# Electronic Supplementary Material (ESI) for Dalton Transactions
# This journal is © The Royal Society of Chemistry 2011
data_global
_journal_name_full 'Dalton Trans.'
_journal_coden_Cambridge 0222
_journal_volume ?
_journal_page_first ?
_journal_year ?
loop_
_publ_author_name
_publ_author_address
'E.Serrano Larrea'
;Dpto. Mineralog\'ia y Petrolog\'ia
Universidad del Pa\'is Vasco, UPV/EHU
B. Sarriena s/n
48940 Leioa
Spain
;
J.Mesa
;Dpto. Qu\'imica Inorg\'anica
Universidad del Pa\'is Vasco, UPV/EHU
B. Sarriena s/n
48940 Leioa
Spain
;
J.Pizarro
;Dpto. Mineralog\'ia y Petrolog\'ia
Universidad del Pa\'is Vasco, UPV/EHU
B. Sarriena s/n
48940 Leioa
Spain
;
M.Iglesias
;Dpto. Qu\'imica Inorg\'anica
Universidad del Pa\'is Vasco, UPV/EHU
B. Sarriena s/n
48940 Leioa
Spain
;
T.Rojo
;Dpto. Mineralog\'ia y Petrolog\'ia
Universidad del Pa\'is Vasco, UPV/EHU
B. Sarriena s/n
48940 Leioa
Spain
;
;
M.Arriortua
;
''
_publ_contact_author_name 'Dr Edurne Serrano Larrea'
_publ_contact_author_email maribel.arriortua@ehu.es
_publ_section_title
;
M(C6H16N3)
2(VO3)4 as Heterogeneous Catalysts.
Study of three new Hybrid Vanadates of Cobalt(II),
Nickel(II) and Copper(II) with 1-(2-aminoethyl)-piperazonium.
;
_publ_contact_author_address
;Dpto. Mineralog\'ia y Petrolog\'ia
Universidad del Pa\'is Vasco, UPV/EHU
B. Sarriena s/n
48940 Leioa
Spain
;
_publ_contact_author_fax 0034946013500
_publ_contact_author_phone 0034946015372
_publ_requested_category FM
# Attachment '- archive_CoVAep.cif'
#\#CIF_1.1
# CIF produced by WinGX routine CIF_UPDATE
# Created on 2009-02-10 at 11:40:17
# Using CIFtbx version 2.6.2 16 Jun 1998
# Dictionary name : cif_core.dic
# Dictionary vers : 2.3
# Request file : c:\wingx\files\archive.dat
# CIF files read : co_95 red
data_co_95
_database_code_depnum_ccdc_archive 'CCDC 826549'
_audit_creation_date 2009-02-10T11:40:17-00:00
_audit_creation_method 'WinGX routine CIF_UPDATE'
_audit_conform_dict_name cif_core.dic
_audit_conform_dict_version 2.3
_audit_conform_dict_location ftp://ftp.iucr.org/pub/cif_core.dic
#----------------------------------------------------------------------------#
# CHEMICAL INFORMATION #
#----------------------------------------------------------------------------#
_chemical_name_systematic
;
?
;
_chemical_formula_sum 'C6 H16 Co0.50 N3 O6 V2'
_chemical_formula_weight 357.56
#----------------------------------------------------------------------------#
# UNIT CELL INFORMATION #
#----------------------------------------------------------------------------#
_symmetry_cell_setting monoclinic
_symmetry_space_group_name_H-M P21/c
_symmetry_Int_Tables_number 14
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'
_cell_length_a 9.8810(10)
_cell_length_b 9.4000(10)
_cell_length_c 15.024(2)
_cell_angle_alpha 90
_cell_angle_beta 116.542(9)
_cell_angle_gamma 90
_cell_volume 1248.4(2)
_cell_formula_units_Z 4
_cell_measurement_temperature 293(2)
_cell_measurement_reflns_used 15027
_cell_measurement_theta_min 2.26
_cell_measurement_theta_max 30.27
#----------------------------------------------------------------------------#
# CRYSTAL INFORMATION #
#----------------------------------------------------------------------------#
_exptl_crystal_colour orange
_exptl_crystal_size_max 0.17
_exptl_crystal_size_mid 0.17
_exptl_crystal_size_min 0.05
_exptl_crystal_density_diffrn 1.902
_exptl_crystal_density_method flotation
_exptl_crystal_density_meas 1.90(1)
_exptl_crystal_F_000 722
loop_
_exptl_crystal_face_index_h
_exptl_crystal_face_index_k
_exptl_crystal_face_index_l
_exptl_crystal_face_perp_dist
0 -1 -1 0.098
-1 4 -3 0.118
1 -4 3 0.058
0 1 1 0.076
-1 0 1 0.02
1 0 -1 0.031
_exptl_special_details
;
?
;
#----------------------------------------------------------------------------#
# ABSORPTION CORRECTION #
#----------------------------------------------------------------------------#
_exptl_absorpt_coefficient_mu 2.159
_exptl_absorpt_correction_type integration
_exptl_absorpt_process_details 'STOE X-SHAPE'
_exptl_absorpt_correction_T_min 0.6301
_exptl_absorpt_correction_T_max 0.8989
#----------------------------------------------------------------------------#
# DATA COLLECTION #
#----------------------------------------------------------------------------#
_diffrn_source
'sealed X-ray tube, 12 x 0.4 mm long-fine focus'
_diffrn_ambient_temperature 293(2)
_diffrn_radiation_wavelength 0.71073
_diffrn_radiation_type MoK\a
_diffrn_radiation_monochromator graphite
_diffrn_detector 'image plate (34 cm diameter)'
_diffrn_detector_area_resol_mean 6.67
_diffrn_measurement_device '2-circle goniometer'
_diffrn_measurement_device_type 'STOE IPDS 2T'
_diffrn_measurement_method 'rotation method'
_diffrn_reflns_av_R_equivalents 0.0446
_diffrn_reflns_av_unetI/netI 0.0388
_diffrn_reflns_number 24283
_diffrn_reflns_limit_h_min -13
_diffrn_reflns_limit_h_max 13
_diffrn_reflns_limit_k_min -13
_diffrn_reflns_limit_k_max 13
_diffrn_reflns_limit_l_min -20
_diffrn_reflns_limit_l_max 20
_diffrn_reflns_theta_min 2.87
_diffrn_reflns_theta_max 29.78
_diffrn_reflns_theta_full 29.78
_diffrn_measured_fraction_theta_full 0.989
_diffrn_measured_fraction_theta_max 0.989
_reflns_number_total 3531
_reflns_number_gt 2696
_reflns_threshold_expression >2sigma(I)
#----------------------------------------------------------------------------#
# COMPUTER PROGRAMS USED #
#----------------------------------------------------------------------------#
_computing_data_collection 'STOE X-AREA'
_computing_cell_refinement 'STOE X-AREA'
_computing_data_reduction 'STOE X-RED'
_computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)'
#----------------------------------------------------------------------------#
# REFINEMENT INFORMATION #
#----------------------------------------------------------------------------#
_refine_special_details
;
Refinement of F^2^ against ALL reflections. The weighted R-factor wR and
goodness of fit S are based on F^2^, conventional R-factors R are based
on F, with F set to zero for negative F^2^. The threshold expression of
F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is
not relevant to the choice of reflections for refinement. R-factors based
on F^2^ are statistically about twice as large as those based on F, and R-
factors based on ALL data will be even larger.
