#------------------------------------------------------------------------------
#$Date: 2016-03-23 14:44:38 +0200 (Wed, 23 Mar 2016) $
#$Revision: 179304 $
#$URL: svn://www.crystallography.net/cod/cif/4/32/01/4320156.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_4320156
loop_
_publ_author_name
'Zurine E. Serna'
'M. Karmele Urtiaga'
'M. Gotzone Barandika'
'Roberto Cortés'
'Susana Martin'
'Luis Lezama'
'M. Isabel Arriortua'
'Teófilo Rojo'
_publ_contact_author
;
   Dra. Miren Karmele Urtiaga
   Dpto. de Mineralogía y Petrología 
   Universidad del País Vasco
   Apartado 644
   48080 Bilbao
   Spain
;
_publ_contact_author_email       nppurgrm@lg.ehu.es
_publ_contact_author_fax         '34 4 4648500'
_publ_contact_author_phone       '34 4 6012555'
_publ_section_title
;
 Dicubane-like Tetrameric Cobalt(II)-Pseudohalide Ferromagnetic Clusters
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              4550
_journal_page_last               4555
_journal_paper_doi               10.1021/ic0013476
_journal_volume                  40
_journal_year                    2001
_chemical_formula_sum            'C25 H20 Co2 N6 O6'
_chemical_formula_weight         618.33
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 122.575(9)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   13.0395(13)
_cell_length_b                   12.3033(13)
_cell_length_c                   19.3648(15)
_cell_measurement_temperature    293(2)
_cell_volume                     2618.0(5)
_computing_data_collection       'Stoe IPDS diffractometer'
_computing_data_reduction        'Stoe IPDS Software'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 0.830
_diffrn_measured_fraction_theta_max 0.830
_diffrn_measurement_device_type  'Stoe IPDS diffractometer'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71070
_diffrn_reflns_av_R_equivalents  0.1483
_diffrn_reflns_av_sigmaI/netI    0.2575
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -18
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       25
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_number            14672
_diffrn_reflns_theta_full        30.53
_diffrn_reflns_theta_max         30.53
_diffrn_reflns_theta_min         1.85
_exptl_absorpt_coefficient_mu    1.319
_exptl_crystal_density_diffrn    1.569
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             1256
_refine_diff_density_max         0.531
_refine_diff_density_min         -0.605
_refine_diff_density_rms         0.093
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.799
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     353
_refine_ls_number_reflns         6653
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.799
_refine_ls_R_factor_all          0.2125
_refine_ls_R_factor_gt           0.0581
_refine_ls_shift/su_max          0.728
_refine_ls_shift/su_mean         0.129
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[σ²(Fo²)+(0.0392P)²+0.0000P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0981
_refine_ls_wR_factor_ref         0.1352
_reflns_number_gt                2375
_reflns_number_total             6653
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic0013476_2.cif
_cod_data_source_block           val
_cod_depositor_comments
;
The following automatic conversions were performed:

'_symmetry_cell_setting' value 'Monoclinic' changed to 'monoclinic'
according to the built-in table from CIF Core dictionary named
'cif_core.dic' version 2.4.1 from 2010-06-29.

Automatic conversion script
Id: cif_fix_values 1646 2011-03-28 12:23:43Z adriana 
;
_cod_original_cell_volume        2618.0(4)
_cod_original_sg_symbol_H-M      'P 21/c'
_cod_database_code               4320156
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, y+1/2, -z+1/2'
'-x, -y, -z'
'x, -y-1/2, z-1/2'
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 0.61625(7) 0.57434(5) 0.04604(4) 0.0278(2) Uani 1 1 d . . .
Co2 Co 0.65502(7) 0.31378(6) 0.05153(5) 0.0344(2) Uani 1 1 d . . .
O1 O 0.5495(3) 0.4414(3) 0.07052(19) 0.0264(8) Uani 1 1 d . . .
O2 O 0.4779(3) 0.4894(3) 0.1513(2) 0.0369(10) Uani 1 1 d . . .
