#------------------------------------------------------------------------------
#$Date: 2016-03-23 21:11:09 +0200 (Wed, 23 Mar 2016) $
#$Revision: 179443 $
#$URL: svn://www.crystallography.net/cod/cif/4/33/40/4334035.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_4334035
loop_
_publ_author_name
'Roberto Fernández de Luis'
'M. Karmele Urtiaga'
'José L. Mesa'
'Edurne S. Larrea'
'Marta Iglesias'
'Teófilo Rojo'
'María I. Arriortua'
_publ_contact_author_address
;   Facultad de Ciencia y Tecnología
   Dpto. de Mineralogía y Petrología 
   Universidad del País Vasco
   Apartado 644
   48080 Bilbao
   Spain
;
_publ_contact_author_email       maribel.arriortua@ehu.es
_publ_contact_author_fax         '34 4 4648500'
_publ_contact_author_name        'Dra. María Isabel Arriortua'
_publ_contact_author_phone       '34 4 6015372'
_publ_section_title
;
 Thermal Response, Catalytic Activity, and Color Change of the First
 Hybrid Vanadate Containing Bpe Guest Molecules
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              2615
_journal_page_last               2626
_journal_paper_doi               10.1021/ic302662x
_journal_volume                  52
_journal_year                    2013
_chemical_formula_sum            'C36 H42 Co2 N6 O18 V4'
_chemical_formula_weight         1168.38
_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_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             2012-02-07T13:25:32-00:00
_audit_creation_method           'WinGX routine CIF_UPDATE'
_cell_angle_alpha                96.8030(10)
_cell_angle_beta                 105.710(2)
_cell_angle_gamma                99.225(2)
_cell_formula_units_Z            1
_cell_length_a                   7.7745(2)
_cell_length_b                   11.46350(10)
_cell_length_c                   13.5377(2)
_cell_measurement_reflns_used    17697
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      32.3781
_cell_measurement_theta_min      2.7539
_cell_volume                     1129.67(4)
_computing_cell_refinement
;
        CrysAlis RED, Oxford Diffraction Ltd.,
        Version 1.171.32.15 (release 10-01-2008 CrysAlis171 .NET)
        (compiled Jan 10 2008,16:37:18)
;
_computing_data_collection
;
        CrysAlis CCD, Oxford Diffraction Ltd.,
        Version 1.171.32.15 (release 10-01-2008 CrysAlis171 .NET)
        (compiled Jan 10 2008,16:37:18)
;
_computing_data_reduction
;
        CrysAlis RED, Oxford Diffraction Ltd.,
        Version 1.171.32.15 (release 10-01-2008 CrysAlis171 .NET)
        (compiled Jan 10 2008,16:37:18)
;
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_diffrn_ambient_temperature      293(2)
_diffrn_detector_area_resol_mean 8.3504
_diffrn_measured_fraction_theta_full 0.923
_diffrn_measured_fraction_theta_max 0.923
_diffrn_orient_matrix_UB_11      -0.0904343484
_diffrn_orient_matrix_UB_12      0.0099949731
_diffrn_orient_matrix_UB_13      -0.011223776
_diffrn_orient_matrix_UB_21      0.0342517762
_diffrn_orient_matrix_UB_22      0.062156795
_diffrn_orient_matrix_UB_23      0.018889343
_diffrn_orient_matrix_UB_31      0.0016154715
_diffrn_orient_matrix_UB_32      0.0091110154
_diffrn_orient_matrix_UB_33      -0.0506542102
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0386
_diffrn_reflns_av_unetI/netI     0.0304
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            33349
_diffrn_reflns_theta_full        32.43
_diffrn_reflns_theta_max         32.43
_diffrn_reflns_theta_min         2.76
_exptl_absorpt_coefficient_mu    1.59
_exptl_absorpt_correction_T_max  0.79
_exptl_absorpt_correction_T_min  0.452
_exptl_absorpt_correction_type   analytical
_exptl_absorpt_process_details
;
        CrysAlis RED, Oxford Diffraction Ltd.,
        Version 1.171.32.15 (release 10-01-2008 CrysAlis171 .NET)
        (compiled Jan 10 2008,16:37:18)
Analytical numeric absorption correction using a multifaceted crystal
                        model based on expressions derived by R.C. Clark & J.S.