;
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type full
_refine_ls_weighting_scheme calc
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0150P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_atom_sites_solution_primary direct
_atom_sites_solution_secondary difmap
_atom_sites_solution_hydrogens geom
_refine_ls_hydrogen_treatment constr
_refine_ls_extinction_method none
_refine_ls_number_reflns 3531
_refine_ls_number_parameters 160
_refine_ls_number_restraints 0
_refine_ls_R_factor_all 0.0412
_refine_ls_R_factor_gt 0.024
_refine_ls_wR_factor_ref 0.0396
_refine_ls_wR_factor_gt 0.0379
_refine_ls_goodness_of_fit_ref 0.944
_refine_ls_restrained_S_all 0.944
_refine_ls_shift/su_max 0
_refine_ls_shift/su_mean 0
_refine_diff_density_max 0.409
_refine_diff_density_min -0.235
_refine_diff_density_rms 0.056
#----------------------------------------------------------------------------#
# ATOMIC TYPES, COORDINATES AND THERMAL PARAMETERS #
#----------------------------------------------------------------------------#
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_
_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
Co Co 0 0 0 0.01817(7) Uani 1 2 d S . .
V1 V 0.13941(3) 0.10714(3) 0.267029(18) 0.01867(6) Uani 1 1 d . . .
V2 V 0.15055(3) 0.46008(3) 0.213800(19) 0.02246(6) Uani 1 1 d . . .
O1 O 0.06487(12) 0.05431(13) 0.14947(7) 0.0277(3) Uani 1 1 d . . .
O2 O 0.31142(12) 0.04103(13) 0.32621(8) 0.0306(3) Uani 1 1 d . . .
O3 O 0.18469(14) 0.43422(14) 0.11707(9) 0.0357(3) Uani 1 1 d . . .
O4 O 0.03109(14) 0.04660(15) 0.32769(9) 0.0398(3) Uani 1 1 d . . .
O5 O 0.15095(18) 0.29551(13) 0.27615(10) 0.0452(3) Uani 1 1 d . . .
O6 O 0.28470(16) 0.56044(16) 0.29161(9) 0.0476(4) Uani 1 1 d . . .
N1 N 0.22155(14) -0.11541(15) 0.03974(9) 0.0220(3) Uani 1 1 d . . .
N2 N -0.12555(15) -0.17430(15) 0.01361(9) 0.0256(3) Uani 1 1 d . . .
H14 H -0.1005 -0.1842 0.0735 0.031 Uiso 1 1 d R . .
H15 H -0.1143 -0.2632 -0.0063 0.031 Uiso 1 1 d R . .
N3 N 0.40046(15) -0.37677(16) 0.11381(10) 0.0308(3) Uani 1 1 d . . .
H11 H 0.4774 -0.414 0.1313 0.037 Uiso 1 1 d R . .
H12 H 0.336 -0.435 0.1179 0.037 Uiso 1 1 d R . .
C1 C 0.28519(18) -0.1613(2) 0.14509(11) 0.0283(4) Uani 1 1 d . . .
H9 H 0.2087 -0.2152 0.1543 0.034 Uiso 1 1 calc R . .
H10 H 0.3078 -0.0773 0.1868 0.034 Uiso 1 1 calc R . .
C2 C -0.2871(2) -0.1397(2) -0.04485(14) 0.0371(4) Uani 1 1 d . . .
H1 H -0.3479 -0.207 -0.0293 0.045 Uiso 1 1 calc R . .
H16 H -0.3147 -0.1476 -0.1153 0.045 Uiso 1 1 calc R . .
C3 C 0.3423(2) -0.3328(2) 0.00812(12) 0.0358(4) Uani 1 1 d . . .
H6 H 0.3195 -0.4165 -0.0339 0.043 Uiso 1 1 calc R . .
H13 H 0.419 -0.2782 -0.0004 0.043 Uiso 1 1 calc R . .
C4 C 0.20056(19) -0.2435(2) -0.02266(12) 0.0325(4) Uani 1 1 d . . .
H4 H 0.1661 -0.2138 -0.0912 0.039 Uiso 1 1 calc R . .
H5 H 0.1219 -0.3021 -0.0197 0.039 Uiso 1 1 calc R . .
C5 C 0.42718(19) -0.2511(2) 0.18003(12) 0.0324(4) Uani 1 1 d . . .
H7 H 0.5089 -0.1941 0.1798 0.039 Uiso 1 1 calc R . .
H8 H 0.4569 -0.2829 0.2476 0.039 Uiso 1 1 calc R . .
C6 C 0.3189(2) -0.0086(2) 0.02198(14) 0.0353(4) Uani 1 1 d . . .
H2 H 0.3007 -0.0135 -0.047 0.042 Uiso 1 1 calc R . .
H3 H 0.4245 -0.0312 0.0635 0.042 Uiso 1 1 calc R . .
loop_
_atom_site_aniso_label
_atom_site_aniso_U_11
_atom_site_aniso_U_22
_atom_site_aniso_U_33
_atom_site_aniso_U_23
_atom_site_aniso_U_13
_atom_site_aniso_U_12
Co 0.01604(13) 0.02209(16) 0.01499(12) -0.00026(11) 0.00569(10) -0.00023(12)
V1 0.01798(12) 0.02246(14) 0.01592(11) -0.00016(10) 0.00790(9) -0.00151(11)
V2 0.02327(14) 0.02191(15) 0.02410(12) -0.00153(11) 0.01230(11) 0.00069(11)
O1 0.0249(6) 0.0373(7) 0.0177(5) -0.0012(5) 0.0065(4) 0.0036(5)
O2 0.0193(5) 0.0403(7) 0.0265(5) 0.0015(5) 0.0051(5) -0.0002(5)
O3 0.0408(7) 0.0370(8) 0.0397(7) -0.0070(5) 0.0274(6) -0.0020(6)
O4 0.0348(7) 0.0596(9) 0.0333(6) -0.0098(6) 0.0225(5) -0.0186(6)
O5 0.0748(10) 0.0247(7) 0.0438(7) 0.0009(6) 0.0334(7) 0.0011(7)
O6 0.0468(8) 0.0520(9) 0.0368(7) -0.0079(6) 0.0123(6) -0.0198(7)
N1 0.0186(6) 0.0259(7) 0.0202(6) -0.0008(5) 0.0076(5) 0.0008(6)
N2 0.0288(7) 0.0240(8) 0.0246(6) 0.0014(5) 0.0124(6) -0.0014(6)
N3 0.0185(6) 0.0306(9) 0.0429(8) 0.0033(6) 0.0133(6) 0.0060(6)
C1 0.0263(8) 0.0363(10) 0.0210(7) 0.0014(7) 0.0093(6) 0.0079(7)
C2 0.0252(9) 0.0368(11) 0.0488(10) 0.0003(8) 0.0160(8) -0.0078(8)
C3 0.0306(9) 0.0409(11) 0.0326(9) -0.0099(8) 0.0110(7) 0.0085(8)
C4 0.0264(8) 0.0388(11) 0.0258(8) -0.0085(7) 0.0059(7) 0.0070(8)
C5 0.0271(9) 0.0398(11) 0.0239(7) 0.0008(7) 0.0057(7) 0.0077(8)
C6 0.0280(8) 0.0424(11) 0.0421(9) 0.0060(8) 0.0215(8) 0.0021(8)
#----------------------------------------------------------------------------#
# MOLECULAR GEOMETRY #
#----------------------------------------------------------------------------#
_geom_special_details
;
All esds (except the esd in the dihedral angle between two l.s. planes)
are estimated using the full covariance matrix. The cell esds are taken
into account individually in the estimation of esds in distances, angles
and torsion angles; correlations between esds in cell parameters are only
used when they are defined by crystal symmetry. An approximate (isotropic)
treatment of cell esds is used for estimating esds involving l.s. planes.
