#------------------------------------------------------------------------------
#$Date: 2016-03-23 21:11:09 +0200 (Wed, 23 Mar 2016) $
#$Revision: 179443 $
#$URL: svn://www.crystallography.net/cod/cif/4/33/40/4334036.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_4334036
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 N6 Ni2 O18 V4'
_chemical_formula_weight         1167.94
_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             2012-04-17T10:45:27-00:00
_audit_creation_method           'WinGX routine CIF_UPDATE'
_cell_angle_alpha                96.395(2)
_cell_angle_beta                 105.619(3)
_cell_angle_gamma                99.339(3)
_cell_formula_units_Z            1
_cell_length_a                   7.7086(3)
_cell_length_b                   11.4007(4)
_cell_length_c                   13.4990(3)
_cell_measurement_reflns_used    7137
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      76.3072
_cell_measurement_theta_min      3.9797
_cell_volume                     1112.28(7)
_computing_cell_refinement
;
        CrysAlisPro, Agilent Technologies,
        Version 1.171.35.11 (release 16-05-2011 CrysAlis171 .NET)
        (compiled May 16 2011,17:55:39)
;
_computing_data_collection
;
        CrysAlisPro, Agilent Technologies,
        Version 1.171.35.11 (release 16-05-2011 CrysAlis171 .NET)
        (compiled May 16 2011,17:55:39)
;
_computing_data_reduction
;
        CrysAlisPro, Agilent Technologies,
        Version 1.171.35.11 (release 16-05-2011 CrysAlis171 .NET)
        (compiled May 16 2011,17:55:39)
;
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_diffrn_ambient_temperature      293(2)
_diffrn_detector_area_resol_mean 5.2012
_diffrn_measured_fraction_theta_full 0.975
_diffrn_measured_fraction_theta_max 0.975
_diffrn_measurement_device_type  'SuperNova, Single source at offset), Atlas'
_diffrn_measurement_method       'ω scans'
_diffrn_orient_matrix_UB_11      -0.1098508
_diffrn_orient_matrix_UB_12      -0.1234658
_diffrn_orient_matrix_UB_13      -0.062439
_diffrn_orient_matrix_UB_21      0.1802896
_diffrn_orient_matrix_UB_22      -0.0466047
_diffrn_orient_matrix_UB_23      0.0130966
_diffrn_orient_matrix_UB_31      -0.0173482
_diffrn_orient_matrix_UB_32      -0.0430222
_diffrn_orient_matrix_UB_33      0.1017656
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.5418
_diffrn_reflns_av_R_equivalents  0.0238
_diffrn_reflns_av_unetI/netI     0.0288
_diffrn_reflns_limit_h_max       8
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       -12
_diffrn_reflns_number            8762
_diffrn_reflns_theta_full        76.5
_diffrn_reflns_theta_max         76.5
_diffrn_reflns_theta_min         4.82
_exptl_absorpt_coefficient_mu    8.388
_exptl_absorpt_correction_T_max  0.445
_exptl_absorpt_correction_T_min  0.179
_exptl_absorpt_correction_type   analytical
_exptl_absorpt_process_details
;
        CrysAlisPro, Agilent Technologies,
        Version 1.171.35.11 (release 16-05-2011 CrysAlis171 .NET)
        (compiled May 16 2011,17:55:39)
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    1.744
_exptl_crystal_F_000             592
_exptl_crystal_size_max          0.3129
_exptl_crystal_size_mid          0.2418
_exptl_crystal_size_min          0.1404
_refine_diff_density_max         0.51
_refine_diff_density_min         -0.772
_refine_diff_density_rms         0.098
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.075
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     320
_refine_ls_number_reflns         4545
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.075
_refine_ls_R_factor_all          0.0304
_refine_ls_R_factor_gt           0.0299
_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)+(0.0465P)²+0.5962P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0772
_refine_ls_wR_factor_ref         0.0775
_reflns_number_gt                4451
_reflns_number_total             4545
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic302662x_si_004.cif
_cod_data_source_block           NiBpeBpe
_cod_original_cell_volume        1112.28(6)
_cod_database_code               4334036
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
N1 N 0.0206(2) -0.00687(13) 0.15505(11) 0.0080(3) Uani 1 1 d .