H1O2 H 0.4896 0.4832 0.1972 0.080(5) Uiso 1 1 calc R . .
O3 O 0.6873(3) 0.4475(3) 0.0032(2) 0.0306(9) Uani 1 1 d . . .
O4 O 0.8519(3) 0.4090(3) -0.0109(3) 0.0481(11) Uani 1 1 d . . .
O5 O 0.8435(5) 0.0932(4) -0.0107(3) 0.103(2) Uani 1 1 d . . .
O6 O 0.4008(6) 0.1663(5) -0.1630(4) 0.141(3) Uani 1 1 d . . .
N1 N 0.6143(4) 0.2462(4) 0.1356(3) 0.0394(12) Uani 1 1 d . . .
N2 N 0.7318(4) 0.5599(3) 0.1779(3) 0.0324(11) Uani 1 1 d . . .
N3 N 0.8421(4) 0.3655(4) 0.1469(3) 0.0399(12) Uani 1 1 d . . .
N4 N 0.7374(4) 0.6559(4) 0.0243(3) 0.0348(12) Uani 1 1 d . . .
N5 N 0.7270(5) 0.1813(4) 0.0309(3) 0.0619(16) Uani 1 1 d . . .
N6 N 0.4747(4) 0.2912(3) -0.0540(3) 0.0393(13) Uani 1 1 d . . .
C1 C 0.6118(6) 0.1380(5) 0.1475(4) 0.0584(19) Uani 1 1 d . . .
H1 H 0.6472 0.0912 0.1284 0.080(5) Uiso 1 1 calc R . .
C2 C 0.5596(7) 0.0949(6) 0.1861(5) 0.076(2) Uani 1 1 d . . .
H2 H 0.5559 0.0200 0.1907 0.080(5) Uiso 1 1 calc R . .
C3 C 0.5125(7) 0.1636(6) 0.2181(4) 0.072(2) Uani 1 1 d . . .
H3 H 0.4786 0.1355 0.2460 0.080(5) Uiso 1 1 calc R . .
C4 C 0.5158(6) 0.2749(5) 0.2086(4) 0.0487(17) Uani 1 1 d . . .
H4 H 0.4838 0.3223 0.2297 0.080(5) Uiso 1 1 calc R . .
C5 C 0.5677(5) 0.3143(5) 0.1671(3) 0.0355(14) Uani 1 1 d . . .
C6 C 0.5705(5) 0.4337(4) 0.1483(3) 0.0325(13) Uani 1 1 d . . .
C7 C 0.6906(5) 0.4889(4) 0.2104(3) 0.0295(13) Uani 1 1 d . . .
C8 C 0.7512(5) 0.4719(5) 0.2945(3) 0.0411(16) Uani 1 1 d . . .
H8 H 0.7207 0.4238 0.3162 0.080(5) Uiso 1 1 calc R . .
C9 C 0.8583(6) 0.5283(5) 0.3452(4) 0.0501(18) Uani 1 1 d . . .
H9 H 0.9021 0.5169 0.4015 0.080(5) Uiso 1 1 calc R . .
C10 C 0.8995(6) 0.6016(5) 0.3114(4) 0.0559(19) Uani 1 1 d . . .
H10 H 0.9706 0.6410 0.3444 0.080(5) Uiso 1 1 calc R . .
C11 C 0.8334(6) 0.6149(5) 0.2282(4) 0.0446(16) Uani 1 1 d . . .
H11 H 0.8609 0.6648 0.2056 0.080(5) Uiso 1 1 calc R . .
C12 C 0.9108(7) 0.3294(5) 0.2235(4) 0.0562(19) Uani 1 1 d . . .
H12 H 0.8773 0.2801 0.2425 0.080(5) Uiso 1 1 calc R . .
C13 C 1.0290(8) 0.3619(6) 0.2758(5) 0.074(2) Uani 1 1 d . . .
H13 H 1.0731 0.3375 0.3297 0.080(5) Uiso 1 1 calc R . .
C14 C 1.0817(7) 0.4306(6) 0.2478(5) 0.081(3) Uani 1 1 d . . .