        (Clark, R. C. & Reid, J. S. (1995). Acta Cryst. A51, 887-897)
;
_exptl_crystal_density_diffrn    1.717
_exptl_crystal_F_000             590
_exptl_crystal_size_max          0.8316
_exptl_crystal_size_mid          0.3091
_exptl_crystal_size_min          0.1764
_refine_diff_density_max         1.286
_refine_diff_density_min         -0.382
_refine_diff_density_rms         0.105
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.02
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     317
_refine_ls_number_reflns         7514
_refine_ls_number_restraints     18
_refine_ls_restrained_S_all      1.02
_refine_ls_R_factor_all          0.0452
_refine_ls_R_factor_gt           0.0325
_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)+(0.0558P)²+0.0000P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.082
_refine_ls_wR_factor_ref         0.0863
_reflns_number_gt                5961
_reflns_number_total             7514
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic302662x_si_003.cif
_cod_data_source_block           CoBpeBpe
_cod_original_cell_volume        1129.67(3)
_cod_database_code               4334035
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
N1 N 0.0244(2) -0.00610(12) 0.15741(10) 0.0217(3) Uani 1 1 d . . .
C1 C -0.0361(3) 0.07378(17) 0.21265(14) 0.0334(4) Uani 1 1 d . . .
H1 H -0.0781 0.1361 0.1816 0.04 Uiso 1 1 calc R . .
C2 C -0.0393(3) 0.06843(19) 0.31310(14) 0.0384(5) Uani 1 1 d . . .
H2 H -0.082 0.1264 0.3487 0.046 Uiso 1 1 calc R . .
C3 C 0.0219(3) -0.02451(18) 0.36118(13) 0.0307(4) Uani 1 1 d . . .
C4 C 0.0853(3) -0.10696(17) 0.30377(13) 0.0306(4) Uani 1 1 d . . .
H4 H 0.1271 -0.1707 0.3324 0.037 Uiso 1 1 calc R . .
C5 C 0.0858(2) -0.09375(15) 0.20336(12) 0.0241(3) Uani 1 1 d . . .
H5 H 0.1313 -0.1488 0.1665 0.029 Uiso 1 1 calc R . .
C6 C 0.0202(3) -0.0382(2) 0.46695(14) 0.0399(5) Uani 1 1 d . . .
H6 H 0.0508 -0.1077 0.4895 0.048 Uiso 1 1 calc R . .
N2 N 0.5014(3) 0.10679(17) 0.35411(16) 0.0470(5) Uani 1 1 d . . .
C7 C 0.5455(4) 0.1544(2) 0.4541(2) 0.0567(7) Uani 1 1 d . . .
H7 H 0.5852 0.1063 0.5028 0.068 Uiso 1 1 calc R . .
C8 C 0.5367(4) 0.2697(2) 0.49073(16) 0.0524(7) Uani 1 1 d . . .
H8 H 0.5687 0.2971 0.562 0.063 Uiso 1 1 calc R . .
C9 C 0.4796(3) 0.34500(17) 0.42058(14) 0.0321(4) Uani 1 1 d . . .
C10 C 0.4330(3) 0.2952(2) 0.31605(15) 0.0408(5) Uani 1 1 d . . .
H10 H 0.3934 0.3411 0.2654 0.049 Uiso 1 1 calc R . .
C11 C 0.4450(3) 0.1782(2) 0.28670(17) 0.0455(5) Uani 1 1 d . . .
H11 H 0.4118 0.1475 0.216 0.055 Uiso 1 1 calc R . .
C12 C 0.4708(2) 0.46924(15) 0.45099(12) 0.0342(4) Uani 1 1 d . . .
H12 H 0.4205 0.5098 0.3982 0.041 Uiso 1 1 calc R . .