;
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
Co O1 2.1042(10) 3 ?
Co O1 2.1042(10) . ?
Co N2 2.1195(14) 3 ?
Co N2 2.1195(14) . ?
Co N1 2.2710(13) 3 ?
Co N1 2.2710(13) . ?
V1 O2 1.6477(11) . ?
V1 O1 1.6571(10) . ?
V1 O5 1.7757(13) . ?
V1 O4 1.7809(12) . ?
V2 O6 1.6213(13) . ?
V2 O3 1.6502(11) . ?
V2 O5 1.8076(13) . ?
V2 O4 1.8088(12) 2 ?
O4 V2 1.8088(12) 2_545 ?
N1 C1 1.4822(19) . ?
N1 C4 1.482(2) . ?
N1 C6 1.495(2) . ?
N2 C2 1.474(2) . ?
N2 H14 0.8249 . ?
N2 H15 0.9105 . ?
N3 C3 1.486(2) . ?
N3 C5 1.490(2) . ?
N3 H11 0.7689 . ?
N3 H12 0.8624 . ?
C1 C5 1.516(2) . ?
C1 H9 0.97 . ?
C1 H10 0.97 . ?
C2 C6 1.502(3) 3 ?
C2 H1 0.97 . ?
C2 H16 0.97 . ?
C3 C4 1.517(2) . ?
C3 H6 0.97 . ?
C3 H13 0.97 . ?
C4 H4 0.97 . ?
C4 H5 0.97 . ?
C5 H7 0.97 . ?
C5 H8 0.97 . ?
C6 C2 1.502(3) 3 ?
C6 H2 0.97 . ?
C6 H3 0.97 . ?
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 Co O1 180.00(2) 3 . ?
O1 Co N2 89.82(5) 3 3 ?
O1 Co N2 90.18(5) . 3 ?
O1 Co N2 90.18(5) 3 . ?
O1 Co N2 89.82(5) . . ?
N2 Co N2 180.00(8) 3 . ?
O1 Co N1 92.13(4) 3 3 ?
O1 Co N1 87.87(4) . 3 ?
N2 Co N1 98.18(5) 3 3 ?
N2 Co N1 81.82(5) . 3 ?
O1 Co N1 87.87(4) 3 . ?
O1 Co N1 92.13(4) . . ?
N2 Co N1 81.82(5) 3 . ?
N2 Co N1 98.18(5) . . ?
N1 Co N1 180.00(8) 3 . ?
O2 V1 O1 108.79(6) . . ?
O2 V1 O5 108.62(7) . . ?
O1 V1 O5 111.33(6) . . ?
O2 V1 O4 108.31(6) . . ?
O1 V1 O4 111.54(6) . . ?
O5 V1 O4 108.16(7) . . ?
O6 V2 O3 107.32(7) . . ?
O6 V2 O5 108.22(7) . . ?
O3 V2 O5 112.11(6) . . ?
O6 V2 O4 110.64(8) . 2 ?
O3 V2 O4 108.94(6) . 2 ?
O5 V2 O4 109.60(7) . 2 ?
V1 O1 Co 171.31(7) . . ?
V1 O4 V2 134.27(7) . 2_545 ?
V1 O5 V2 145.91(8) . . ?
C1 N1 C4 108.18(13) . . ?
C1 N1 C6 112.71(13) . . ?
C4 N1 C6 110.61(13) . . ?
C1 N1 Co 108.59(9) . . ?
C4 N1 Co 112.06(9) . . ?
C6 N1 Co 104.70(10) . . ?
C2 N2 Co 107.27(10) . . ?
C2 N2 H14 113.1 . . ?
Co N2 H14 106.8 . . ?
C2 N2 H15 105.4 . . ?
Co N2 H15 121 . . ?
H14 N2 H15 103.5 . . ?
C3 N3 C5 111.19(14) . . ?
C3 N3 H11 110.1 . . ?
C5 N3 H11 106.2 . . ?
C3 N3 H12 107.9 . . ?
C5 N3 H12 111.8 . . ?
H11 N3 H12 109.6 . . ?
N1 C1 C5 114.65(13) . . ?
N1 C1 H9 108.6 . . ?
C5 C1 H9 108.6 . . ?
N1 C1 H10 108.6 . . ?
C5 C1 H10 108.6 . . ?
H9 C1 H10 107.6 . . ?
N2 C2 C6 110.48(15) . 3 ?
N2 C2 H1 109.6 . . ?
C6 C2 H1 109.6 3 . ?
N2 C2 H16 109.6 . . ?
C6 C2 H16 109.6 3 . ?
H1 C2 H16 108.1 . . ?
N3 C3 C4 110.08(14) . . ?
N3 C3 H6 109.6 . . ?
C4 C3 H6 109.6 . . ?
N3 C3 H13 109.6 . . ?
C4 C3 H13 109.6 . . ?
H6 C3 H13 108.2 . . ?
N1 C4 C3 114.05(13) . . ?
N1 C4 H4 108.7 . . ?
C3 C4 H4 108.7 . . ?
N1 C4 H5 108.7 . . ?
C3 C4 H5 108.7 . . ?
H4 C4 H5 107.6 . . ?
N3 C5 C1 110.48(13) . . ?
N3 C5 H7 109.6 . . ?
C1 C5 H7 109.6 . . ?
N3 C5 H8 109.6 . . ?
C1 C5 H8 109.6 . . ?
H7 C5 H8 108.1 . . ?
N1 C6 C2 111.44(14) . 3 ?
N1 C6 H2 109.3 . . ?
C2 C6 H2 109.3 3 . ?
N1 C6 H3 109.3 . . ?
C2 C6 H3 109.3 3 . ?
H2 C6 H3 108 . . ?
# Attachment '- archive_CuVAep.cif'
#\#CIF_1.1
# CIF produced by WinGX routine CIF_UPDATE
# Created on 2008-11-16 at 12:47:16
# Using CIFtbx version 2.6.2 16 Jun 1998
# Dictionary name : cif_core.dic
# Dictionary vers : 2.3
# Request file : c:\wingx\files\archive.dat
# CIF files read : cuvaep red
data_cuvaep
_database_code_depnum_ccdc_archive 'CCDC 826550'
_audit_creation_date 2008-11-16T12:47:16-00:00
_audit_creation_method 'WinGX routine CIF_UPDATE'
_audit_conform_dict_name cif_core.dic
_audit_conform_dict_version 2.3
_audit_conform_dict_location ftp://ftp.iucr.org/pub/cif_core.dic
#----------------------------------------------------------------------------#
# CHEMICAL INFORMATION #
#----------------------------------------------------------------------------#
_chemical_name_systematic
;
?
