#------------------------------------------------------------------------------
#$Date: 2016-03-26 22:07:42 +0200 (Sat, 26 Mar 2016) $
#$Revision: 180491 $
#$URL: svn://www.crystallography.net/cod/cif/7/21/60/7216083.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_7216083
loop_
_publ_author_name
'Yucesan, Gundog'
'Yu, Min Hui'
'O'Connor, Charles J.'
'Zubieta, Jon'
_publ_section_title
;
 Structural consequences of the steric effects of the organoimine ligand
 in the oxovanadium--organophosphonate/copper--mephenterpy family of
 hybrid oxides (mephenterpy =
 4′-(4-methyphenyl)-2,2′∶6′,2″-terpyridine)
;
_journal_issue                   117
_journal_name_full               CrystEngComm
_journal_page_first              711
_journal_paper_doi               10.1039/b511147a
_journal_volume                  7
_journal_year                    2005
_chemical_formula_moiety         '[{Cu(mephenterpy)}VO2(O3PCH2CH2CH2PO3)]'
_chemical_formula_sum            'C25 H24 Cu N3 O8 P2 V'
_chemical_formula_weight         670.89
_chemical_name_common            ((Cu(mephenterpy))VO2(HO3PCH2CH2CH2PO3))
_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_creation_method           SHELXL-97
_cell_angle_alpha                74.024(2)
_cell_angle_beta                 81.549(2)
_cell_angle_gamma                80.0350(10)
_cell_formula_units_Z            2
_cell_length_a                   8.9849(11)
_cell_length_b                   11.2108(11)
_cell_length_c                   13.6744(19)
_cell_measurement_reflns_used    8825
_cell_measurement_temperature    96(2)
_cell_measurement_theta_max      32.96
_cell_measurement_theta_min      1.91
_cell_volume                     1297.0(3)
_computing_cell_refinement       'Bruker SMART'
_computing_data_collection       'Bruker SMART'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    'Bruker SHELXTL and CrystalMaker 6.x'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      96(2)
_diffrn_detector_area_resol_mean '512 x 512'
_diffrn_measured_fraction_theta_full 0.907
_diffrn_measured_fraction_theta_max 0.907
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       'Phi and omega scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0248
_diffrn_reflns_av_sigmaI/netI    0.0452
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            17476
_diffrn_reflns_theta_full        32.96
_diffrn_reflns_theta_max         32.96
_diffrn_reflns_theta_min         1.91
_diffrn_standards_decay_%        0.001
_exptl_absorpt_coefficient_mu    1.360
_exptl_absorpt_correction_T_max  0.8220
_exptl_absorpt_correction_T_min  0.6475
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS SHELX-97 (shledrick, 1997)'
_exptl_crystal_colour            green
_exptl_crystal_density_diffrn    1.718
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             682
_exptl_crystal_size_max          0.35
_exptl_crystal_size_mid          0.25
_exptl_crystal_size_min          0.15
_refine_diff_density_max         1.519
_refine_diff_density_min         -1.493
_refine_diff_density_rms         0.134
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.050
_refine_ls_hydrogen_treatment    refall
_refine_ls_matrix_type           full
_refine_ls_number_parameters     366
_refine_ls_number_reflns         8825
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.050
_refine_ls_R_factor_all          0.0559
_refine_ls_R_factor_gt           0.0447
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[σ²(Fo²)+(0.0805P)²+1.5864P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1209
_refine_ls_wR_factor_ref         0.1272
_reflns_number_gt                7219
_reflns_number_total             8825
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            b511147a.txt
_cod_data_source_block           Compound3
_cod_original_sg_symbol_H-M      P-1
_cod_database_code               7216083
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
Cu1 Cu 0.62347(4) 0.78206(3) 0.83378(2) 0.01306(8) Uani 1 1 d .
V1 V -0.01015(5) 0.95520(4) 0.78379(3) 0.01488(10) Uani 1 1 d .
P1 P 0.30053(7) 0.79662(6) 0.71859(5) 0.01177(12) Uani 1 1 d .