C1 C -0.0457(3) 0.07144(16) 0.20918(13) 0.0114(3) Uani 1 1 d .
H1 H -0.0914 0.1328 0.1771 0.014 Uiso 1 1 calc R
C2 C -0.0494(3) 0.06552(16) 0.31037(14) 0.0131(3) Uani 1 1 d .
H2 H -0.0956 0.1222 0.3453 0.016 Uiso 1 1 calc R
C3 C 0.0172(3) -0.02681(16) 0.35957(13) 0.0115(3) Uani 1 1 d .
C4 C 0.0856(3) -0.10815(16) 0.30295(13) 0.0116(3) Uani 1 1 d .
H4 H 0.1298 -0.1714 0.3324 0.014 Uiso 1 1 calc R
C5 C 0.0872(2) -0.09417(15) 0.20227(13) 0.0095(3) Uani 1 1 d .
H5 H 0.1367 -0.1477 0.1662 0.011 Uiso 1 1 calc R
C6 C 0.0170(3) -0.04053(17) 0.46642(14) 0.0146(4) Uani 1 1 d .
H6 H 0.0427 -0.1117 0.4889 0.018 Uiso 1 1 calc R
N2 N 0.5016(2) 0.10442(14) 0.35342(13) 0.0160(3) Uani 1 1 d .
C7 C 0.5507(3) 0.15234(18) 0.45449(16) 0.0205(4) Uani 1 1 d .
H7 H 0.5921 0.1038 0.5031 0.025 Uiso 1 1 calc R
C8 C 0.5440(3) 0.26916(18) 0.49149(15) 0.0199(4) Uani 1 1 d .
H8 H 0.5806 0.2974 0.5628 0.024 Uiso 1 1 calc R
C9 C 0.4813(2) 0.34440(16) 0.42001(14) 0.0116(3) Uani 1 1 d .
C10 C 0.4287(3) 0.29440(17) 0.31473(14) 0.0144(4) Uani 1 1 d .
H10 H 0.385 0.3403 0.2642 0.017 Uiso 1 1 calc R
C11 C 0.4413(3) 0.17643(17) 0.28521(14) 0.0159(4) Uani 1 1 d .
H11 H 0.4062 0.1456 0.2144 0.019 Uiso 1 1 calc R
C12 C 0.4706(3) 0.47001(16) 0.45113(14) 0.0131(3) Uani 1 1 d .
H12 H 0.4186 0.5112 0.3986 0.016 Uiso 1 1 calc R
N3 N 0.32764(19) 0.50207(13) -0.14906(11) 0.0075(3) Uani 1 1 d .
C13 C 0.2977(2) 0.41307(16) -0.22992(13) 0.0105(3) Uani 1 1 d .
H13 H 0.3485 0.3455 -0.2178 0.013 Uiso 1 1 calc R
C14 C 0.1947(2) 0.41758(16) -0.33037(13) 0.0123(3) Uani 1 1 d .
H14 H 0.1795 0.3547 -0.3841 0.015 Uiso 1 1 calc R
C15 C 0.1136(2) 0.51703(16) -0.35076(13) 0.0108(3) Uani 1 1 d .
C16 C 0.1393(2) 0.60633(16) -0.26571(14) 0.0122(3) Uani 1 1 d .
H16 H 0.0841 0.6726 -0.2747 0.015 Uiso 1 1 calc R
C17 C 0.2472(2) 0.59645(16) -0.16766(13) 0.0102(3) Uani 1 1 d .
H17 H 0.2645 0.658 -0.1125 0.012 Uiso 1 1 calc R
C18 C 0.0054(2) 0.53273(17) -0.45471(14) 0.0129(3) Uani 1 1 d .
H18 H -0.0614 0.5939 -0.4574 0.015 Uiso 1 1 calc R
Ni1 Ni 0.5 0.5 0 0.00515(10) Uani 1 2 d S
Ni2 Ni 0 0 0 0.00521(10) Uani 1 2 d S
O1 O 0.34701(16) 0.59564(11) 0.06755(9) 0.0086(2) Uani 1 1 d .
O2 O 0.35308(16) 0.33542(10) 0.01090(9) 0.0080(2) Uani 1 1 d .