N3A N 0.3239(2) 0.50235(15) -0.14954(12) 0.0190(4) Uani 0.775(5) 1 d PRD A 1
C13A C 0.2909(2) 0.41293(15) -0.23002(12) 0.0291(3) Uani 0.775(5) 1 d PRD A 1
H13A H 0.3367 0.3443 -0.2173 0.035 Uiso 0.775(5) 1 d PR A 1
C14A C 0.1926(4) 0.4193(3) -0.3322(2) 0.0291(3) Uani 0.775(5) 1 d PD A 1
H14A H 0.1805 0.358 -0.3866 0.035 Uiso 0.775(5) 1 calc PR A 1
C15A C 0.1132(4) 0.5184(3) -0.35140(19) 0.0291(3) Uani 0.775(5) 1 d PD A 1
C16A C 0.1409(4) 0.6063(3) -0.2655(2) 0.0291(3) Uani 0.775(5) 1 d PD A 1
H16A H 0.0864 0.6725 -0.2734 0.035 Uiso 0.775(5) 1 calc PR A 1
C17A C 0.2485(5) 0.5964(3) -0.1685(2) 0.0291(3) Uani 0.775(5) 1 d PD A 1
H17A H 0.2692 0.659 -0.1136 0.035 Uiso 0.775(5) 1 calc PR A 1
N3B N 0.3335(13) 0.4897(9) -0.1597(7) 0.0190(4) Uani 0.225(5) 1 d PD A 2
C13B C 0.3148(14) 0.3982(9) -0.2284(7) 0.0336(13) Uani 0.225(5) 1 d PD A 2
H13B H 0.3832 0.3406 -0.2091 0.04 Uiso 0.225(5) 1 calc PR A 2
C14B C 0.2035(14) 0.3790(10) -0.3266(7) 0.0336(13) Uani 0.225(5) 1 d PD A 2
H14B H 0.1796 0.305 -0.3695 0.04 Uiso 0.225(5) 1 calc PR A 2
C15B C 0.1252(13) 0.4729(10) -0.3623(6) 0.0336(13) Uani 0.225(5) 1 d PD A 2
C16B C 0.1351(13) 0.5699(9) -0.2931(7) 0.0336(13) Uani 0.225(5) 1 d PD A 2
H16B H 0.077 0.6315 -0.3144 0.04 Uiso 0.225(5) 1 calc PR A 2
C17B C 0.2363(18) 0.5775(11) -0.1862(8) 0.0336(13) Uani 0.225(5) 1 d PD A 2
H17B H 0.2363 0.6403 -0.1359 0.04 Uiso 0.225(5) 1 calc PR A 2
C18A C 0.0063(3) 0.5330(2) -0.45466(17) 0.0291(3) Uani 0.775(5) 1 d P . 1
H18A H -0.0591 0.5943 -0.4573 0.035 Uiso 0.775(5) 1 calc PR A 1
C18B C 0.0275(12) 0.4643(9) -0.4767(6) 0.0336(13) Uani 0.225(5) 1 d P . 2
H18B H 0.0085 0.3888 -0.5164 0.04 Uiso 0.225(5) 1 calc PR A 2
Co1 Co 0.5 0.5 0 0.01350(6) Uani 1 2 d S . .
Co2 Co 0 0 0 0.01331(6) Uani 1 2 d S . .
O1 O 0.34591(16) 0.59634(10) 0.06739(9) 0.0227(2) Uani 1 1 d . A .
O2 O 0.34944(15) 0.33652(10) 0.01021(9) 0.0199(2) Uani 1 1 d . A .
O3 O -0.00154(16) 0.36742(11) -0.08305(9) 0.0234(2) Uani 1 1 d . . .
O4 O 0.06195(17) 0.18436(10) 0.03318(9) 0.0241(2) Uani 1 1 d . A .
O5 O 0.15265(17) 0.42152(10) 0.14120(8) 0.0222(2) Uani 1 1 d . A .
O6 O 0.30457(18) 0.65558(11) 0.25644(9) 0.0296(3) Uani 1 1 d . . .
O7 O 0.27553(19) 0.00080(15) 0.02469(12) 0.0323(3) Uani 1 1 d . . .
V1 V 0.14243(3) 0.32339(2) 0.025226(19) 0.01429(6) Uani 1 1 d . . .
V2 V 0.20555(3) 0.58047(2) 0.139561(18) 0.01411(6) Uani 1 1 d . . .
O1W O 0.5301(2) 0.86097(14) 0.07546(15) 0.0406(4) Uani 1 1 d D . .
O2W O 0.5626(3) 0.87488(17) 0.28218(16) 0.0531(4) Uani 1 1 d D . .