P2 P 0.16155(7) 1.11815(7) 0.37230(5) 0.01557(14) Uani 1 1 d .
O1 O 0.4109(2) 0.73156(17) 0.79443(13) 0.0132(3) Uani 1 1 d .
O2 O 0.1998(2) 0.70144(18) 0.70888(15) 0.0165(4) Uani 1 1 d .
O3 O 0.1956(2) 0.91055(17) 0.74679(15) 0.0168(4) Uani 1 1 d .
O4 O -0.0395(2) 1.08117(19) 0.82407(17) 0.0233(4) Uani 1 1 d .
O5 O 0.3033(2) 1.16011(19) 0.30598(14) 0.0183(4) Uani 1 1 d .
O6 O -0.0842(2) 0.84505(19) 0.87133(15) 0.0209(4) Uani 1 1 d .
O7 O 0.1080(2) 1.01484(18) 0.33240(15) 0.0187(4) Uani 1 1 d .
O8 O 0.0329(2) 1.22146(19) 0.38136(15) 0.0189(4) Uani 1 1 d .
N1 N 0.4907(3) 0.9443(2) 0.85342(17) 0.0176(4) Uani 1 1 d .
N2 N 0.5478(3) 0.7303(2) 0.97650(16) 0.0145(4) Uani 1 1 d .
N3 N 0.7523(3) 0.6114(2) 0.87499(17) 0.0173(4) Uani 1 1 d .
C1 C 0.4694(4) 1.0536(2) 0.7824(2) 0.0212(5) Uani 1 1 d .
H1 H 0.5365 1.0665 0.7211 0.025 Uiso 1 1 calc R
C2 C 0.3531(4) 1.1484(3) 0.7954(2) 0.0254(6) Uani 1 1 d .
H2 H 0.3399 1.2247 0.7437 0.031 Uiso 1 1 calc R
C3 C 0.2567(4) 1.1297(3) 0.8850(2) 0.0260(6) Uani 1 1 d .
H3 H 0.1760 1.1933 0.8956 0.031 Uiso 1 1 calc R
C4 C 0.2785(4) 1.0171(3) 0.9599(2) 0.0232(6) Uani 1 1 d .
H4 H 0.2136 1.0029 1.0222 0.028 Uiso 1 1 calc R
C5 C 0.3962(4) 0.9267(2) 0.9415(2) 0.0189(5) Uani 1 1 d .
C6 C 0.4342(3) 0.8040(2) 1.01455(19) 0.0180(5) Uani 1 1 d .
C7 C 0.3669(4) 0.7645(3) 1.1138(2) 0.0238(6) Uani 1 1 d .
H7 H 0.2845 0.8166 1.1398 0.029 Uiso 1 1 calc R
C8 C 0.4216(4) 0.6465(2) 1.1759(2) 0.0203(5) Uani 1 1 d .
C9 C 0.5395(3) 0.5719(2) 1.13269(19) 0.0167(5) Uani 1 1 d .
H9 H 0.5782 0.4913 1.1718 0.020 Uiso 1 1 calc R
C10 C 0.5999(3) 0.6162(2) 1.03214(19) 0.0152(5) Uani 1 1 d .
C11 C 0.7220(3) 0.5489(3) 0.9746(2) 0.0170(5) Uani 1 1 d .
C12 C 0.8009(3) 0.4336(3) 1.0171(2) 0.0301(7) Uani 1 1 d .
H12 H 0.7781 0.3918 1.0869 0.036 Uiso 1 1 calc R
C13 C 0.9149(4) 0.3798(4) 0.9553(3) 0.0487(12) Uani 1 1 d .
H13 H 0.9706 0.3002 0.9824 0.058 Uiso 1 1 calc R
C14 C 0.9460(4) 0.4433(4) 0.8546(3) 0.0463(12) Uani 1 1 d .
H14 H 1.0239 0.4082 0.8115 0.056 Uiso 1 1 calc R
C15 C 0.8619(3) 0.5594(3) 0.8166(2) 0.0291(7) Uani 1 1 d .