H14 H 1.1626 0.4515 0.2818 0.080(5) Uiso 1 1 calc R . .
C15 C 1.0117(6) 0.4683(5) 0.1675(4) 0.0591(19) Uani 1 1 d . . .
H15 H 1.0449 0.5153 0.1470 0.080(5) Uiso 1 1 calc R . .
C16 C 0.8929(5) 0.4352(5) 0.1191(4) 0.0402(15) Uani 1 1 d . . .
C17 C 0.8061(5) 0.4710(4) 0.0297(3) 0.0352(14) Uani 1 1 d . . .
C18 C 0.8161(5) 0.5927(5) 0.0176(3) 0.0368(14) Uani 1 1 d . . .
C19 C 0.8961(6) 0.6370(6) -0.0004(4) 0.0532(18) Uani 1 1 d . . .
H19 H 0.9493 0.5918 -0.0049 0.080(5) Uiso 1 1 calc R . .
C20 C 0.8984(6) 0.7468(6) -0.0116(4) 0.062(2) Uani 1 1 d . . .
H20 H 0.9534 0.7768 -0.0228 0.080(5) Uiso 1 1 calc R . .
C21 C 0.8173(6) 0.8114(6) -0.0059(4) 0.0582(19) Uani 1 1 d . . .
H21 H 0.8156 0.8861 -0.0140 0.080(5) Uiso 1 1 calc R . .
C22 C 0.7380(5) 0.7636(5) 0.0121(3) 0.0431(16) Uani 1 1 d . . .
H22 H 0.6832 0.8076 0.0159 0.080(5) Uiso 1 1 calc R . .
C23 C 0.7720(6) 0.3914(6) -0.0938(5) 0.075(2) Uani 1 1 d . . .
H23A H 0.8118 0.3497 -0.1147 0.080(5) Uiso 1 1 calc R . .
H23B H 0.7464 0.4599 -0.1218 0.080(5) Uiso 1 1 calc R . .
H23C H 0.7023 0.3522 -0.1025 0.080(5) Uiso 1 1 calc R . .
C24 C 0.7823(7) 0.1398(6) 0.0097(4) 0.060(2) Uani 1 1 d . . .
C25 C 0.4390(6) 0.2283(6) -0.1071(4) 0.059(2) Uani 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'
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
O1 Co1 N6 106.87(15) . 3_665 ?
O1 Co1 N4 153.96(16) . . ?
N6 Co1 N4 98.91(18) 3_665 . ?
O1 Co1 O1 81.73(13) . 3_665 ?
N6 Co1 O1 81.81(16) 3_665 3_665 ?
N4 Co1 O1 105.95(14) . 3_665 ?
O1 Co1 N2 76.79(15) . . ?
N6 Co1 N2 92.31(17) 3_665 . ?
N4 Co1 N2 98.91(17) . . ?
O1 Co1 N2 155.04(15) 3_665 . ?
O1 Co1 O3 80.55(13) . . ?
N6 Co1 O3 164.48(16) 3_665 . ?
N4 Co1 O3 75.35(15) . . ?
O1 Co1 O3 85.92(12) 3_665 . ?
N2 Co1 O3 102.76(14) . . ?
N5 Co2 O3 109.04(19) . . ?
N5 Co2 N1 99.7(2) . . ?
O3 Co2 N1 149.25(16) . . ?
N5 Co2 N6 95.44(19) . . ?
O3 Co2 N6 93.33(15) . . ?
N1 Co2 N6 94.63(18) . . ?
N5 Co2 N3 88.66(19) . . ?
O3 Co2 N3 75.27(16) . . ?
N1 Co2 N3 95.17(18) . . ?
N6 Co2 N3 168.59(18) . . ?
N5 Co2 O1 170.18(18) . . ?
O3 Co2 O1 78.90(12) . . ?
N1 Co2 O1 73.82(15) . . ?
N6 Co2 O1 78.01(14) . . ?
N3 Co2 O1 99.16(14) . . ?
C6 O1 Co1 116.9(3) . . ?
C6 O1 Co1 129.8(3) . 3_665 ?