;
_chemical_formula_sum 'C6 H16 Cu0.5 N3 O6 V2'
_chemical_formula_weight 359.86
#----------------------------------------------------------------------------#
# UNIT CELL INFORMATION #
#----------------------------------------------------------------------------#
_symmetry_cell_setting monoclinic
_symmetry_space_group_name_H-M 'P 1 21/c 1'
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'
_cell_length_a 9.7630(10)
_cell_length_b 9.2950(10)
_cell_length_c 15.1577(18)
_cell_angle_alpha 90
_cell_angle_beta 116.313(8)
_cell_angle_gamma 90
_cell_volume 1233.0(2)
_cell_formula_units_Z 4
_cell_measurement_temperature 293(2)
_cell_measurement_reflns_used 6572
_cell_measurement_theta_min 2.6474
_cell_measurement_theta_max 32.6068
#----------------------------------------------------------------------------#
# CRYSTAL INFORMATION #
#----------------------------------------------------------------------------#
_exptl_crystal_colour blue
_exptl_crystal_size_max 0.3713
_exptl_crystal_size_mid 0.2151
_exptl_crystal_size_min 0.0549
_exptl_crystal_density_diffrn 1.939
_exptl_crystal_density_method flotation
_exptl_crystal_density_meas 1.93(1)
_exptl_crystal_F_000 726
_exptl_special_details
;
?
;
#----------------------------------------------------------------------------#
# ABSORPTION CORRECTION #
#----------------------------------------------------------------------------#
_exptl_absorpt_coefficient_mu 2.376
_exptl_absorpt_correction_type analytical
_exptl_absorpt_process_details
;
CrysAlis RED, Oxford Diffraction Ltd.,
Version 1.171.32.5 (release 08-05-2007 CrysAlis171 .NET)
(compiled May 8 2007,13:10:02)
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_absorpt_correction_T_min 0.655
_exptl_absorpt_correction_T_max 0.885
#----------------------------------------------------------------------------#
# DATA COLLECTION #
#----------------------------------------------------------------------------#
_diffrn_ambient_temperature 293(2)
_diffrn_radiation_wavelength 0.71073
_diffrn_radiation_type MoK\a
_diffrn_radiation_monochromator graphite
_diffrn_detector_area_resol_mean 8.3504
_diffrn_orient_matrix_ub_11 0.0131775878
_diffrn_orient_matrix_ub_12 -0.0747327869
_diffrn_orient_matrix_ub_13 -0.0024642677
_diffrn_orient_matrix_ub_21 -0.0610032413
_diffrn_orient_matrix_ub_22 -0.0150387672
_diffrn_orient_matrix_ub_23 0.0181086785
_diffrn_orient_matrix_ub_31 -0.0404919635
_diffrn_orient_matrix_ub_32 -0.0017839958
_diffrn_orient_matrix_ub_33 -0.0488623426
_diffrn_reflns_av_R_equivalents 0.0255
_diffrn_reflns_av_unetI/netI 0.0317
_diffrn_reflns_number 12128
_diffrn_reflns_limit_h_min -14
_diffrn_reflns_limit_h_max 13
_diffrn_reflns_limit_k_min -12
_diffrn_reflns_limit_k_max 13
_diffrn_reflns_limit_l_min -21
_diffrn_reflns_limit_l_max 22
_diffrn_reflns_theta_min 2.87
_diffrn_reflns_theta_max 32.62
_diffrn_reflns_theta_full 25
_diffrn_measured_fraction_theta_full 0.994
_diffrn_measured_fraction_theta_max 0.904
_reflns_number_total 4069
_reflns_number_gt 3125
_reflns_threshold_expression >2sigma(I)
#----------------------------------------------------------------------------#
# COMPUTER PROGRAMS USED #
#----------------------------------------------------------------------------#
_computing_data_collection
;
CrysAlis CCD, Oxford Diffraction Ltd.,
Version 1.171.32.5 (release 08-05-2007 CrysAlis171 .NET)
(compiled May 8 2007,13:10:02)
;
_computing_cell_refinement
;
CrysAlis RED, Oxford Diffraction Ltd.,
Version 1.171.32.5 (release 08-05-2007 CrysAlis171 .NET)
(compiled May 8 2007,13:10:02)
;
_computing_data_reduction
;
CrysAlis RED, Oxford Diffraction Ltd.,
Version 1.171.32.5 (release 08-05-2007 CrysAlis171 .NET)
(compiled May 8 2007,13:10:02)
;
_computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)'
#----------------------------------------------------------------------------#
# REFINEMENT INFORMATION #
#----------------------------------------------------------------------------#
_refine_special_details
;
Refinement of F^2^ against ALL reflections. The weighted R-factor wR and
goodness of fit S are based on F^2^, conventional R-factors R are based
on F, with F set to zero for negative F^2^. The threshold expression of
F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is
not relevant to the choice of reflections for refinement. R-factors based
on F^2^ are statistically about twice as large as those based on F, and R-
factors based on ALL data will be even larger.
;
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type full
_refine_ls_weighting_scheme calc
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0426P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_atom_sites_solution_primary direct
_atom_sites_solution_secondary difmap
_atom_sites_solution_hydrogens geom
_refine_ls_hydrogen_treatment constr
_refine_ls_extinction_method none
_refine_ls_number_reflns 4069
_refine_ls_number_parameters 161
_refine_ls_number_restraints 0
_refine_ls_R_factor_all 0.0393
_refine_ls_R_factor_gt 0.0284
_refine_ls_wR_factor_ref 0.0709
_refine_ls_wR_factor_gt 0.0677
_refine_ls_goodness_of_fit_ref 0.99
_refine_ls_restrained_S_all 0.99
_refine_ls_shift/su_max 0
_refine_ls_shift/su_mean 0
_refine_diff_density_max 0.712
_refine_diff_density_min -0.438
_refine_diff_density_rms 0.111
#----------------------------------------------------------------------------#
# ATOMIC TYPES, COORDINATES AND THERMAL PARAMETERS #
#----------------------------------------------------------------------------#
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'
Cu Cu 0.3201 1.2651 '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_
_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
Cu Cu 0 0 0 0.01804(7) Uani 1 2 d S . .
V1 V 0.14064(3) 0.11068(3) 0.277648(18) 0.01836(7) Uani 1 1 d . . .
V2 V 0.15307(3) 0.45907(3) 0.21790(2) 0.02193(7) Uani 1 1 d . . .
O1 O 0.06292(15) 0.05971(15) 0.16275(8) 0.0299(3) Uani 1 1 d . . .
O2 O 0.31512(14) 0.04324(16) 0.33316(9) 0.0310(3) Uani 1 1 d . . .
O3 O 0.20013(16) 0.41938(15) 0.12858(10) 0.0343(3) Uani 1 1 d . . .
O4 O 0.03156(16) 0.04607(17) 0.33770(9) 0.0351(3) Uani 1 1 d . . .
O5 O 0.1499(2) 0.30245(15) 0.28722(11) 0.0445(4) Uani 1 1 d . . .
O6 O 0.28202(18) 0.56826(18) 0.29285(10) 0.0437(4) Uani 1 1 d . . .
N1 N 0.21322(15) -0.11698(15) 0.04030(9) 0.0208(3) Uani 1 1 d . . .
N2 N -0.11651(16) -0.16894(16) 0.01158(10) 0.0231(3) Uani 1 1 d . . .
H14 H -0.0971 -0.1823 0.0743 0.028 Uiso 1 1 d R . .
H15 H -0.1249 -0.2607 -0.0087 0.028 Uiso 1 1 d R . .
N3 N 0.40108(17) -0.37534(17) 0.11768(11) 0.0296(3) Uani 1 1 d . . .
H11 H 0.492 -0.4194 0.1337 0.036 Uiso 1 1 d R . .
H12 H 0.3417 -0.4428 0.1272 0.036 Uiso 1 1 d R . .
