#------------------------------------------------------------------------------
#$Date: 2016-02-16 22:30:59 +0200 (Tue, 16 Feb 2016) $
#$Revision: 176467 $
#$URL: svn://www.crystallography.net/cod/cif/4/31/99/4319992.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_4319992
loop_
_publ_author_name
'Robert C. Finn'
'Robert Lam'
'John E. Greedan'
'Jon Zubieta'
_publ_section_title
;
 Solid-State Coordination Chemistry: Structural Influences of
 Copper-Phenanthroline Subunits on Oxovanadium Organophosphonate Phases.
 Hydrothermal Synthesis and Structural Characterization of the
 Two-Dimensional Materials [Cu(phen)(VO)(O3PCH2PO3)(H2O)],
 [{Cu(phen)}2(V2O5)(O3PCH2CH2PO3)], and
 [{Cu(phen)}2(V3O5)(O3PCH2CH2CH2PO3)2(H2O)] and of the Three-Dimensional
 Phase [{Cu(phen)}2(V3O5)(O3PCH2PO3)2(H2O)]
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              3745
_journal_page_last               3754
_journal_paper_doi               10.1021/ic010186i
_journal_volume                  40
_journal_year                    2001
_chemical_formula_sum            'C15 H14 Cu N2 O9 P2 V1.5'
_chemical_formula_weight         568.17
_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                118.1870(10)
_cell_angle_beta                 91.4160(10)
_cell_angle_gamma                107.8210(10)
_cell_formula_units_Z            2
_cell_length_a                   9.4356(6)
_cell_length_b                   10.6556(6)
_cell_length_c                   11.0354(7)
_cell_measurement_temperature    90(2)
_cell_volume                     911.88(10)
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 0.910
_diffrn_measured_fraction_theta_max 0.910
_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  0.0275
_diffrn_reflns_av_sigmaI/netI    0.0323
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       14
_diffrn_reflns_limit_l_min       -13
_diffrn_reflns_number            6013
_diffrn_reflns_theta_full        28.28
_diffrn_reflns_theta_max         28.28
_diffrn_reflns_theta_min         2.14
_exptl_absorpt_coefficient_mu    2.152
_exptl_crystal_density_diffrn    2.069
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             567
_exptl_crystal_size_max          0.32
_exptl_crystal_size_mid          0.26
_exptl_crystal_size_min          0.17
_refine_diff_density_max         0.567
_refine_diff_density_min         -0.637
_refine_diff_density_rms         0.138
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.063
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     300
_refine_ls_number_reflns         4119
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.063
_refine_ls_R_factor_all          0.0457
_refine_ls_R_factor_gt           0.0396
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[σ²(Fo²)+(0.0793P)²+0.1884P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1107
_refine_ls_wR_factor_ref         0.1146
_reflns_number_gt                3591
_reflns_number_total             4119
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic010186i_3.cif
_cod_data_source_block           p-1
_cod_original_formula_sum        'C15 H14 Cu N2 O9 P2 V1.50'
_cod_database_code               4319992
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
Cu1 Cu 0.28203(4) 0.49406(4) 0.29711(3) 0.01330(12) Uani 1 1 d . . .
V1 V -0.52718(10) 0.52893(10) 0.03986(10) 0.01132(19) Uani 0.50 1 d P . .
V2A V -0.1804(4) 0.5977(5) 0.0530(4) 0.0064(13) Uani 0.110(2) 1 d P . .
V2 V -0.14057(6) 0.68136(6) 0.14502(6) 0.01088(19) Uani 0.890(2) 1 d P . .
P1 P -0.05388(8) 0.38781(8) 0.11807(7) 0.01175(16) Uani 1 1 d . . .
P2 P -0.31415(8) 0.77039(8) -0.03760(7) 0.01201(16) Uani 1 1 d . . .
O1 O 0.2947(2) 0.2954(2) 0.1892(2) 0.0168(4) Uani 1 1 d . . .
O2 O 0.3638(15) 0.5831(8) 0.1478(12) 0.011(3) Uani 0.41(5) 1 d P . .
O2A O 0.307(3) 0.5816(9) 0.1170(15) 0.056(4) Uani 0.59(5) 1 d P . .