Co1 O1 Co1 98.27(13) . 3_665 ?
C6 O1 Co2 110.6(3) . . ?
Co1 O1 Co2 98.53(13) . . ?
Co1 O1 Co2 97.15(12) 3_665 . ?
C6 O2 H1O2 109.4 . . ?
C17 O3 Co2 117.7(3) . . ?
C17 O3 Co1 109.2(3) . . ?
Co2 O3 Co1 99.58(14) . . ?
C23 O4 C17 116.4(4) . . ?
C1 N1 C5 118.2(5) . . ?
C1 N1 Co2 123.4(4) . . ?
C5 N1 Co2 117.2(3) . . ?
C11 N2 C7 118.5(5) . . ?
C11 N2 Co1 127.5(4) . . ?
C7 N2 Co1 113.9(4) . . ?
C12 N3 C16 118.2(5) . . ?
C12 N3 Co2 127.7(5) . . ?
C16 N3 Co2 113.8(4) . . ?
C18 N4 C22 118.3(5) . . ?
C18 N4 Co1 116.0(4) . . ?
C22 N4 Co1 125.6(4) . . ?
C24 N5 Co2 153.1(6) . . ?
C25 N6 Co1 128.2(5) . 3_665 ?
C25 N6 Co2 129.6(5) . . ?
Co1 N6 Co2 101.66(19) 3_665 . ?
N1 C1 C2 122.8(6) . . ?
N1 C1 H1 118.6 . . ?
C2 C1 H1 118.6 . . ?
C1 C2 C3 119.0(6) . . ?
C1 C2 H2 120.5 . . ?
C3 C2 H2 120.5 . . ?
C2 C3 C4 119.7(7) . . ?
C2 C3 H3 120.2 . . ?
C4 C3 H3 120.1 . . ?
C3 C4 C5 118.8(6) . . ?
C3 C4 H4 120.7 . . ?
C5 C4 H4 120.6 . . ?
N1 C5 C4 121.4(5) . . ?
N1 C5 C6 114.5(5) . . ?
C4 C5 C6 124.0(5) . . ?
O1 C6 O2 109.8(4) . . ?
O1 C6 C5 108.1(4) . . ?
O2 C6 C5 109.1(4) . . ?
O1 C6 C7 110.2(4) . . ?
O2 C6 C7 106.8(4) . . ?
C5 C6 C7 112.8(4) . . ?
N2 C7 C8 121.8(5) . . ?
N2 C7 C6 114.7(5) . . ?
C8 C7 C6 123.4(5) . . ?
C9 C8 C7 118.3(6) . . ?
C9 C8 H8 120.8 . . ?
C7 C8 H8 120.9 . . ?
C10 C9 C8 119.5(6) . . ?
C10 C9 H9 120.2 . . ?
C8 C9 H9 120.3 . . ?
C11 C10 C9 118.5(6) . . ?
C11 C10 H10 120.8 . . ?
C9 C10 H10 120.7 . . ?
N2 C11 C10 123.3(6) . . ?
N2 C11 H11 118.4 . . ?
C10 C11 H11 118.3 . . ?
N3 C12 C13 122.6(7) . . ?
N3 C12 H12 118.7 . . ?
C13 C12 H12 118.7 . . ?
C14 C13 C12 119.5(7) . . ?
C14 C13 H13 120.2 . . ?
C12 C13 H13 120.3 . . ?
C13 C14 C15 118.7(7) . . ?
C13 C14 H14 120.7 . . ?
C15 C14 H14 120.6 . . ?
C16 C15 C14 119.0(7) . . ?
C16 C15 H15 120.5 . . ?
C14 C15 H15 120.5 . . ?
N3 C16 C15 121.9(6) . . ?
N3 C16 C17 114.0(5) . . ?
C15 C16 C17 124.1(6) . . ?
O3 C17 O4 113.7(4) . . ?
O3 C17 C18 108.6(4) . . ?
O4 C17 C18 109.9(5) . . ?
O3 C17 C16 111.1(5) . . ?
O4 C17 C16 101.2(4) . . ?