O3 O 0.00041(16) 0.36830(11) -0.08418(9) 0.0094(2) Uani 1 1 d .
O4 O 0.05915(17) 0.18331(11) 0.03300(9) 0.0086(2) Uani 1 1 d .
O5 O 0.15249(17) 0.41966(11) 0.14222(9) 0.0086(2) Uani 1 1 d .
O6 O 0.30706(17) 0.65468(11) 0.25838(9) 0.0110(2) Uani 1 1 d .
O7 O 0.27842(17) 0.00349(12) 0.02852(10) 0.0104(2) Uani 1 1 d .
V1 V 0.14293(4) 0.32289(2) 0.02534(2) 0.00466(8) Uani 1 1 d .
V2 V 0.20598(4) 0.57960(2) 0.14078(2) 0.00463(8) Uani 1 1 d .
O1W O 0.53022(19) 0.86064(12) 0.07533(11) 0.0137(3) Uani 1 1 d .
O2W O 0.5645(2) 0.87299(13) 0.28160(11) 0.0178(3) Uani 1 1 d .
HW4 H 0.542(4) 0.937(3) 0.309(2) 0.029(3) Uiso 1 1 d .
HW1 H 0.538(4) 0.800(3) 0.054(2) 0.029(3) Uiso 1 1 d .
HW2 H 0.548(4) 0.864(3) 0.139(3) 0.029(3) Uiso 1 1 d .
HW3 H 0.488(4) 0.820(3) 0.294(2) 0.029(3) Uiso 1 1 d .
HW5 H 0.331(4) -0.050(3) 0.036(2) 0.029(3) Uiso 1 1 d .
HW6 H 0.337(4) 0.046(3) -0.007(2) 0.029(3) 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 0.0181 0.0091 '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'
Ni Ni -3.0029 0.5091 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0492 0.0322 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0311 0.018 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
V V 0.0687 2.1097 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
loop_
_exptl_crystal_face_index_h
_exptl_crystal_face_index_k
_exptl_crystal_face_index_l
_exptl_crystal_face_perp_dist
-5 4 0 0.0939
0 7 1 0.0628
0 -7 0 0.0633
-5 0 0 0.1066
0 1 8 0.1005
0 3 -8 0.1321
4 -5 0 0.108
2 0 -9 0.1583
4 1 0 0.1331
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 117.86(15) . .
C5 N1 Ni2 121.52(12) . .
C1 N1 Ni2 120.44(11) . .
N1 C1 C2 123.18(16) . .
C1 C2 C3 119.23(16) . .
C4 C3 C2 117.39(16) . .
C4 C3 C6 119.74(16) . .
C2 C3 C6 122.88(16) . .
C5 C4 C3 119.57(16) . .
N1 C5 C4 122.74(16) . .
C6 C6 C3 125.3(2) 2_556 .
C7 N2 C11 116.36(17) . .
N2 C7 C8 124.45(18) . .
C7 C8 C9 119.10(17) . .
C10 C9 C8 116.56(17) . .
C10 C9 C12 120.06(16) . .
C8 C9 C12 123.38(17) . .
C11 C10 C9 120.11(17) . .
N2 C11 C10 123.42(17) . .
C12 C12 C9 125.3(2) 2_666 .
C17 N3 C13 117.40(14) . .
C17 N3 Ni1 119.98(11) . .
C13 N3 Ni1 122.58(11) . .
N3 C13 C14 123.03(16) . .
C13 C14 C15 119.82(16) . .
C16 C15 C14 116.65(16) . .
C16 C15 C18 118.89(16) . .
C14 C15 C18 124.46(17) . .
C17 C16 C15 120.15(16) . .
N3 C17 C16 122.87(16) . .
C18 C18 C15 126.0(2) 2_564 .
O1 Ni1 O1 180.00(6) . 2_665
O1 Ni1 O2 86.79(5) . 2_665
O1 Ni1 O2 93.21(5) 2_665 2_665
O1 Ni1 O2 93.21(5) . .
O1 Ni1 O2 86.79(5) 2_665 .
O2 Ni1 O2 180.00(6) 2_665 .
