#------------------------------------------------------------------------------
#$Date: 2016-02-16 22:30:59 +0200 (Tue, 16 Feb 2016) $
#$Revision: 176467 $
#$URL: svn://www.crystallography.net/cod/cif/4/30/76/4307659.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_4307659
loop_
_publ_author_name
'Jung Hee Yoon'
'Jeong Hak Lim'
'Seok Woo Choi'
'Hyoung Chan Kim'
'Chang Seop Hong'
_publ_section_title
;
Cyanide-Bridged WV-CoII Double-Zigzag Chain Based on an Octacoordinated W
Precursor: Metamagnetism and Spin Canting
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              1529
_journal_page_last               1531
_journal_paper_doi               10.1021/ic062143d
_journal_volume                  46
_journal_year                    2007
_chemical_formula_sum            'C16 H14 Co0.5 N8 O3 W'
_chemical_formula_weight         579.67
_chemical_name_systematic
;
 ?
;
_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                99.5090(10)
_cell_angle_beta                 100.8330(10)
_cell_angle_gamma                107.0080(10)
_cell_formula_units_Z            2
_cell_length_a                   8.3504(6)
_cell_length_b                   10.5157(8)
_cell_length_c                   11.8710(9)
_cell_measurement_temperature    130
_cell_volume                     951.76(12)
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_diffrn_ambient_temperature      130
_diffrn_measured_fraction_theta_full 0.904
_diffrn_measured_fraction_theta_max 0.904
_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  0.0141
_diffrn_reflns_av_sigmaI/netI    0.0164
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       14
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_number            9999
_diffrn_reflns_theta_full        27.39
_diffrn_reflns_theta_max         27.39
_diffrn_reflns_theta_min         1.80
_exptl_absorpt_coefficient_mu    6.525
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   sadabs
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    2.023
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             555
_exptl_crystal_size_max          0.3
_exptl_crystal_size_mid          0.1
_exptl_crystal_size_min          0.08
_refine_diff_density_max         1.074
_refine_diff_density_min         -0.661
_refine_diff_density_rms         0.074
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.086
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     283
_refine_ls_number_reflns         3905
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.086
_refine_ls_R_factor_all          0.0146
_refine_ls_R_factor_gt           0.0140
_refine_ls_shift/su_max          0.057
_refine_ls_shift/su_mean         0.001
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[σ²(Fo²)+(0.0089P)²+1.2718P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0315
_refine_ls_wR_factor_ref         0.0317
_reflns_number_gt                3813
_reflns_number_total             3905
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic062143dsi20061110_091544.cif
_cod_data_source_block           p-1
_cod_original_formula_sum        'C16 H14 Co0.50 N8 O3 W'
_cod_database_code               4307659
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
W1 W 0.347045(11) 0.813677(9) 0.727214(8) 0.01297(3) Uani 1 1 d . . .
C1 C 0.6098(3) 0.8818(2) 0.8322(2) 0.0175(5) Uani 1 1 d . . .
N1 N 0.7484(3) 0.9165(2) 0.88965(18) 0.0198(4) Uani 1 1 d . . .
C2 C 0.4145(3) 0.6310(3) 0.7195(2) 0.0195(5) Uani 1 1 d . . .
N2 N 0.4460(3) 0.5318(2) 0.7106(2) 0.0272(5) Uani 1 1 d . . .
C3 C 0.3521(3) 0.7912(3) 0.9038(2) 0.0200(5) Uani 1 1 d . . .
N3 N 0.3401(3) 0.7793(3) 0.99667(19) 0.0284(5) Uani 1 1 d . . .
C4 C 0.4970(3) 0.7989(2) 0.6000(2) 0.0191(5) Uani 1 1 d . . .
N4 N 0.5765(3) 0.7882(2) 0.5321(2) 0.0267(5) Uani 1 1 d . . .
C5 C 0.4680(3) 1.0238(3) 0.7257(2) 0.0190(5) Uani 1 1 d . . .
N5 N 0.5353(3) 1.1347(2) 0.72281(19) 0.0278(5) Uani 1 1 d . . .
C6 C 0.1913(3) 0.9226(2) 0.8009(2) 0.0172(5) Uani 1 1 d . . .
N6 N 0.1129(3) 0.9727(2) 0.85157(18) 0.0192(4) Uani 1 1 d . . .