O3 O -0.1079(2) 0.5228(2) 0.1675(2) 0.0168(4) Uani 1 1 d . . .
O4 O 0.0683(2) 0.4197(2) 0.2314(2) 0.0181(4) Uani 1 1 d . . .
O5 O 0.0133(2) 0.6584(2) 0.0270(2) 0.0161(4) Uani 1 1 d . . .
O6 O -0.0604(3) 0.8217(2) 0.2995(2) 0.0231(5) Uani 1 1 d . . .
O7 O -0.1786(2) 0.7971(2) 0.0622(2) 0.0148(4) Uani 1 1 d . . .
O8 O -0.3322(2) 0.6170(2) 0.1480(2) 0.0178(4) Uani 1 1 d . . .
O9 O -0.4653(2) 0.6683(2) -0.0271(2) 0.0154(4) Uani 1 1 d . . .
N1 N 0.5010(3) 0.5855(3) 0.3975(3) 0.0196(5) Uani 1 1 d . . .
N2 N 0.2865(3) 0.7036(3) 0.4381(3) 0.0156(5) Uani 1 1 d . . .
C1 C 0.6054(4) 0.5217(4) 0.3729(3) 0.0254(7) Uani 1 1 d . . .
H1 H 0.5803 0.4222 0.2990 0.030 Uiso 1 1 calc R . .
C2 C 0.7530(4) 0.6003(5) 0.4555(4) 0.0318(8) Uani 1 1 d . . .
H2 H 0.8234 0.5521 0.4376 0.038 Uiso 1 1 calc R . .
C3 C 0.7928(4) 0.7480(5) 0.5625(4) 0.0344(9) Uani 1 1 d . . .
H3 H 0.8900 0.7998 0.6182 0.041 Uiso 1 1 calc R . .
C4 C 0.6874(4) 0.8211(4) 0.5880(3) 0.0273(7) Uani 1 1 d . . .
C5 C 0.5413(3) 0.7330(4) 0.5029(3) 0.0202(6) Uani 1 1 d . . .
C6 C 0.7167(4) 0.9758(4) 0.6923(3) 0.0348(9) Uani 1 1 d . . .
H6 H 0.8127 1.0349 0.7497 0.042 Uiso 1 1 calc R . .
C7 C 0.6084(4) 1.0398(4) 0.7105(3) 0.0319(8) Uani 1 1 d . . .
H7 H 0.6323 1.1419 0.7780 0.038 Uiso 1 1 calc R . .
C8 C 0.4580(4) 0.9512(3) 0.6265(3) 0.0232(7) Uani 1 1 d . . .
C9 C 0.4255(3) 0.7976(3) 0.5241(3) 0.0185(6) Uani 1 1 d . . .
C10 C 0.3390(4) 1.0075(3) 0.6381(3) 0.0253(7) Uani 1 1 d . . .
H10 H 0.3546 1.1082 0.7047 0.030 Uiso 1 1 calc R . .
C11 C 0.1998(4) 0.9129(3) 0.5504(3) 0.0235(7) Uani 1 1 d . . .
H11 H 0.1210 0.9496 0.5565 0.028 Uiso 1 1 calc R . .
C12 C 0.1765(4) 0.7607(3) 0.4515(3) 0.0185(6) Uani 1 1 d . . .
H12 H 0.0813 0.6975 0.3934 0.022 Uiso 1 1 calc R . .
C13 C -0.2141(3) 0.2307(3) 0.0979(3) 0.0153(5) Uani 1 1 d . . .
H13A H -0.2479 0.2607 0.1864 0.018 Uiso 1 1 calc R . .
H13B H -0.2964 0.2100 0.0287 0.018 Uiso 1 1 calc R . .
C14 C -0.1833(3) 1.0830(3) 0.0527(3) 0.0143(5) Uani 1 1 d . . .
H14A H -0.1367 1.0587 -0.0289 0.017 Uiso 1 1 calc R . .
H14B H -0.1135 1.0970 0.1279 0.017 Uiso 1 1 calc R . .
C15 C -0.3322(3) 0.9516(3) 0.0175(3) 0.0141(5) Uani 1 1 d . . .