C1 C 0.2774(2) -0.1596(2) 0.14542(11) 0.0270(4) Uani 1 1 d . . .
H9 H 0.2015 -0.2154 0.1554 0.032 Uiso 1 1 calc R . .
H10 H 0.298 -0.0735 0.1854 0.032 Uiso 1 1 calc R . .
C2 C -0.2816(2) -0.1380(2) -0.04322(16) 0.0347(4) Uani 1 1 d . . .
H1 H -0.3333 -0.1962 -0.0186 0.042 Uiso 1 1 d R . .
H16 H -0.3177 -0.1437 -0.1157 0.059(8) Uiso 1 1 d R . .
C3 C 0.3399(2) -0.3361(2) 0.01268(13) 0.0345(4) Uani 1 1 d . . .
H6 H 0.3193 -0.4227 -0.0269 0.041 Uiso 1 1 calc R . .
H13 H 0.415 -0.2797 0.0022 0.041 Uiso 1 1 calc R . .
C4 C 0.1936(2) -0.2497(2) -0.01890(13) 0.0329(4) Uani 1 1 d . . .
H4 H 0.1565 -0.2232 -0.0876 0.039 Uiso 1 1 calc R . .
H5 H 0.1166 -0.3099 -0.0134 0.039 Uiso 1 1 calc R . .
C5 C 0.4234(2) -0.2473(2) 0.18041(12) 0.0309(4) Uani 1 1 d . . .
H7 H 0.504 -0.188 0.1789 0.037 Uiso 1 1 calc R . .
H8 H 0.4547 -0.2776 0.2479 0.037 Uiso 1 1 calc R . .
C6 C 0.3113(2) -0.0128(2) 0.01983(15) 0.0337(4) Uani 1 1 d . . .
H2 H 0.29 -0.0188 -0.0489 0.04 Uiso 1 1 calc R . .
H3 H 0.418 -0.0368 0.0594 0.04 Uiso 1 1 calc R . .
loop_
_atom_site_aniso_label
_atom_site_aniso_U_11
_atom_site_aniso_U_22
_atom_site_aniso_U_33
_atom_site_aniso_U_23
_atom_site_aniso_U_13
_atom_site_aniso_U_12
Cu 0.01530(13) 0.01881(14) 0.01927(12) 0.00113(10) 0.00700(10) -0.00019(10)
V1 0.01772(13) 0.02081(14) 0.01762(12) 0.00068(10) 0.00881(10) -0.00028(9)
V2 0.02281(14) 0.02034(15) 0.02533(13) -0.00125(11) 0.01313(11) 0.00039(10)
O1 0.0276(6) 0.0403(8) 0.0185(5) -0.0020(5) 0.0073(5) 0.0058(6)
O2 0.0180(6) 0.0405(8) 0.0301(6) 0.0040(6) 0.0069(5) -0.0004(5)
O3 0.0404(8) 0.0334(7) 0.0412(7) -0.0067(6) 0.0290(6) -0.0003(6)
O4 0.0313(7) 0.0513(9) 0.0299(6) -0.0058(6) 0.0200(6) -0.0140(6)
O5 0.0763(12) 0.0217(7) 0.0472(8) 0.0032(6) 0.0380(8) 0.0022(7)
O6 0.0440(9) 0.0468(9) 0.0363(7) -0.0086(7) 0.0142(7) -0.0180(7)
N1 0.0192(6) 0.0217(7) 0.0201(6) 0.0005(5) 0.0075(5) 0.0012(5)
N2 0.0221(7) 0.0214(7) 0.0256(6) 0.0030(5) 0.0105(6) -0.0009(5)
N3 0.0190(7) 0.0276(8) 0.0421(8) 0.0041(7) 0.0134(6) 0.0057(6)
C1 0.0256(8) 0.0349(10) 0.0184(7) 0.0012(7) 0.0077(6) 0.0103(7)
C2 0.0220(8) 0.0309(10) 0.0497(11) 0.0017(9) 0.0144(8) -0.0064(7)
C3 0.0282(9) 0.0400(11) 0.0315(8) -0.0091(8) 0.0097(7) 0.0095(8)
C4 0.0266(9) 0.0368(10) 0.0264(7) -0.0103(7) 0.0036(7) 0.0087(8)
C5 0.0249(9) 0.0395(11) 0.0237(7) 0.0024(7) 0.0066(7) 0.0097(8)
C6 0.0264(9) 0.0374(11) 0.0435(10) 0.0081(9) 0.0211(8) 0.0042(8)
#----------------------------------------------------------------------------#
# MOLECULAR GEOMETRY #
#----------------------------------------------------------------------------#
_geom_special_details
;
All esds (except the esd in the dihedral angle between two l.s. planes)
are estimated using the full covariance matrix. The cell esds are taken
into account individually in the estimation of esds in distances, angles
and torsion angles; correlations between esds in cell parameters are only
used when they are defined by crystal symmetry. An approximate (isotropic)
treatment of cell esds is used for estimating esds involving l.s. planes.
;
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
Cu N2 1.9919(14) . ?
Cu N2 1.9919(14) 3 ?
Cu N1 2.1821(14) 3 ?
Cu N1 2.1821(14) . ?
Cu O1 2.3296(11) 3 ?
Cu O1 2.3296(11) . ?
V1 O1 1.6316(12) . ?
V1 O2 1.6528(13) . ?
V1 O4 1.7840(12) . ?
V1 O5 1.7875(15) . ?
V2 O6 1.6241(14) . ?
V2 O3 1.6529(12) . ?
V2 O5 1.8037(14) . ?
V2 O4 1.8074(14) 2 ?
O4 V2 1.8074(14) 2_545 ?
N1 C1 1.484(2) . ?
N1 C4 1.487(2) . ?
N1 C6 1.488(2) . ?
N2 C2 1.478(2) . ?
N2 H14 0.8919 . ?
N2 H15 0.8982 . ?
N3 C3 1.476(2) . ?
N3 C5 1.478(2) . ?
N3 H11 0.9073 . ?
N3 H12 0.9081 . ?
C1 C5 1.519(2) . ?
C1 H9 0.97 . ?
C1 H10 0.97 . ?
C2 C6 1.505(3) 3 ?
C2 H1 0.9235 . ?
C2 H16 0.995 . ?
C3 C4 1.519(2) . ?
C3 H6 0.97 . ?
C3 H13 0.97 . ?
C4 H4 0.97 . ?
C4 H5 0.97 . ?
C5 H7 0.97 . ?
C5 H8 0.97 . ?
C6 C2 1.505(3) 3 ?
C6 H2 0.97 . ?
C6 H3 0.97 . ?
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
N2 Cu N2 180.00(9) . 3 ?
N2 Cu N1 84.62(5) . 3 ?
N2 Cu N1 95.38(5) 3 3 ?
N2 Cu N1 95.38(5) . . ?
N2 Cu N1 84.62(5) 3 . ?
N1 Cu N1 180.00(10) 3 . ?
N2 Cu O1 90.72(5) . 3 ?
N2 Cu O1 89.28(5) 3 3 ?
N1 Cu O1 92.93(5) 3 3 ?
N1 Cu O1 87.07(5) . 3 ?
N2 Cu O1 89.28(5) . . ?
N2 Cu O1 90.72(5) 3 . ?
N1 Cu O1 87.07(5) 3 . ?
N1 Cu O1 92.93(5) . . ?
O1 Cu O1 180.00(2) 3 . ?
O1 V1 O2 108.66(7) . . ?
