#------------------------------------------------------------------------------
#$Date: 2016-02-16 02:10:39 +0100 (mar 16 de feb de 2016) $
#$Revision: 176453 $
#$URL: svn://www.crystallography.net/cod/cif/7/20/66/7206610.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_7206610
loop_
_publ_author_name
'Fernández de Luis, Roberto'
'Urtiaga, M. Karmele'
'Mesa, José L.'
'Segura, Joseba Orive Gómez de'
'Rojo, Teófilo'
'Arriortua, María I.'
_publ_section_title
;
 {Co(HBpe)2}(V4O12): pedal motion induced order--disorder P\=1→
 C\=1 transition and disrupted C\=1→ C2/m displacive transition
 due to thermal instability
;
_journal_issue                   21
_journal_name_full               CrystEngComm
_journal_page_first              6488
_journal_paper_doi               10.1039/c1ce05418j
_journal_volume                  13
_journal_year                    2011
_chemical_compound_source        'synthesis as described'
_chemical_formula_moiety         'C6 H5.50 Co0.25 N O3 V'
_chemical_formula_sum            'C6 H5.5 Co0.25 N O3 V'
_chemical_formula_weight         205.29
_chemical_name_systematic
;
?
;
_space_group_IT_number           12
_symmetry_cell_setting           monoclinic
_symmetry_Int_Tables_number      12
_symmetry_space_group_name_Hall  '-C 2y'
_symmetry_space_group_name_H-M   'C 1 2/m 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_conform_dict_location     ftp://ftp.iucr.org/pub/cif_core.dic
_audit_conform_dict_name         cif_core.dic
_audit_conform_dict_version      2.3
_audit_creation_date             2010-04-22T10:10:58-00:00
_audit_creation_method           'WinGX routine CIF_UPDATE'
_cell_angle_alpha                90
_cell_angle_beta                 94.95(2)
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   15.404(5)
_cell_length_b                   12.082(4)
_cell_length_c                   7.885(2)
_cell_measurement_reflns_used    279
_cell_measurement_temperature    533(2)
_cell_measurement_theta_max      28.39
_cell_measurement_theta_min      3.2722
_cell_volume                     1462.0(8)
_computing_cell_refinement
;
CrysAlisPro, Oxford Diffraction Ltd.,
Version 1.171.33.42 (release 29-05-2009 CrysAlis171 .NET)
(compiled May 29 2009,17:40:42)
;
_computing_data_collection
;
CrysAlisPro, Oxford Diffraction Ltd.,
Version 1.171.33.42 (release 29-05-2009 CrysAlis171 .NET)
(compiled May 29 2009,17:40:42)
;
_computing_data_reduction
;
CrysAlisPro, Oxford Diffraction Ltd.,
Version 1.171.33.42 (release 29-05-2009 CrysAlis171 .NET)
(compiled May 29 2009,17:40:42)
;
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SIR-92 (Altomare, 1993)'
_diffrn_ambient_temperature      533(2)
_diffrn_detector_area_resol_mean 8.3504
_diffrn_measured_fraction_theta_full 0.651
_diffrn_measured_fraction_theta_max 0.628
_diffrn_measurement_device_type  'Xcalibur, Sapphire2, large Be window'
_diffrn_measurement_method       'ω scans'
_diffrn_orient_matrix_UB_11      0.0362831258
_diffrn_orient_matrix_UB_12      -0.0359880599
_diffrn_orient_matrix_UB_13      -0.0010417424
_diffrn_orient_matrix_UB_21      -0.0285889773
_diffrn_orient_matrix_UB_22      -0.0461605312
_diffrn_orient_matrix_UB_23      0.0099284599
_diffrn_orient_matrix_UB_31      0.0005257056
_diffrn_orient_matrix_UB_32      -0.0046892681
_diffrn_orient_matrix_UB_33      -0.0898046041
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.111
_diffrn_reflns_av_unetI/netI     0.1663
_diffrn_reflns_limit_h_max       6
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -1
_diffrn_reflns_limit_l_max       7
_diffrn_reflns_limit_l_min       -8
_diffrn_reflns_number            1087
_diffrn_reflns_theta_full        25.24
_diffrn_reflns_theta_max         26.36
_diffrn_reflns_theta_min         3.28
_exptl_absorpt_coefficient_mu    1.856
_exptl_absorpt_correction_T_max  1