H15A H -0.4013 0.9406 -0.0565 0.017 Uiso 1 1 calc R . .
H15B H -0.3781 0.9786 0.0996 0.017 Uiso 1 1 calc R . .
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
_geom_angle_publ_flag
O4 Cu1 O1 93.23(9) . . ?
O4 Cu1 N2 92.51(9) . . ?
O1 Cu1 N2 170.34(9) . . ?
O4 Cu1 N1 170.89(9) . . ?
O1 Cu1 N1 91.74(10) . . ?
N2 Cu1 N1 81.58(10) . . ?
O4 Cu1 O2 99.2(4) . . ?
O1 Cu1 O2 97.47(17) . . ?
N2 Cu1 O2 89.27(18) . . ?
N1 Cu1 O2 87.7(4) . . ?
V1 V1 O2 168.4(3) 2_465 1_455 ?
V1 V1 O8 81.90(12) 2_465 . ?
O2 V1 O8 106.2(5) 1_455 . ?
V1 V1 O9 80.41(11) 2_465 . ?
O2 V1 O9 107.7(3) 1_455 . ?
O8 V1 O9 88.55(9) . . ?
V1 V1 O2A 155.9(7) 2_465 1_455 ?
O2 V1 O2A 17.8(3) 1_455 1_455 ?
O8 V1 O2A 122.2(7) . 1_455 ?
O9 V1 O2A 98.6(5) . 1_455 ?
V1 V1 O8 66.64(11) 2_465 2_465 ?
O2 V1 O8 104.9(5) 1_455 2_465 ?
O8 V1 O8 148.53(6) . 2_465 ?
O9 V1 O8 86.30(9) . 2_465 ?
O2A V1 O8 89.3(7) 1_455 2_465 ?
V1 V1 O9 68.43(10) 2_465 2_465 ?
O2 V1 O9 103.1(3) 1_455 2_465 ?
O8 V1 O9 87.12(9) . 2_465 ?
O9 V1 O9 148.84(6) . 2_465 ?
O2A V1 O9 109.8(4) 1_455 2_465 ?
O8 V1 O9 81.53(9) 2_465 2_465 ?
V1 V1 V2A 109.01(14) 2_465 2_465 ?
O2 V1 V2A 61.5(5) 1_455 2_465 ?
O8 V1 V2A 164.80(12) . 2_465 ?
O9 V1 V2A 103.44(11) . 2_465 ?
O2A V1 V2A 47.5(6) 1_455 2_465 ?
O8 V1 V2A 43.69(11) 2_465 2_465 ?
O9 V1 V2A 87.23(10) 2_465 2_465 ?
V1 V1 V2A 52.22(12) 2_465 . ?
O2 V1 V2A 137.1(5) 1_455 . ?
O8 V1 V2A 31.28(10) . . ?
O9 V1 V2A 75.46(9) . . ?
O2A V1 V2A 151.1(5) 1_455 . ?
O8 V1 V2A 118.00(11) 2_465 . ?
O9 V1 V2A 85.14(9) 2_465 . ?
V2A V1 V2A 161.22(5) 2_465 . ?
V2 V2A O8 70.7(2) . . ?
V2 V2A O5 84.4(3) . . ?
O8 V2A O5 154.7(3) . . ?
V2 V2A O2A 165.9(6) . 2_565 ?
O8 V2A O2A 95.4(6) . 2_565 ?
O5 V2A O2A 109.6(6) . 2_565 ?
V2 V2A O3 72.7(2) . . ?
O8 V2A O3 88.62(18) . . ?
O5 V2A O3 87.83(18) . . ?
O2A V2A O3 105.9(8) 2_565 . ?
V2 V2A O7 69.3(2) . . ?
O8 V2A O7 84.00(17) . . ?
O5 V2A O7 83.36(16) . . ?
O2A V2A O7 112.2(8) 2_565 . ?
O3 V2A O7 141.6(2) . . ?
V2 V2A O2 156.8(4) . 2_565 ?
O8 V2A O2 87.8(3) . 2_565 ?
O5 V2A O2 116.0(3) . 2_565 ?
O2A V2A O2 13.2(7) 2_565 2_565 ?
O3 V2A O2 116.6(3) . 2_565 ?