O1 V1 O4 110.28(7) . . ?
O2 V1 O4 109.04(7) . . ?
O1 V1 O5 111.04(7) . . ?
O2 V1 O5 109.47(8) . . ?
O4 V1 O5 108.32(7) . . ?
O6 V2 O3 107.56(8) . . ?
O6 V2 O5 107.76(8) . . ?
O3 V2 O5 112.33(7) . . ?
O6 V2 O4 110.50(8) . 2 ?
O3 V2 O4 107.45(6) . 2 ?
O5 V2 O4 111.20(7) . 2 ?
V1 O1 Cu 168.26(8) . . ?
V1 O4 V2 127.60(7) . 2_545 ?
V1 O5 V2 140.43(8) . . ?
C1 N1 C4 107.85(14) . . ?
C1 N1 C6 113.15(14) . . ?
C4 N1 C6 109.68(14) . . ?
C1 N1 Cu 109.26(10) . . ?
C4 N1 Cu 113.11(10) . . ?
C6 N1 Cu 103.86(10) . . ?
C2 N2 Cu 108.67(11) . . ?
C2 N2 H14 106.8 . . ?
Cu N2 H14 110.1 . . ?
C2 N2 H15 94.7 . . ?
Cu N2 H15 133.4 . . ?
H14 N2 H15 100.2 . . ?
C3 N3 C5 111.63(14) . . ?
C3 N3 H11 106.3 . . ?
C5 N3 H11 110.1 . . ?
C3 N3 H12 111.1 . . ?
C5 N3 H12 112 . . ?
H11 N3 H12 105.3 . . ?
N1 C1 C5 113.73(13) . . ?
N1 C1 H9 108.8 . . ?
C5 C1 H9 108.8 . . ?
N1 C1 H10 108.8 . . ?
C5 C1 H10 108.8 . . ?
H9 C1 H10 107.7 . . ?
N2 C2 C6 108.97(16) . 3 ?
N2 C2 H1 108.3 . . ?
C6 C2 H1 104.7 3 . ?
N2 C2 H16 112 . . ?
C6 C2 H16 107.4 3 . ?
H1 C2 H16 115.1 . . ?
N3 C3 C4 110.19(15) . . ?
N3 C3 H6 109.6 . . ?
C4 C3 H6 109.6 . . ?
N3 C3 H13 109.6 . . ?
C4 C3 H13 109.6 . . ?
H6 C3 H13 108.1 . . ?
N1 C4 C3 113.38(15) . . ?
N1 C4 H4 108.9 . . ?
C3 C4 H4 108.9 . . ?
N1 C4 H5 108.9 . . ?
C3 C4 H5 108.9 . . ?
H4 C4 H5 107.7 . . ?
N3 C5 C1 111.09(14) . . ?
N3 C5 H7 109.4 . . ?
C1 C5 H7 109.4 . . ?
N3 C5 H8 109.4 . . ?
C1 C5 H8 109.4 . . ?
H7 C5 H8 108 . . ?
N1 C6 C2 110.36(14) . 3 ?
N1 C6 H2 109.6 . . ?
C2 C6 H2 109.6 3 . ?
N1 C6 H3 109.6 . . ?
C2 C6 H3 109.6 3 . ?
H2 C6 H3 108.1 . . ?
# Attachment '- archive_NiVAep.cif'
#\#CIF_1.1
# CIF produced by WinGX routine CIF_UPDATE
# Created on 2009-02-10 at 11:55:45
# Using CIFtbx version 2.6.2 16 Jun 1998
# Dictionary name : cif_core.dic
# Dictionary vers : 2.3
# Request file : c:\wingx\files\archive.dat
# CIF files read : nivaep red
data_nivaep
_database_code_depnum_ccdc_archive 'CCDC 826551'
_audit_creation_date 2009-02-10T11:55:45-00:00
_audit_creation_method 'WinGX routine CIF_UPDATE'
_audit_conform_dict_name cif_core.dic
_audit_conform_dict_version 2.3
_audit_conform_dict_location ftp://ftp.iucr.org/pub/cif_core.dic
#----------------------------------------------------------------------------#
# CHEMICAL INFORMATION #
#----------------------------------------------------------------------------#
_chemical_name_systematic
;
?
;
_chemical_formula_sum 'C6 H16 N3 Ni0.50 O6 V2'
_chemical_formula_weight 357.45
#----------------------------------------------------------------------------#
# UNIT CELL INFORMATION #
#----------------------------------------------------------------------------#
_symmetry_cell_setting monoclinic
_symmetry_space_group_name_H-M 'P 21/c'
_symmetry_Int_Tables_number 14
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'
_cell_length_a 9.8481(8)
_cell_length_b 9.4424(6)
_cell_length_c 14.9648(13)
_cell_angle_alpha 90
_cell_angle_beta 116.516(6)
_cell_angle_gamma 90
_cell_volume 1245.19(17)
_cell_formula_units_Z 4
_cell_measurement_temperature 293(2)
_cell_measurement_reflns_used 10122
_cell_measurement_theta_min 3.01
_cell_measurement_theta_max 35.17
#----------------------------------------------------------------------------#
# CRYSTAL INFORMATION #
#----------------------------------------------------------------------------#
_exptl_crystal_colour green
_exptl_crystal_size_max 0.28
_exptl_crystal_size_mid 0.25
_exptl_crystal_size_min 0.15
_exptl_crystal_density_diffrn 1.907
_exptl_crystal_density_method flotation
_exptl_crystal_density_meas 1.90(1)
_exptl_crystal_F_000 724
loop_
_exptl_crystal_face_index_h
_exptl_crystal_face_index_k
_exptl_crystal_face_index_l
_exptl_crystal_face_perp_dist
0 -1 1 0.148
0 1 -1 0.135
0 1 1 0.117
0 -1 -1 0.161
-1 0 1 0.062
1 0 -1 0.043
_exptl_special_details
;
?
;
#----------------------------------------------------------------------------#
# ABSORPTION CORRECTION #
#----------------------------------------------------------------------------#
_exptl_absorpt_coefficient_mu 2.254
_exptl_absorpt_correction_type integration
_exptl_absorpt_process_details 'STOE X-SHAPE'
_exptl_absorpt_correction_T_min 0.5439
_exptl_absorpt_correction_T_max 0.8031
#----------------------------------------------------------------------------#
# DATA COLLECTION #
#----------------------------------------------------------------------------#
_diffrn_source
'sealed X-ray tube, 12 x 0.4 mm long-fine focus'
_diffrn_ambient_temperature 293(2)
_diffrn_radiation_wavelength 0.71073
_diffrn_radiation_type MoK\a
_diffrn_radiation_monochromator graphite
_diffrn_detector 'image plate (34 cm diameter)'
_diffrn_detector_area_resol_mean 6.67
_diffrn_measurement_device '2-circle goniometer'
_diffrn_measurement_device_type 'STOE IPDS 2T'
_diffrn_measurement_method 'rotation method'
_diffrn_reflns_av_R_equivalents 0.0314
_diffrn_reflns_av_unetI/netI 0.0325
_diffrn_reflns_number 16043
_diffrn_reflns_limit_h_min -15
_diffrn_reflns_limit_h_max 15
_diffrn_reflns_limit_k_min -13
_diffrn_reflns_limit_k_max 14
_diffrn_reflns_limit_l_min -19
_diffrn_reflns_limit_l_max 22
_diffrn_reflns_theta_min 3.6
_diffrn_reflns_theta_max 33.14
_diffrn_reflns_theta_full 33.14
_diffrn_measured_fraction_theta_full 0.966
_diffrn_measured_fraction_theta_max 0.966
_reflns_number_total 4583
_reflns_number_gt 3629
_reflns_threshold_expression >2sigma(I)
#----------------------------------------------------------------------------#
# COMPUTER PROGRAMS USED #
#----------------------------------------------------------------------------#
_computing_data_collection 'STOE X-AREA'
_computing_cell_refinement 'STOE X-AREA'
_computing_data_reduction 'STOE X-RED'
_computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)'
#----------------------------------------------------------------------------#
# REFINEMENT INFORMATION #
#----------------------------------------------------------------------------#
_refine_special_details
;
Refinement of F^2^ against ALL reflections. The weighted R-factor wR and
goodness of fit S are based on F^2^, conventional R-factors R are based
on F, with F set to zero for negative F^2^. The threshold expression of
F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is
not relevant to the choice of reflections for refinement. R-factors based
on F^2^ are statistically about twice as large as those based on F, and R-
factors based on ALL data will be even larger.