H15 H 0.8834 0.6028 0.7471 0.035 Uiso 1 1 calc R
C16 C 0.3563(4) 0.6036(3) 1.2833(2) 0.0276(7) Uani 1 1 d .
C17 C 0.2501(4) 0.6776(3) 1.3313(2) 0.0309(7) Uani 1 1 d .
H17A H 0.2164 0.7607 1.2945 0.037 Uiso 1 1 calc R
C18 C 0.1902(4) 0.6349(3) 1.4319(2) 0.0293(7) Uani 1 1 d .
H18A H 0.1160 0.6894 1.4619 0.035 Uiso 1 1 calc R
C19 C 0.2344(6) 0.5178(3) 1.4888(2) 0.0438(11) Uani 1 1 d .
C20 C 0.3356(14) 0.4443(5) 1.4408(4) 0.098(7) Uani 1 1 d .
H20A H 0.3675 0.3607 1.4775 0.141 Uiso 1 1 calc R
C21 C 0.3957(13) 0.4851(5) 1.3398(4) 0.125(10) Uani 1 1 d .
H21A H 0.4662 0.4286 1.3095 0.185 Uiso 1 1 calc R
C22 C 0.1698(7) 0.4714(3) 1.5986(3) 0.0520(13) Uani 1 1 d .
H22A H 0.1515 0.3845 1.6111 0.078 Uiso 1 1 calc R
H22B H 0.0738 0.5241 1.6117 0.078 Uiso 1 1 calc R
H22C H 0.2421 0.4756 1.6443 0.078 Uiso 1 1 calc R
C23 C 0.3095(3) 0.9091(3) 0.5030(2) 0.0204(5) Uani 1 1 d .
H23A H 0.3814 0.9150 0.4401 0.024 Uiso 1 1 calc R
H23B H 0.2401 0.8493 0.5034 0.024 Uiso 1 1 calc R
C24 C 0.2160(3) 1.0377(3) 0.4980(2) 0.0190(5) Uani 1 1 d .
H24A H 0.2759 1.0902 0.5201 0.023 Uiso 1 1 calc R
H24B H 0.1232 1.0274 0.5467 0.023 Uiso 1 1 calc R
C25 C 0.3999(3) 0.8561(3) 0.5960(2) 0.0199(5) Uani 1 1 d .
H25A H 0.4544 0.9231 0.6018 0.024 Uiso 1 1 calc R
H25B H 0.4780 0.7877 0.5811 0.024 Uiso 1 1 calc R
H100 H 0.108(5) 0.735(4) 0.668(3) 0.036(11) 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 0.0000 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'
P P 0.1023 0.0942 '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'
Cu Cu 0.3201 1.2651 '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
O5 Cu1 N2 177.62(9) 2_676 .
O5 Cu1 N3 102.05(9) 2_676 .
N2 Cu1 N3 79.91(9) . .
O5 Cu1 N1 98.75(9) 2_676 .
N2 Cu1 N1 79.11(9) . .
N3 Cu1 N1 157.26(9) . .
O5 Cu1 O1 92.51(7) 2_676 .
N2 Cu1 O1 88.37(8) . .
N3 Cu1 O1 102.12(8) . .
N1 Cu1 O1 85.96(8) . .
O4 V1 O6 108.57(11) . .
O4 V1 O7 108.99(10) . 2_576
O6 V1 O7 108.06(10) . 2_576
O4 V1 O3 111.41(10) . .
O6 V1 O3 112.81(10) . .
O7 V1 O3 106.87(9) 2_576 .
O1 P1 O3 113.61(11) . .
O1 P1 O2 109.12(10) . .
O3 P1 O2 108.80(11) . .
O1 P1 C25 110.13(11) . .
O3 P1 C25 106.35(12) . .
O2 P1 C25 108.70(13) . .
O8 P2 O5 115.27(12) . .
O8 P2 O7 110.89(11) . .
O5 P2 O7 108.95(12) . .
O8 P2 C24 109.01(13) . .
O5 P2 C24 107.35(11) . .
O7 P2 C24 104.79(12) . .
P1 O1 Cu1 133.46(11) . .
P1 O3 V1 137.76(13) . .