O7 V2A O2 100.7(3) . 2_565 ?
V2 V2A V1 119.8(3) . 2_465 ?
O8 V2A V1 50.39(12) . 2_465 ?
O5 V2A V1 151.5(2) . 2_465 ?
O2A V2A V1 47.1(7) 2_565 2_465 ?
O3 V2A V1 112.50(17) . 2_465 ?
O7 V2A V1 91.24(15) . 2_465 ?
O2 V2A V1 37.6(2) 2_565 2_465 ?
V2 V2A V1 101.0(3) . . ?
O8 V2A V1 32.48(10) . . ?
O5 V2A V1 163.3(2) . . ?
O2A V2A V1 65.8(7) 2_565 . ?
O3 V2A V1 108.86(15) . . ?
O7 V2A V1 83.83(13) . . ?
O2 V2A V1 56.3(2) 2_565 . ?
V1 V2A V1 18.78(5) 2_465 . ?
V2A V2 O6 175.5(3) . . ?
V2A V2 O8 78.5(2) . . ?
O6 V2 O8 105.63(11) . . ?
V2A V2 O3 79.5(2) . . ?
O6 V2 O3 98.42(10) . . ?
O8 V2 O3 92.46(9) . . ?
V2A V2 O7 83.9(2) . . ?
O6 V2 O7 97.80(10) . . ?
O8 V2 O7 89.57(9) . . ?
O3 V2 O7 162.45(9) . . ?
V2A V2 O5 67.1(2) . . ?
O6 V2 O5 108.88(10) . . ?
O8 V2 O5 145.37(10) . . ?
O3 V2 O5 85.44(8) . . ?
O7 V2 O5 83.02(8) . . ?
O4 P1 O3 110.34(12) . . ?
O4 P1 O5 115.85(12) . 2_565 ?
O3 P1 O5 110.76(11) . 2_565 ?
O4 P1 C13 106.34(13) . . ?
O3 P1 C13 105.92(12) . . ?
O5 P1 C13 107.01(13) 2_565 . ?
O1 P2 O7 113.08(12) 2_565 . ?
O1 P2 O9 110.30(12) 2_565 . ?
O7 P2 O9 111.50(11) . . ?
O1 P2 C15 107.69(12) 2_565 . ?
O7 P2 C15 107.82(12) . . ?
O9 P2 C15 106.10(12) . . ?
P2 O1 Cu1 122.89(12) 2_565 . ?
O2A O2 V1 109.9(16) . 1_655 ?
O2A O2 Cu1 106.7(12) . . ?
V1 O2 Cu1 126.4(5) 1_655 . ?
O2A O2 V2A 44.8(13) . 2_565 ?
V1 O2 V2A 80.9(5) 1_655 2_565 ?
Cu1 O2 V2A 99.9(3) . 2_565 ?
O2 O2A V1 52.3(16) . 1_655 ?
O2 O2A V2A 122.0(19) . 2_565 ?
V1 O2A V2A 85.4(4) 1_655 2_565 ?
P1 O3 V2 150.98(14) . . ?
P1 O3 V2A 128.12(17) . . ?
V2 O3 V2A 27.79(12) . . ?
P1 O4 Cu1 144.29(14) . . ?
P1 O5 V2A 123.40(19) 2_565 . ?
P1 O5 V2 149.11(13) 2_565 . ?
V2A O5 V2 28.46(14) . . ?
P2 O7 V2 133.28(12) . . ?
P2 O7 V2A 112.56(16) . . ?
V2 O7 V2A 26.86(12) . . ?
V2 O8 V2A 30.85(14) . . ?
V2 O8 V1 143.73(13) . . ?
V2A O8 V1 116.24(18) . . ?
V2 O8 V1 115.90(12) . 2_465 ?
V2A O8 V1 85.92(17) . 2_465 ?
V1 O8 V1 31.47(6) . 2_465 ?
P2 O9 V1 137.60(13) . . ?
P2 O9 V1 117.98(12) . 2_465 ?
V1 O9 V1 31.16(6) . 2_465 ?
C1 N1 C5 118.4(3) . . ?
C1 N1 Cu1 128.8(2) . . ?
