A 0.93(3) . ?