_exptl_absorpt_correction_T_min  0.85477
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro, Oxford Diffraction Ltd.,
Version 1.171.33.42 (release 29-05-2009 CrysAlis171 .NET)
(compiled May 29 2009,17:40:42)
Empirical absorption correction using spherical harmonics,
implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            Red
_exptl_crystal_density_diffrn    1.865
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       Prism
_exptl_crystal_F_000             818
_exptl_crystal_size_max          0.2828
_exptl_crystal_size_mid          0.1283
_exptl_crystal_size_min          0.0586
_refine_diff_density_max         0.485
_refine_diff_density_min         -0.469
_refine_diff_density_rms         0.108
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.843
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     96
_refine_ls_number_reflns         988
_refine_ls_number_restraints     5
_refine_ls_restrained_S_all      0.842
_refine_ls_R_factor_all          0.1659
_refine_ls_R_factor_gt           0.0609
_refine_ls_shift/su_max          0
_refine_ls_shift/su_mean         0
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[σ²(Fo²)+(0.0581P)²+0.0000P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1207
_refine_ls_wR_factor_ref         0.1476
_reflns_number_gt                381
_reflns_number_total             988
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c1ce05418j.txt
_cod_data_source_block           CoHBpe533K
_cod_original_sg_symbol_H-M      'C 2/m'
_cod_original_formula_sum        'C6 H5.50 Co0.25 N O3 V'
_cod_database_code               7206610
#BEGIN Tags that were not found in dictionaries:
_cell_oxdiff_length_a            15.404(5)
_cell_oxdiff_length_b            12.082(4)
_cell_oxdiff_length_c            7.885(2)
_cell_oxdiff_angle_alpha         90.11(2)
_cell_oxdiff_angle_beta          85.05(2)
_cell_oxdiff_angle_gamma         90.31(2)
_cell_oxdiff_volume              1461.9(8)
#END Tags that were not found in dictionaries
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, y, -z'
'x+1/2, y+1/2, z'
'-x+1/2, y+1/2, -z'
'-x, -y, -z'
'x, -y, z'
'-x+1/2, -y+1/2, -z'
'x+1/2, -y+1/2, 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 0 0 0.0492(11) Uani 1 4 d SD . .
V2 V 0.08058(10) 0.13203(16) 0.3654(3) 0.0475(7) Uani 1 1 d . . .
O3 O 0.0378(4) 0.1253(6) 0.1658(9) 0.065(2) Uani 1 1 d . . .
O4 O 0.1284(5) 0 0.4239(14) 0.055(3) Uani 1 2 d S . .
O6 O 0.1552(4) 0.2219(6) 0.3773(12) 0.075(3) Uani 1 1 d . . .
O8 O 0 0.1718(10) 0.5 0.094(5) Uani 1 2 d S . .
N1 N 0.1299(7) 0 -0.0815(19) 0.065(4) Uani 1 2 d SD . .
C1A C 0.1614(11) -0.1011(15) -0.098(5) 0.066(3) Uani 0.5 1 d PD A 1
H1A H 0.1252 -0.1624 -0.0943 0.079 Uiso 0.5 1 calc PR A 1
C1B C 0.1833(11) 0.0855(16) -0.089(4) 0.066(3) Uani 0.5 1 d PD A 2
H1B H 0.166 0.1564 -0.0606 0.079 Uiso 0.5 1 calc PR A 2
C2A C 0.2480(11) -0.114(2) -0.122(4) 0.066(3) Uani 0.5 1 d PD . .
H2A H 0.2697 -0.1861 -0.1171 0.079 Uiso 0.5 1 calc PR A 1
C2B C 0.2651(10) 0.066(2) -0.141(4) 0.066(3) Uani 0.5 1 d PD . .
H2B H 0.2961 0.1283 -0.1715 0.079 Uiso 0.5 1 calc PR A 2
C3 C 0.3052(11) 0.0319(19) -0.153(3) 0.066(3) Uani 0.5 1 d P . .
C4 C 0.3888(10) -0.0434(16) -0.189(3) 0.066(3) Uani 0.5 1 d P . .
H4 H 0.4093 -0.1156 -0.1939 0.079 Uiso 0.5 1 calc PR . .
C5 C 0.4442(10) 0.0345(18) -0.216(3) 0.066(3) Uani 0.5 1 d P . .
H5 H 0.4301 0.1087 -0.2035 0.079 Uiso 0.5 1 calc PR . .
C6 C 0.5340(9) 0 -0.271(3) 0.066(3) Uani 1 2 d S . .
C7A C 0.5865(16) 0.111(3) -0.286(4) 0.066(3) Uani 0.5 1 d P . .
H7A H 0.564 0.1803 -0.2645 0.079 Uiso 0.5 1 calc PR . .
C7B C 0.5687(13) 0.073(3) -0.299(5) 0.066(3) Uani 0.5 1 d P . .
H7B H 0.5374 0.1385 -0.2939 0.079 Uiso 0.5 1 calc PR . .
C8A C 0.6498(17) 0.098(3) -0.324(6) 0.066(3) Uani 0.5 1 d P . .
H8A H 0.6809 0.1629 -0.3365 0.079 Uiso 0.5 1 calc PR . .