P2 O5 Cu1 140.43(12) . 2_676
P2 O7 V1 125.33(11) . 2_576
C1 N1 C5 118.8(3) . .
C1 N1 Cu1 126.8(2) . .
C5 N1 Cu1 113.10(17) . .
C6 N2 C10 121.5(2) . .
C6 N2 Cu1 119.01(17) . .
C10 N2 Cu1 119.18(19) . .
C15 N3 C11 118.9(2) . .
C15 N3 Cu1 127.16(18) . .
C11 N3 Cu1 113.93(18) . .
N1 C1 C2 122.3(3) . .
C3 C2 C1 118.6(3) . .
C2 C3 C4 119.6(3) . .
C5 C4 C3 118.6(3) . .
N1 C5 C4 122.0(2) . .
N1 C5 C6 113.6(2) . .
C4 C5 C6 124.4(3) . .
N2 C6 C7 120.6(2) . .
N2 C6 C5 112.9(2) . .
C7 C6 C5 126.5(3) . .
C6 C7 C8 119.6(3) . .
C9 C8 C7 117.9(2) . .
C9 C8 C16 121.1(2) . .
C7 C8 C16 121.0(3) . .
C10 C9 C8 119.5(2) . .
N2 C10 C9 120.8(2) . .
N2 C10 C11 112.7(2) . .
C9 C10 C11 126.4(2) . .
N3 C11 C12 122.2(3) . .
N3 C11 C10 114.1(2) . .
C12 C11 C10 123.7(2) . .
C11 C12 C13 118.5(3) . .
C14 C13 C12 119.3(3) . .
C13 C14 C15 119.2(3) . .
N3 C15 C14 121.9(3) . .
C21 C16 C17 115.6(3) . .
C21 C16 C8 121.3(3) . .
C17 C16 C8 123.1(3) . .
C16 C17 C18 122.0(3) . .
C19 C18 C17 122.0(3) . .
C20 C19 C18 115.9(3) . .
C20 C19 C22 122.0(3) . .
C18 C19 C22 122.0(3) . .
C19 C20 C21 122.8(4) . .
C16 C21 C20 121.6(4) . .
C24 C23 C25 114.9(3) . .
C23 C24 P2 113.4(2) . .
C23 C25 P1 118.92(19) . .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
Cu1 O5 1.8978(19) 2_676
Cu1 N2 1.932(2) .
Cu1 N3 2.037(2) .
Cu1 N1 2.056(2) .
Cu1 O1 2.2586(18) .
V1 O4 1.620(2) .
V1 O6 1.624(2) .
V1 O7 1.851(2) 2_576
V1 O3 1.862(2) .
P1 O1 1.4922(18) .
P1 O3 1.555(2) .
P1 O2 1.556(2) .
P1 C25 1.790(3) .
P2 O8 1.506(2) .
P2 O5 1.5162(19) .
P2 O7 1.578(2) .
P2 C24 1.803(3) .
O5 Cu1 1.8978(19) 2_676
O7 V1 1.851(2) 2_576
N1 C1 1.341(3) .
N1 C5 1.356(4) .
N2 C6 1.336(4) .
N2 C10 1.340(3) .
N3 C15 1.332(4) .
N3 C11 1.361(3) .
C1 C2 1.385(4) .
C2 C3 1.380(5) .
C3 C4 1.394(4) .
C4 C5 1.378(4) .
C5 C6 1.479(4) .
C6 C7 1.387(4) .
C7 C8 1.411(4) .
C8 C9 1.398(4) .
C8 C16 1.480(4) .
C9 C10 1.389(4) .
C10 C11 1.476(4) .
C11 C12 1.379(4) .
C12 C13 1.392(5) .
C13 C14 1.378(4) .
C14 C15 1.392(4) .
C16 C21 1.356(5) .
C16 C17 1.368(4) .
C17 C18 1.386(4) .
C18 C19 1.354(4) .
C19 C20 1.342(6) .
C19 C22 1.510(5) .
C20 C21 1.389(6) .
C23 C24 1.527(4) .
C23 C25 1.533(4) .