O1 Ni1 N3 89.02(5) . 2_665
O1 Ni1 N3 90.98(5) 2_665 2_665
O2 Ni1 N3 92.87(5) 2_665 2_665
O2 Ni1 N3 87.13(5) . 2_665
O1 Ni1 N3 90.98(5) . .
O1 Ni1 N3 89.02(5) 2_665 .
O2 Ni1 N3 87.13(5) 2_665 .
O2 Ni1 N3 92.87(5) . .
N3 Ni1 N3 180.00(8) 2_665 .
O4 Ni2 O4 180.000(18) . 2
O4 Ni2 N1 89.54(5) . .
O4 Ni2 N1 90.46(5) 2 .
O4 Ni2 N1 90.46(5) . 2
O4 Ni2 N1 89.54(5) 2 2
N1 Ni2 N1 180.00(8) . 2
O4 Ni2 O7 91.45(5) . 2
O4 Ni2 O7 88.55(5) 2 2
N1 Ni2 O7 89.16(5) . 2
N1 Ni2 O7 90.84(5) 2 2
O4 Ni2 O7 88.56(5) . .
O4 Ni2 O7 91.44(5) 2 .
N1 Ni2 O7 90.84(5) . .
N1 Ni2 O7 89.16(5) 2 .
O7 Ni2 O7 180 2 .
V2 O1 Ni1 140.61(7) . .
V1 O2 Ni1 120.99(6) . .
V1 O3 V2 148.33(8) . 2_565
V1 O4 Ni2 158.71(8) . .
V1 O5 V2 115.96(6) . .
O4 V1 O2 110.85(6) . .
O4 V1 O3 109.90(6) . .
O2 V1 O3 107.85(6) . .
O4 V1 O5 109.08(6) . .
O2 V1 O5 109.62(6) . .
O3 V1 O5 109.52(6) . .
O4 V1 V2 140.54(4) . .
O2 V1 V2 95.56(4) . .
O3 V1 V2 87.84(4) . .
O5 V1 V2 32.10(4) . .
O6 V2 O1 110.18(6) . .
O6 V2 O3 109.71(6) . 2_565
O1 V2 O3 110.51(6) . 2_565
O6 V2 O5 111.24(6) . .
O1 V2 O5 105.18(6) . .
O3 V2 O5 109.95(6) 2_565 .
O6 V2 V1 138.07(5) . .
O1 V2 V1 78.11(4) . .
O3 V2 V1 104.75(4) 2_565 .
O5 V2 V1 31.94(4) . .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
N1 C5 1.339(2) .
N1 C1 1.340(2) .
N1 Ni2 2.0673(14) .
C1 C2 1.383(2) .
C2 C3 1.400(2) .
C3 C4 1.393(2) .
C3 C6 1.468(2) .
C4 C5 1.389(2) .
C6 C6 1.328(4) 2_556
N2 C7 1.339(3) .
N2 C11 1.341(3) .
C7 C8 1.383(3) .
C8 C9 1.403(3) .
C9 C10 1.394(2) .
C9 C12 1.469(3) .
C10 C11 1.386(3) .
C12 C12 1.338(4) 2_666
N3 C17 1.341(2) .
N3 C13 1.348(2) .
N3 Ni1 2.0966(14) .
C13 C14 1.386(2) .
C14 C15 1.400(3) .
C15 C16 1.395(2) .
C15 C18 1.473(2) .
C16 C17 1.388(2) .
C18 C18 1.334(4) 2_564
Ni1 O1 2.0459(12) .
Ni1 O1 2.0459(12) 2_665
Ni1 O2 2.0703(12) 2_665
Ni1 O2 2.0703(12) .
Ni1 N3 2.0966(14) 2_665
Ni2 O4 2.0367(12) .
Ni2 O4 2.0367(12) 2
Ni2 N1 2.0673(14) 2
Ni2 O7 2.0688(13) 2
Ni2 O7 2.0688(13) .
O1 V2 1.6574(12) .
O2 V1 1.6685(12) .
O3 V1 1.7722(12) .
O3 V2 1.7948(12) 2_565
O4 V1 1.6430(12) .
O5 V1 1.7987(12) .
O5 V2 1.8065(12) .
O6 V2 1.6356(12) .
V1 V2 3.0568(4) .
V2 O3 1.7948(12) 2_565