C8B C 0.6714(16) 0.087(3) -0.351(6) 0.066(3) Uani 0.5 1 d P . .
H8B H 0.7011 0.1528 -0.3679 0.079 Uiso 0.5 1 calc PR . .
N2 N 0.6968(8) 0 -0.360(2) 0.072(5) Uani 1 2 d S . .
H2 H 0.7487 0.0081 -0.3904 0.087 Uiso 0.5 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 0 '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 0.006 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
V V 0.3005 0.5294 '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
O3 Co1 O3 180.0(4) . 5
O3 Co1 O3 95.1(4) . 6
O3 Co1 O3 84.9(4) 5 6
O3 Co1 O3 84.9(4) . 2
O3 Co1 O3 95.1(4) 5 2
O3 Co1 O3 180.0(5) 6 2
O3 Co1 N1 91.7(3) . 5
O3 Co1 N1 88.3(3) 5 5
O3 Co1 N1 91.7(3) 6 5
O3 Co1 N1 88.3(3) 2 5
O3 Co1 N1 88.3(3) . .
O3 Co1 N1 91.7(3) 5 .
O3 Co1 N1 88.3(3) 6 .
O3 Co1 N1 91.7(3) 2 .
N1 Co1 N1 180.0(8) 5 .
O3 Co1 N1 88.3(3) . 6
O3 Co1 N1 91.7(3) 5 6
O3 Co1 N1 88.3(3) 6 6
O3 Co1 N1 91.7(3) 2 6
N1 Co1 N1 180.0(8) 5 6
N1 Co1 N1 0.0(8) . 6
O6 V2 O3 108.6(4) . .
O6 V2 O8 108.9(4) . .
O3 V2 O8 110.0(2) . .
O6 V2 O4 108.3(3) . .
O3 V2 O4 108.7(4) . .
O8 V2 O4 112.3(5) . .
V2 O3 Co1 135.3(4) . .
V2 O4 V2 124.8(5) 6 .
V2 O8 V2 148.5(7) . 2_556
C1A N1 C1B 118.7(14) . .
C1A N1 Co1 112.8(11) . .
C1B N1 Co1 127.6(10) . .
N1 C1A C2A 119(2) . .
N1 C1B C2B 118(2) . .
C3 C2A C1A 126(2) 6 .
C3 C2B C1B 127(2) 6 .
C3 C2B C4 54.0(10) 6 6
C1B C2B C4 173(3) . 6
C3 C3 C2A 136.8(13) 6 6
C2B C3 C2A 108.9(16) 6 6
C3 C3 C4 95.9(13) 6 6
C2B C3 C4 123.9(18) 6 6
C2A C3 C4 127(2) 6 6
C5 C4 C3 127.7(19) . 6
C5 C4 C2B 141.6(15) . 6
C4 C5 C6 117.9(15) . .
C7B C6 C5 108.2(19) 6 6
C7B C6 C5 140(2) 6 .
C7B C6 C7A 114.7(18) 6 .
C5 C6 C7A 137.0(15) 6 .
C5 C6 C7A 105.7(15) . .
C5 C6 C7A 105.7(15) 6 6
C5 C6 C7A 137.0(15) . 6
C7A C6 C7A 116(2) . 6
C8A C7A C6 113(3) . .
C6 C7B C8B 130(3) 6 .
C7A C8A N2 132(4) . .
N2 C8B C7B 105(3) 6 .
C8B N2 C8A 125.2(17) 6 .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
Co1 O3 2.051(7) .
Co1 O3 2.051(7) 5
Co1 O3 2.051(7) 6
Co1 O3 2.051(7) 2
Co1 N1 2.154(12) 5
Co1 N1 2.154(12) .
Co1 N1 2.154(12) 6
V2 O6 1.578(6) .
V2 O3 1.655(7) .
V2 O8 1.768(4) .
V2 O4 1.800(4) .
O4 V2 1.800(4) 6
O8 V2 1.768(4) 2_556
N1 C1A 1.325(16) .
N1 C1B 1.325(16) .
C1A C2A 1.372(16) .
C1B C2B 1.379(17) .
C2A C3 1.36(3) 6
C2B C3 1.345(15) 6
C3 C3 0.77(5) 6
C3 C2B 1.345(15) 6
C3 C2A 1.36(3) 6
C3 C4 1.35(2) 6
C4 C5 1.30(2) .
C4 C3 1.35(2) 6
C5 C6 1.54(2) .
C6 C7B 1.06(2) 6
C6 C5 1.54(2) 6
C6 C7A 1.57(2) .
C6 C7A 1.57(2) 6
C7A C8A 1.06(3) .
C7B C6 1.06(2) 6
C7B C8B 1.68(4) .
C8A N2 1.43(3) .
C8B N2 1.13(4) 6
N2 C8B 1.13(4) 6