;
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type full
_refine_ls_weighting_scheme calc
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0273P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_atom_sites_solution_primary direct
_atom_sites_solution_secondary difmap
_atom_sites_solution_hydrogens geom
_refine_ls_hydrogen_treatment constr
_refine_ls_extinction_method none
_refine_ls_number_reflns 4583
_refine_ls_number_parameters 160
_refine_ls_number_restraints 0
_refine_ls_R_factor_all 0.0378
_refine_ls_R_factor_gt 0.0245
_refine_ls_wR_factor_ref 0.0506
_refine_ls_wR_factor_gt 0.0484
_refine_ls_goodness_of_fit_ref 0.921
_refine_ls_restrained_S_all 0.921
_refine_ls_shift/su_max 0.003
_refine_ls_shift/su_mean 0
_refine_diff_density_max 0.709
_refine_diff_density_min -0.346
_refine_diff_density_rms 0.063
#----------------------------------------------------------------------------#
# ATOMIC TYPES, COORDINATES AND THERMAL PARAMETERS #
#----------------------------------------------------------------------------#
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'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Ni Ni 0.3393 1.1124 '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_
_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
Ni1 Ni 0 0 0 0.01637(5) Uani 1 2 d S . .
V1 V 0.13902(2) 0.10721(2) 0.267145(16) 0.01722(5) Uani 1 1 d . . .
V2 V 0.15115(2) 0.45922(2) 0.213581(17) 0.02121(5) Uani 1 1 d . . .
O1 O 0.06466(10) 0.05411(10) 0.14916(7) 0.02596(19) Uani 1 1 d . . .
O2 O 0.31238(10) 0.04177(11) 0.32715(8) 0.0299(2) Uani 1 1 d . . .
O3 O 0.18473(13) 0.43318(12) 0.11616(9) 0.0348(2) Uani 1 1 d . . .
O4 O 0.03063(13) 0.04690(14) 0.32829(9) 0.0393(3) Uani 1 1 d . . .
O5 O 0.14983(17) 0.29574(11) 0.27598(10) 0.0453(3) Uani 1 1 d . . .
O6 O 0.28702(15) 0.55873(15) 0.29229(10) 0.0473(3) Uani 1 1 d . . .
N1 N 0.21719(11) -0.11436(11) 0.03985(8) 0.0214(2) Uani 1 1 d . . .
N2 N -0.11939(12) -0.17220(11) 0.01464(9) 0.0234(2) Uani 1 1 d . . .
H14 H -0.0999 -0.1828 0.076 0.028 Uiso 1 1 d R . .
H15 H -0.1026 -0.2579 -0.0017 0.028 Uiso 1 1 d R . .
N3 N 0.39976(13) -0.37506(12) 0.11348(10) 0.0304(3) Uani 1 1 d . . .
H11 H 0.4904 -0.4159 0.1325 0.037 Uiso 1 1 d R . .
H12 H 0.329 -0.4389 0.1141 0.037 Uiso 1 1 d R . .
C1 C 0.28200(15) -0.16058(16) 0.14516(10) 0.0283(3) Uani 1 1 d . . .
H9 H 0.2058 -0.2149 0.1546 0.034 Uiso 1 1 calc R . .
H10 H 0.3046 -0.0772 0.1873 0.034 Uiso 1 1 calc R . .
C2 C -0.28265(16) -0.13945(16) -0.04358(14) 0.0361(3) Uani 1 1 d . . .
H1 H -0.3423 -0.2065 -0.0267 0.043 Uiso 1 1 calc R . .
H16 H -0.3114 -0.1485 -0.1143 0.043 Uiso 1 1 calc R . .
C3 C 0.34053(17) -0.33015(18) 0.00734(12) 0.0367(4) Uani 1 1 d . . .
H6 H 0.3187 -0.413 -0.0352 0.044 Uiso 1 1 calc R . .
H13 H 0.4166 -0.2742 -0.0011 0.044 Uiso 1 1 calc R . .
C4 C 0.19663(16) -0.24284(17) -0.02306(11) 0.0330(3) Uani 1 1 d . . .
H4 H 0.1606 -0.2136 -0.092 0.04 Uiso 1 1 calc R . .
H5 H 0.119 -0.3023 -0.0193 0.04 Uiso 1 1 calc R . .
C5 C 0.42564(16) -0.24986(16) 0.17996(11) 0.0314(3) Uani 1 1 d . . .
H7 H 0.5072 -0.1926 0.1796 0.038 Uiso 1 1 calc R . .
H8 H 0.4559 -0.2817 0.2478 0.038 Uiso 1 1 calc R . .
C6 C 0.31533(17) -0.00840(17) 0.02151(14) 0.0349(3) Uani 1 1 d . . .
H2 H 0.2974 -0.0142 -0.0476 0.042 Uiso 1 1 calc R . .
H3 H 0.4212 -0.0306 0.0635 0.042 Uiso 1 1 calc R . .