HW4 H 0.553(4) 0.9383(19) 0.310(2) 0.048(8) Uiso 1 1 d D . .
HW1 H 0.544(5) 0.798(2) 0.054(3) 0.087(12) Uiso 1 1 d D . .
HW2 H 0.551(5) 0.870(3) 0.1371(15) 0.092(13) Uiso 1 1 d D . .
HW3 H 0.492(4) 0.820(2) 0.288(3) 0.078(11) Uiso 1 1 d D . .
HW5 H 0.309(4) -0.058(3) 0.024(2) 0.057(9) Uiso 1 1 d . . .
HW6 H 0.330(4) 0.045(3) -0.006(2) 0.055(8) 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 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'
O O 0.0106 0.006 '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'
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
C5 N1 C1 117.55(14) . .
C5 N1 Co2 121.91(11) . .
C1 N1 Co2 120.31(12) . .
N1 C1 C2 123.27(17) . .
C1 C2 C3 119.50(17) . .
C4 C3 C2 117.07(15) . .
C4 C3 C6 119.84(18) . .
C2 C3 C6 123.08(18) . .
C5 C4 C3 119.54(17) . .
N1 C5 C4 123.05(16) . .
C6 C6 C3 126.3(3) 2_556 .
C7 N2 C11 115.9(2) . .
N2 C7 C8 124.7(2) . .
C7 C8 C9 119.6(2) . .
C10 C9 C8 115.76(19) . .
C10 C9 C12 120.21(18) . .
C8 C9 C12 124.02(17) . .
C11 C10 C9 120.5(2) . .
N2 C11 C10 123.5(2) . .
C12 C12 C9 125.62(19) 2_666 .
C17A N3A C13A 117.05(13) . .
C17A N3A Co1 120.64(15) . .
C13A N3A Co1 122.2 . .
N3A C13A C14A 122.94(13) . .
C15A C14A C13A 119.5(2) . .
C16A C15A C14A 116.1(2) . .
C16A C15A C18A 120.1(2) . .
C14A C15A C18A 123.8(2) . .
C17A C16A C15A 120.7(2) . .
N3A C17A C16A 123.5(2) . .
C13B N3B C17B 119.0(7) . .
C13B N3B Co1 120.5(6) . .
C17B N3B Co1 120.4(7) . .
N3B C13B C14B 124.9(9) . .
C13B C14B C15B 118.2(8) . .
C16B C15B C14B 118.8(8) . .
C16B C15B C18B 120.8(9) . .
C14B C15B C18B 120.4(8) . .
C15B C16B C17B 119.3(9) . .
N3B C17B C16B 118.4(9) . .
C18A C18A C15A 126.4(3) 2_564 .
C18B C18B C15B 131.0(12) 2_564 .
O1 Co1 O1 180.00(6) 2_665 .
O1 Co1 O2 92.34(4) 2_665 2_665
O1 Co1 O2 87.66(4) . 2_665
O1 Co1 O2 87.66(4) 2_665 .
O1 Co1 O2 92.34(4) . .
O2 Co1 O2 180 2_665 .
O1 Co1 N3A 90.18(6) 2_665 .
O1 Co1 N3A 89.82(6) . .
O2 Co1 N3A 87.74(6) 2_665 .
O2 Co1 N3A 92.26(6) . .
O1 Co1 N3A 89.82(6) 2_665 2_665
O1 Co1 N3A 90.18(6) . 2_665
O2 Co1 N3A 92.26(6) 2_665 2_665
O2 Co1 N3A 87.74(6) . 2_665
N3A Co1 N3A 180.00(10) . 2_665
O1 Co1 N3B 95.5(3) 2_665 2_665
O1 Co1 N3B 84.5(3) . 2_665
O2 Co1 N3B 91.1(3) 2_665 2_665
O2 Co1 N3B 88.9(3) . 2_665
N3A Co1 N3B 174.2(3) . 2_665
N3A Co1 N3B 5.8(3) 2_665 2_665
O1 Co1 N3B 84.5(3) 2_665 .
O1 Co1 N3B 95.5(3) . .
O2 Co1 N3B 88.9(3) 2_665 .
O2 Co1 N3B 91.1(3) . .
N3A Co1 N3B 5.8(3) . .