N7 N 0.1749(2) 0.8203(2) 0.56251(17) 0.0163(4) Uani 1 1 d . . .
N8 N 0.0970(2) 0.6458(2) 0.69654(17) 0.0169(4) Uani 1 1 d . . .
C7 C 0.2237(3) 0.9046(3) 0.4914(2) 0.0205(5) Uani 1 1 d . . .
H7 H 0.3386 0.9608 0.5096 0.025 Uiso 1 1 calc R . .
C8 C 0.1110(3) 0.9111(3) 0.3932(2) 0.0235(5) Uani 1 1 d . . .
H8 H 0.1497 0.9701 0.3462 0.028 Uiso 1 1 calc R . .
C9 C -0.0602(3) 0.8288(3) 0.3657(2) 0.0225(5) Uani 1 1 d . . .
H9 H -0.1389 0.8320 0.3004 0.027 Uiso 1 1 calc R . .
C10 C -0.1123(3) 0.7416(3) 0.4371(2) 0.0198(5) Uani 1 1 d . . .
H10 H -0.2271 0.6854 0.4201 0.024 Uiso 1 1 calc R . .
C11 C 0.0066(3) 0.7377(2) 0.5340(2) 0.0159(5) Uani 1 1 d . . .
C12 C -0.0367(3) 0.6410(2) 0.6084(2) 0.0169(5) Uani 1 1 d . . .
C13 C -0.2001(3) 0.5449(3) 0.5886(2) 0.0212(5) Uani 1 1 d . . .
H13 H -0.2907 0.5445 0.5293 0.025 Uiso 1 1 calc R . .
C14 C -0.2278(3) 0.4505(3) 0.6568(2) 0.0233(5) Uani 1 1 d . . .
H14 H -0.3367 0.3859 0.6440 0.028 Uiso 1 1 calc R . .
C15 C -0.0911(3) 0.4534(3) 0.7444(2) 0.0237(5) Uani 1 1 d . . .
H15 H -0.1064 0.3898 0.7907 0.028 Uiso 1 1 calc R . .
C16 C 0.0681(3) 0.5519(3) 0.7623(2) 0.0215(5) Uani 1 1 d . . .
H16 H 0.1592 0.5538 0.8220 0.026 Uiso 1 1 calc R . .
Co1 Co 1.0000 1.0000 1.0000 0.01250(9) Uani 1 2 d S . .
O1 O 0.9933(3) 1.1871(2) 0.9772(2) 0.0301(5) Uani 1 1 d . . .
H1A H 0.911(5) 1.202(4) 0.972(3) 0.045(11) Uiso 1 1 d . . .
H1B H 1.075(5) 1.253(4) 0.972(3) 0.058(12) Uiso 1 1 d . . .
O2 O 0.4817(3) 0.6181(2) 0.1295(2) 0.0463(6) Uani 1 1 d . . .
H2A H 0.520(12) 0.563(10) 0.202(9) 0.26(4) Uiso 1 1 d . . .
H2B H 0.469(10) 0.726(9) 0.162(7) 0.20(3) Uiso 1 1 d . . .
O3 O 0.2365(3) 0.4015(3) 0.9550(2) 0.0438(6) Uani 1 1 d . . .
H3A H 0.316(5) 0.358(4) 0.928(3) 0.055(11) Uiso 1 1 d . . .
H3B H 0.295(5) 0.459(4) 1.021(4) 0.064(13) Uiso 1 1 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'
W W -0.8490 6.8722 '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
C3 W1 C2 80.13(9) . . ?
C3 W1 C4 138.99(9) . . ?
C2 W1 C4 70.09(9) . . ?
C3 W1 C5 110.86(9) . . ?
C2 W1 C5 137.91(9) . . ?
C4 W1 C5 77.14(9) . . ?
C3 W1 C1 69.65(9) . . ?
C2 W1 C1 75.33(9) . . ?
C4 W1 C1 75.84(9) . . ?
C5 W1 C1 71.54(9) . . ?
C3 W1 C6 70.60(9) . . ?
C2 W1 C6 143.41(9) . . ?
C4 W1 C6 145.90(9) . . ?
C5 W1 C6 74.92(9) . . ?
C1 W1 C6 112.59(9) . . ?
C3 W1 N7 142.84(8) . . ?
C2 W1 N7 115.05(8) . . ?
C4 W1 N7 77.06(8) . . ?