loop_
_atom_site_aniso_label
_atom_site_aniso_U_11
_atom_site_aniso_U_22
_atom_site_aniso_U_33
_atom_site_aniso_U_23
_atom_site_aniso_U_13
_atom_site_aniso_U_12
Ni1 0.01508(9) 0.01936(9) 0.01365(10) 0.00002(7) 0.00548(7) -0.00006(7)
V1 0.01718(8) 0.01988(9) 0.01525(9) -0.00034(7) 0.00781(7) -0.00165(6)
V2 0.02247(9) 0.01988(9) 0.02319(11) -0.00183(7) 0.01191(8) 0.00060(7)
O1 0.0252(4) 0.0339(5) 0.0165(4) -0.0015(4) 0.0073(4) 0.0037(4)
O2 0.0181(4) 0.0390(5) 0.0266(5) 0.0008(4) 0.0047(4) -0.0017(4)
O3 0.0410(6) 0.0357(5) 0.0387(6) -0.0076(5) 0.0278(5) -0.0010(4)
O4 0.0353(5) 0.0591(7) 0.0332(6) -0.0118(5) 0.0241(5) -0.0208(5)
O5 0.0789(9) 0.0208(5) 0.0446(7) 0.0008(4) 0.0351(7) 0.0011(5)
O6 0.0459(7) 0.0517(7) 0.0371(7) -0.0092(5) 0.0120(5) -0.0208(6)
N1 0.0181(4) 0.0242(5) 0.0202(5) 0.0004(4) 0.0070(4) 0.0013(4)
N2 0.0248(5) 0.0227(5) 0.0236(5) 0.0019(4) 0.0116(4) -0.0007(4)
N3 0.0202(5) 0.0277(6) 0.0431(7) 0.0022(5) 0.0139(5) 0.0064(4)
C1 0.0261(6) 0.0372(7) 0.0200(6) 0.0021(5) 0.0089(5) 0.0105(5)
C2 0.0240(6) 0.0325(7) 0.0495(10) 0.0011(7) 0.0144(6) -0.0073(5)
C3 0.0295(7) 0.0429(8) 0.0338(8) -0.0097(6) 0.0106(6) 0.0108(6)
C4 0.0257(6) 0.0396(7) 0.0259(7) -0.0099(6) 0.0046(5) 0.0093(5)
C5 0.0249(6) 0.0388(7) 0.0247(7) 0.0015(6) 0.0058(5) 0.0102(5)
C6 0.0268(6) 0.0383(7) 0.0452(9) 0.0071(7) 0.0210(6) 0.0033(5)
#----------------------------------------------------------------------------#
# MOLECULAR GEOMETRY #
#----------------------------------------------------------------------------#
_geom_special_details
;
All esds (except the esd in the dihedral angle between two l.s. planes)
are estimated using the full covariance matrix. The cell esds are taken
into account individually in the estimation of esds in distances, angles
and torsion angles; correlations between esds in cell parameters are only
used when they are defined by crystal symmetry. An approximate (isotropic)
treatment of cell esds is used for estimating esds involving l.s. planes.
;
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
Ni1 N2 2.0747(11) 3 ?
Ni1 N2 2.0747(11) . ?
Ni1 O1 2.0928(10) 3 ?
Ni1 O1 2.0928(10) . ?
Ni1 N1 2.2266(10) 3 ?
Ni1 N1 2.2266(10) . ?
V1 O2 1.6535(10) . ?
V1 O1 1.6585(10) . ?
V1 O4 1.7812(11) . ?
V1 O5 1.7847(11) . ?
V2 O6 1.6289(12) . ?
V2 O3 1.6510(12) . ?
V2 O5 1.8072(11) . ?
V2 O4 1.8114(11) 2 ?
O4 V2 1.8114(11) 2_545 ?
N1 C1 1.4776(17) . ?
N1 C4 1.4929(18) . ?
N1 C6 1.4992(19) . ?
N2 C2 1.4795(18) . ?
N2 H14 0.8565 . ?
N2 H15 0.8816 . ?
N3 C3 1.489(2) . ?
N3 C5 1.492(2) . ?
N3 H11 0.8945 . ?
N3 H12 0.9247 . ?
C1 C5 1.5248(18) . ?
C1 H9 0.97 . ?
C1 H10 0.97 . ?
C2 C6 1.502(2) 3 ?
C2 H1 0.97 . ?
C2 H16 0.97 . ?
C3 C4 1.5230(19) . ?
C3 H6 0.97 . ?
C3 H13 0.97 . ?
C4 H4 0.97 . ?
C4 H5 0.97 . ?
C5 H7 0.97 . ?
C5 H8 0.97 . ?
C6 C2 1.502(2) 3 ?
C6 H2 0.97 . ?
C6 H3 0.97 . ?
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
N2 Ni1 N2 180.00(7) 3 . ?
N2 Ni1 O1 89.75(4) 3 3 ?
N2 Ni1 O1 90.25(4) . 3 ?
N2 Ni1 O1 90.25(4) 3 . ?
N2 Ni1 O1 89.75(4) . . ?
O1 Ni1 O1 180.00(2) 3 . ?
N2 Ni1 N1 96.52(4) 3 3 ?
N2 Ni1 N1 83.48(4) . 3 ?
O1 Ni1 N1 91.96(4) 3 3 ?
O1 Ni1 N1 88.04(4) . 3 ?
N2 Ni1 N1 83.48(4) 3 . ?
N2 Ni1 N1 96.52(4) . . ?
O1 Ni1 N1 88.04(4) 3 . ?
O1 Ni1 N1 91.96(4) . . ?
N1 Ni1 N1 180.00(8) 3 . ?
O2 V1 O1 108.86(5) . . ?
O2 V1 O4 108.17(6) . . ?
O1 V1 O4 111.67(5) . . ?
O2 V1 O5 108.63(6) . . ?
O1 V1 O5 111.33(6) . . ?
O4 V1 O5 108.09(6) . . ?
O6 V2 O3 107.51(7) . . ?
O6 V2 O5 108.19(7) . . ?
O3 V2 O5 112.31(6) . . ?
O6 V2 O4 110.63(7) . 2 ?
O3 V2 O4 108.62(6) . 2 ?
O5 V2 O4 109.58(6) . 2 ?
V1 O1 Ni1 171.40(6) . . ?
V1 O4 V2 134.01(7) . 2_545 ?
V1 O5 V2 145.86(8) . . ?
C1 N1 C4 107.75(11) . . ?
C1 N1 C6 112.68(11) . . ?
C4 N1 C6 110.12(12) . . ?
C1 N1 Ni1 109.56(8) . . ?
C4 N1 Ni1 112.43(7) . . ?
C6 N1 Ni1 104.36(8) . . ?
C2 N2 Ni1 106.98(8) . . ?
C2 N2 H14 108.7 . . ?
Ni1 N2 H14 109.8 . . ?
C2 N2 H15 108.5 . . ?
Ni1 N2 H15 120.3 . . ?
H14 N2 H15 102.1 . . ?
C3 N3 C5 110.77(11) . . ?
C3 N3 H11 108.8 . . ?
C5 N3 H11 106.3 . . ?
C3 N3 H12 105 . . ?
C5 N3 H12 114.5 . . ?
H11 N3 H12 111.4 . . ?
N1 C1 C5 114.88(12) . . ?
N1 C1 H9 108.5 . . ?
C5 C1 H9 108.5 . . ?
N1 C1 H10 108.5 . . ?
C5 C1 H10 108.5 . . ?
H9 C1 H10 107.5 . . ?
N2 C2 C6 110.36(12) . 3 ?
N2 C2 H1 109.6 . . ?
C6 C2 H1 109.6 3 . ?
N2 C2 H16 109.6 . . ?
C6 C2 H16 109.6 3 . ?
H1 C2 H16 108.1 . . ?
N3 C3 C4 109.99(13) . . ?
N3 C3 H6 109.7 . . ?
C4 C3 H6 109.7 . . ?
N3 C3 H13 109.7 . . ?
C4 C3 H13 109.7 . . ?
H6 C3 H13 108.2 . . ?
N1 C4 C3 113.92(11) . . ?
N1 C4 H4 108.8 . . ?
C3 C4 H4 108.8 . . ?
N1 C4 H5 108.8 . . ?
C3 C4 H5 108.8 . . ?
H4 C4 H5 107.7 . . ?
N3 C5 C1 110.74(11) . . ?
N3 C5 H7 109.5 . . ?
C1 C5 H7 109.5 . . ?
N3 C5 H8 109.5 . . ?
C1 C5 H8 109.5 . . ?
H7 C5 H8 108.1 . . ?
N1 C6 C2 111.17(12) . 3 ?
N1 C6 H2 109.4 . . ?
C2 C6 H2 109.4 3 . ?
N1 C6 H3 109.4 . . ?
C2 C6 H3 109.4 3 . ?
H2 C6 H3 108 . . ?