N3A Co1 N3B 174.2(3) 2_665 .
N3B Co1 N3B 180.0(5) 2_665 .
O4 Co2 O4 180 2 .
O4 Co2 O7 91.16(6) 2 .
O4 Co2 O7 88.84(6) . .
O4 Co2 O7 88.84(6) 2 2
O4 Co2 O7 91.16(6) . 2
O7 Co2 O7 180.00(9) . 2
O4 Co2 N1 89.85(5) 2 2
O4 Co2 N1 90.15(5) . 2
O7 Co2 N1 88.55(6) . 2
O7 Co2 N1 91.45(6) 2 2
O4 Co2 N1 90.15(5) 2 .
O4 Co2 N1 89.85(5) . .
O7 Co2 N1 91.45(6) . .
O7 Co2 N1 88.55(6) 2 .
N1 Co2 N1 180.00(12) 2 .
V2 O1 Co1 140.48(7) . .
V1 O2 Co1 122.37(6) . .
V1 O3 V2 149.22(7) . 2_565
V1 O4 Co2 159.49(7) . .
V1 O5 V2 116.36(6) . .
O4 V1 O2 110.68(6) . .
O4 V1 O3 110.05(6) . .
O2 V1 O3 108.16(6) . .
O4 V1 O5 109.70(5) . .
O2 V1 O5 109.49(6) . .
O3 V1 O5 108.72(5) . .
O4 V1 V2 141.10(4) . .
O2 V1 V2 95.16(4) . .
O3 V1 V2 87.44(4) . .
O5 V1 V2 31.94(3) . .
O6 V2 O1 110.02(6) . .
O6 V2 O3 109.38(6) . 2_565
O1 V2 O3 110.56(6) . 2_565
O6 V2 O5 111.12(6) . .
O1 V2 O5 105.49(6) . .
O3 V2 O5 110.22(6) 2_565 .
O6 V2 V1 137.88(5) . .
O1 V2 V1 78.72(4) . .
O3 V2 V1 105.05(4) 2_565 .
O5 V2 V1 31.70(3) . .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
N1 C5 1.329(2) .
N1 C1 1.336(2) .
N1 Co2 2.0982(12) .
C1 C2 1.375(2) .
C2 C3 1.394(3) .
C3 C4 1.387(3) .
C3 C6 1.462(2) .
C4 C5 1.387(2) .
C6 C6 1.311(4) 2_556
N2 C7 1.327(3) .
N2 C11 1.331(3) .
C7 C8 1.375(3) .
C8 C9 1.390(3) .
C9 C10 1.387(3) .
C9 C12 1.453(3) .
C10 C11 1.378(3) .
C12 C12 1.347(3) 2_666
N3A C17A 1.326(3) .
N3A C13A 1.3429 .
N3A Co1 2.1205(16) .
C13A C14A 1.405(3) .
C14A C15A 1.395(3) .
C15A C16A 1.390(3) .
C15A C18A 1.464(3) .
C16A C17A 1.381(3) .
N3B C13B 1.278(11) .
N3B C17B 1.377(13) .
N3B Co1 2.176(8) .
C13B C14B 1.346(10) .
C14B C15B 1.391(11) .
C15B C16B 1.344(11) .
C15B C18B 1.513(11) .
C16B C17B 1.432(10) .
C18A C18A 1.334(5) 2_564
C18B C18B 1.156(18) 2_564
Co1 O1 2.0651(11) 2_665
Co1 O1 2.0651(11) .
Co1 O2 2.0849(11) 2_665
Co1 O2 2.0849(11) .
Co1 N3A 2.1205(16) 2_665
Co1 N3B 2.176(8) 2_665
Co2 O4 2.0572(11) 2
Co2 O4 2.0572(11) .
Co2 O7 2.0750(14) .
Co2 O7 2.0750(14) 2
Co2 N1 2.0982(12) 2
O1 V2 1.6535(11) .
O2 V1 1.6616(11) .
O3 V1 1.7675(11) .
O3 V2 1.7924(11) 2_565
O4 V1 1.6434(11) .
O5 V1 1.7949(11) .
O5 V2 1.8067(11) .
O6 V2 1.6256(11) .
V1 V2 3.0603(3) .
V2 O3 1.7924(11) 2_565