C5 N1 Cu1 112.9(2) . . ?
C12 N2 C9 118.2(3) . . ?
C12 N2 Cu1 128.7(2) . . ?
C9 N2 Cu1 112.9(2) . . ?
N1 C1 C2 121.7(3) . . ?
C3 C2 C1 119.9(3) . . ?
C2 C3 C4 120.0(3) . . ?
C3 C4 C5 116.5(3) . . ?
C3 C4 C6 125.3(3) . . ?
C5 C4 C6 118.2(3) . . ?
N1 C5 C4 123.5(3) . . ?
N1 C5 C9 116.3(3) . . ?
C4 C5 C9 120.2(3) . . ?
C7 C6 C4 122.1(3) . . ?
C6 C7 C8 120.5(3) . . ?
C9 C8 C10 117.0(3) . . ?
C9 C8 C7 118.5(3) . . ?
C10 C8 C7 124.5(3) . . ?
N2 C9 C8 123.2(3) . . ?
N2 C9 C5 116.3(3) . . ?
C8 C9 C5 120.4(3) . . ?
C11 C10 C8 119.6(3) . . ?
C10 C11 C12 119.8(3) . . ?
N2 C12 C11 122.1(3) . . ?
C14 C13 P1 114.70(19) 1_545 . ?
C15 C14 C13 110.0(2) . 1_565 ?
C14 C15 P2 115.14(19) . . ?
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
Cu1 O4 1.905(2) . ?
Cu1 O1 1.9223(19) . ?
Cu1 N2 2.016(2) . ?
Cu1 N1 2.020(3) . ?
Cu1 O2 2.303(9) . ?
V1 V1 1.0587(19) 2_465 ?
V1 O2 1.608(7) 1_455 ?
V1 O8 1.862(2) . ?
V1 O9 1.903(2) . ?
V1 O2A 1.91(2) 1_455 ?
V1 O8 2.008(2) 2_465 ?
V1 O9 2.017(2) 2_465 ?
V1 V2A 2.599(4) 2_465 ?
V1 V2A 3.110(4) . ?
V2A V2 0.942(4) . ?
V2A O8 1.800(4) . ?
V2A O5 1.822(4) . ?
V2A O2A 1.923(17) 2_565 ?
V2A O3 1.987(4) . ?
V2A O7 2.073(4) . ?
V2A O2 2.313(14) 2_565 ?
V2A V1 2.599(4) 2_465 ?
V2 O6 1.597(2) . ?
V2 O8 1.734(2) . ?
V2 O3 1.9295(19) . ?
V2 O7 1.9504(19) . ?
V2 O5 1.968(2) . ?
P1 O4 1.515(2) . ?
P1 O3 1.532(2) . ?
P1 O5 1.534(2) 2_565 ?
P1 C13 1.794(3) . ?
P2 O1 1.519(2) 2_565 ?
P2 O7 1.530(2) . ?
P2 O9 1.552(2) . ?
P2 C15 1.795(3) . ?
O1 P2 1.519(2) 2_565 ?
O2 O2A 0.62(2) . ?
O2 V1 1.608(7) 1_655 ?
O2 V2A 2.313(14) 2_565 ?
O2A V1 1.91(2) 1_655 ?
O2A V2A 1.923(17) 2_565 ?
O5 P1 1.534(2) 2_565 ?
O8 V1 2.008(2) 2_465 ?
O9 V1 2.017(2) 2_465 ?
N1 C1 1.324(4) . ?
N1 C5 1.362(4) . ?
N2 C12 1.334(4) . ?
N2 C9 1.364(4) . ?
C1 C2 1.405(5) . ?
C2 C3 1.368(6) . ?
C3 C4 1.399(5) . ?
C4 C5 1.405(4) . ?
C4 C6 1.425(5) . ?
C5 C9 1.429(4) . ?
C6 C7 1.363(6) . ?
C7 C8 1.432(5) . ?
C8 C9 1.407(4) . ?
C8 C10 1.409(5) . ?
C10 C11 1.372(5) . ?
C11 C12 1.403(4) . ?
C13 C14 1.535(3) 1_545 ?
C14 C15 1.530(4) . ?
C14 C13 1.535(3) 1_565 ?