C18 C17 C16 112.3(5) . . ?
N4 C18 C19 121.0(5) . . ?
N4 C18 C17 114.7(5) . . ?
C19 C18 C17 124.3(6) . . ?
C20 C19 C18 121.0(6) . . ?
C20 C19 H19 119.5 . . ?
C18 C19 H19 119.5 . . ?
C21 C20 C19 118.2(6) . . ?
C21 C20 H20 120.8 . . ?
C19 C20 H20 120.9 . . ?
C20 C21 C22 119.0(6) . . ?
C20 C21 H21 120.5 . . ?
C22 C21 H21 120.5 . . ?
N4 C22 C21 122.5(6) . . ?
N4 C22 H22 118.7 . . ?
C21 C22 H22 118.8 . . ?
O4 C23 H23A 109.4 . . ?
O4 C23 H23B 109.4 . . ?
H23A C23 H23B 109.5 . . ?
O4 C23 H23C 109.6 . . ?
H23A C23 H23C 109.5 . . ?
H23B C23 H23C 109.5 . . ?
N5 C24 O5 177.8(8) . . ?
N6 C25 O6 178.1(8) . . ?
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 O1 2.025(3) . ?
Co1 N6 2.088(4) 3_665 ?
Co1 N4 2.096(4) . ?
Co1 O1 2.133(3) 3_665 ?
Co1 N2 2.162(4) . ?
Co1 O3 2.193(3) . ?
Co2 N5 2.025(5) . ?
Co2 O3 2.046(3) . ?
Co2 N1 2.135(4) . ?
Co2 N6 2.146(5) . ?
Co2 N3 2.217(5) . ?
Co2 O1 2.244(3) . ?
O1 C6 1.382(6) . ?
O1 Co1 2.133(3) 3_665 ?
O2 C6 1.416(6) . ?
O2 H1O2 0.8200 . ?
O3 C17 1.375(6) . ?
O4 C23 1.381(7) . ?
O4 C17 1.437(6) . ?
O5 C24 1.208(8) . ?
O6 C25 1.193(8) . ?
N1 C1 1.354(7) . ?
N1 C5 1.357(6) . ?
N2 C11 1.331(7) . ?
N2 C7 1.347(6) . ?
N3 C12 1.330(7) . ?
N3 C16 1.360(7) . ?
N4 C18 1.348(6) . ?
N4 C22 1.347(7) . ?
N5 C24 1.127(8) . ?
N6 C25 1.165(7) . ?
N6 Co1 2.088(4) 3_665 ?
C1 C2 1.360(9) . ?
C1 H1 0.9300 . ?
C2 C3 1.374(9) . ?
C2 H2 0.9300 . ?
C3 C4 1.385(8) . ?
C3 H3 0.9300 . ?
C4 C5 1.388(7) . ?
C4 H4 0.9300 . ?
C5 C6 1.519(7) . ?
C6 C7 1.527(7) . ?
C7 C8 1.391(7) . ?
C8 C9 1.385(8) . ?
C8 H8 0.9300 . ?
C9 C10 1.382(8) . ?
C9 H9 0.9300 . ?
C10 C11 1.367(8) . ?
C10 H10 0.9300 . ?
C11 H11 0.9300 . ?
C12 C13 1.372(9) . ?
C12 H12 0.9300 . ?
C13 C14 1.371(10) . ?
C13 H13 0.9300 . ?
C14 C15 1.393(9) . ?
C14 H14 0.9300 . ?
C15 C16 1.371(7) . ?
C15 H15 0.9300 . ?
C16 C17 1.537(8) . ?
C17 C18 1.532(7) . ?
C18 C19 1.378(7) . ?
C19 C20 1.371(8) . ?
C19 H19 0.9300 . ?
C20 C21 1.375(8) . ?
C20 H20 0.9300 . ?
C21 C22 1.388(7) . ?
C21 H21 0.9300 . ?
C22 H22 0.9300 . ?
C23 H23A 0.9600 . ?
C23 H23B 0.9600 . ?
C23 H23C 0.9600 . ?