C5 W1 N7 81.24(8) . . ?
C1 W1 N7 145.05(8) . . ?
C6 W1 N7 79.70(8) . . ?
C3 W1 N8 79.54(8) . . ?
C2 W1 N8 75.12(8) . . ?
C4 W1 N8 117.32(8) . . ?
C5 W1 N8 145.51(8) . . ?
C1 W1 N8 140.22(8) . . ?
C6 W1 N8 78.31(8) . . ?
N7 W1 N8 72.85(7) . . ?
N1 C1 W1 178.6(2) . . ?
C1 N1 Co1 174.1(2) . . ?
N2 C2 W1 177.1(2) . . ?
N3 C3 W1 174.0(2) . . ?
N4 C4 W1 178.5(2) . . ?
N5 C5 W1 178.0(2) . . ?
N6 C6 W1 171.4(2) . . ?
C6 N6 Co1 150.91(19) . 1_455 ?
C7 N7 C11 117.7(2) . . ?
C7 N7 W1 124.63(15) . . ?
C11 N7 W1 117.56(15) . . ?
C16 N8 C12 118.2(2) . . ?
C16 N8 W1 124.24(16) . . ?
C12 N8 W1 117.49(15) . . ?
N7 C7 C8 123.1(2) . . ?
C7 C8 C9 119.0(2) . . ?
C8 C9 C10 118.7(2) . . ?
C9 C10 C11 120.0(2) . . ?
N7 C11 C10 121.4(2) . . ?
N7 C11 C12 115.6(2) . . ?
C10 C11 C12 122.9(2) . . ?
N8 C12 C13 121.1(2) . . ?
N8 C12 C11 115.6(2) . . ?
C13 C12 C11 123.3(2) . . ?
C14 C13 C12 120.0(2) . . ?
C13 C14 C15 118.9(2) . . ?
C16 C15 C14 119.2(2) . . ?
N8 C16 C15 122.6(2) . . ?
O1 Co1 O1 180.000(1) 2_777 . ?
O1 Co1 N1 87.26(9) 2_777 2_777 ?
O1 Co1 N1 92.74(9) . 2_777 ?
O1 Co1 N1 92.74(9) 2_777 . ?
O1 Co1 N1 87.26(9) . . ?
N1 Co1 N1 180.000(1) 2_777 . ?
O1 Co1 N6 88.71(8) 2_777 1_655 ?
O1 Co1 N6 91.29(8) . 1_655 ?
N1 Co1 N6 88.28(8) 2_777 1_655 ?
N1 Co1 N6 91.72(8) . 1_655 ?
O1 Co1 N6 91.29(8) 2_777 2_677 ?
O1 Co1 N6 88.71(8) . 2_677 ?
N1 Co1 N6 91.72(8) 2_777 2_677 ?
N1 Co1 N6 88.28(8) . 2_677 ?
N6 Co1 N6 180.000(1) 1_655 2_677 ?
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
W1 C3 2.142(3) . ?
W1 C2 2.147(3) . ?
W1 C4 2.149(2) . ?
W1 C5 2.149(3) . ?
W1 C1 2.153(2) . ?
W1 C6 2.176(2) . ?
W1 N7 2.2231(19) . ?
W1 N8 2.2256(19) . ?
C1 N1 1.145(3) . ?
N1 Co1 2.099(2) . ?
C2 N2 1.142(3) . ?
C3 N3 1.150(3) . ?
C4 N4 1.149(3) . ?
C5 N5 1.147(3) . ?
C6 N6 1.146(3) . ?
N6 Co1 2.166(2) 1_455 ?
N7 C7 1.352(3) . ?
N7 C11 1.361(3) . ?
N8 C16 1.353(3) . ?
N8 C12 1.361(3) . ?
C7 C8 1.379(3) . ?
C8 C9 1.381(4) . ?
C9 C10 1.383(4) . ?
C10 C11 1.386(3) . ?
C11 C12 1.466(3) . ?
C12 C13 1.390(3) . ?
C13 C14 1.377(4) . ?
C14 C15 1.381(4) . ?
C15 C16 1.378(3) . ?
Co1 O1 2.045(2) 2_777 ?
Co1 O1 2.045(2) . ?
Co1 N1 2.099(2) 2_777 ?
Co1 N6 2.166(2) 1_655 ?
Co1 N6 2.166(2) 2_677 ?
