#------------------------------------------------------------------------------
#$Date: 2016-03-23 20:48:37 +0200 (Wed, 23 Mar 2016) $
#$Revision: 179425 $
#$URL: svn://www.crystallography.net/cod/cif/4/33/22/4332242.cif $
#------------------------------------------------------------------------------
#
# This file is available in the Crystallography Open Database (COD),
# http://www.crystallography.net/. The original data for this entry
# were provided the Crystal Eye server at
# http://wwmm.ch.cam.ac.uk/crystaleye/, created by Nick Day at the
# Peter Murray-Rust laboratory.
#
# The file may be used within the scientific community so long as
# proper attribution is given to the journal article from which the
# data were obtained.
#
data_4332242
loop_
_publ_author_name
'Ushak, Svetlana'
'Spodine, Evgenia'
'Le Fur, Eric'
'Venegas-Yazigi, Diego'
'Pivan, Jean-Yves'
'Schnelle, Walter'
'Cardoso-Gil, Raul'
'Kniep, Rüdiger'
_publ_section_title
;
 Two New Hybrid Organic/Inorganic Copper(II)−Oxovanadate(V)
 Diphosphonates: [Cu2(phen)2(O3PCH2PO3)(V2O5)(H2O)]·H2O and
 [Cu2(phen)2(O3P(CH2)3PO3)(V2O5)]·C3H8. Synthesis, Structure, and
 Magnetic Properties
;
_journal_issue                   14
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              5393
_journal_page_last               5398
_journal_paper_doi               10.1021/ic060152g
_journal_volume                  45
_journal_year                    2006
_chemical_formula_sum            'C25 H20 Cu2 N4 O13 P2 V2'
_chemical_formula_weight         875.35
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 93.988(2)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   11.7880(17)
_cell_length_b                   17.887(3)
_cell_length_c                   14.158(2)
_cell_measurement_reflns_used    999
_cell_measurement_temperature    298(2)
_cell_measurement_theta_max      24.615
_cell_measurement_theta_min      2.272
_cell_volume                     2978.0(8)
_computing_cell_refinement       'SMART-NT (Bruker, 2001)'
_computing_data_collection       'SMART-NT (Bruker, 2001)'
_computing_data_reduction        'SAINT-NT (Bruker, 2000)'
_computing_molecular_graphics    'Bruker SHELXTL-NT'
_computing_publication_material  'Bruker SHELXTL-NT'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      298(2)
_diffrn_measured_fraction_theta_full 0.929
_diffrn_measured_fraction_theta_max 0.929
_diffrn_measurement_device_type  'Brucker Smart Apex'
_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  0.0493
_diffrn_reflns_av_sigmaI/netI    0.0526
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       23
_diffrn_reflns_limit_k_min       -23
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            24950
_diffrn_reflns_theta_full        28.12
_diffrn_reflns_theta_max         28.12
_diffrn_reflns_theta_min         1.84
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    2.200
_exptl_absorpt_correction_T_max  1
_exptl_absorpt_correction_T_min  0.77
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_process_details   '(SADABS; Sheldrick, 1996)'
_exptl_crystal_colour            green
_exptl_crystal_density_diffrn    1.952
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             1744
_exptl_crystal_size_max          0.444
_exptl_crystal_size_mid          0.196
_exptl_crystal_size_min          0.074
_refine_diff_density_max         0.674
_refine_diff_density_min         -0.346
_refine_diff_density_rms         0.109
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.041
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     450
_refine_ls_number_reflns         6773
_refine_ls_number_restraints     2
_refine_ls_restrained_S_all      1.041
_refine_ls_R_factor_all          0.0667
_refine_ls_R_factor_gt           0.0473
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[σ²(Fo²)+(0.0527P)²+1.2336P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1041
_refine_ls_wR_factor_ref         0.1125
_reflns_number_gt                5287
_reflns_number_total             6773
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic060152gsup1.cif
_cod_data_source_block           su3009045
_cod_original_sg_symbol_H-M      P2(1)/n
_cod_database_code               4332242
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x+1/2, y+1/2, -z+1/2'
'-x, -y, -z'
'x-1/2, -y-1/2, z-1/2'
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 0.70017(4) 0.52138(3) 0.78378(3) 0.02854(13) Uani 1 1 d .
Cu2 Cu 0.38193(4) 0.54220(2) 0.51920(3) 0.02550(12) Uani 1 1 d .
V1 V 0.38272(5) 0.33606(3) 0.82621(4) 0.02638(15) Uani 1 1 d .
V2 V 0.29035(5) 0.70981(3) 0.76132(4) 0.02749(16) Uani 1 1 d .
P1 P 0.48389(8) 0.45024(5) 0.68795(6) 0.0236(2) Uani 1 1 d .
P2 P 0.48971(7) 0.61281(5) 0.70016(6) 0.0232(2) Uani 1 1 d .
O1 O 0.6050(2) 0.44305(13) 0.72716(18) 0.0323(6) Uani 1 1 d .
O2 O 0.4142(2) 0.38109(13) 0.71160(17) 0.0334(6) Uani 1 1 d .
O3 O 0.4754(2) 0.46180(13) 0.58144(16) 0.0269(5) Uani 1 1 d .
O4 O 0.4623(2) 0.61921(13) 0.59459(17) 0.0320(6) Uani 1 1 d .
O5 O 0.4411(2) 0.68147(13) 0.74989(18) 0.0306(6) Uani 1 1 d .
O6 O 0.61459(19) 0.60613(13) 0.72900(17) 0.0294(6) Uani 1 1 d .
O7 O 0.3771(3) 0.39872(16) 0.9077(2) 0.0455(7) Uani 1 1 d .
O8 O 0.4853(3) 0.28011(16) 0.8566(2) 0.0481(8) Uani 1 1 d .
O9 O 0.2480(2) 0.28963(15) 0.81125(19) 0.0395(7) Uani 1 1 d .
O10 O 0.2092(2) 0.64022(16) 0.7318(2) 0.0448(7) Uani 1 1 d .
O11 O 0.2789(2) 0.72947(17) 0.87203(19) 0.0439(7) Uani 1 1 d .
O1W O 0.6238(3) 0.5145(2) 0.9246(2) 0.0474(8) Uani 1 1 d D
O2WA O 0.3924(16) 0.6308(12) -0.0093(10) 0.083(5) Uani 0.50 1 d P
O2WB O 0.3615(12) 0.6318(10) 0.0208(9) 0.056(3) Uani 0.50 1 d P
N1 N 0.8303(2) 0.58847(19) 0.8218(2) 0.0317(7) Uani 1 1 d .
N2 N 0.8156(3) 0.44166(19) 0.8201(2) 0.0376(8) Uani 1 1 d .
N3 N 0.2599(3) 0.61460(16) 0.4747(2) 0.0277(7) Uani 1 1 d .
N4 N 0.2647(3) 0.46813(16) 0.4680(2) 0.0284(7) Uani 1 1 d .
C1 C 0.8349(4) 0.6623(2) 0.8192(3) 0.0416(10) Uani 1 1 d .
H1 H 0.7703 0.6887 0.7974 0.050 Uiso 1 1 calc R
C2 C 0.9324(4) 0.7016(3) 0.8479(3) 0.0514(12) Uani 1 1 d .
H2 H 0.9328 0.7536 0.8460 0.062 Uiso 1 1 calc R
C3 C 1.0280(4) 0.6632(3) 0.8791(3) 0.0594(15) Uani 1 1 d .
H3 H 1.0938 0.6891 0.8989 0.071 Uiso 1 1 calc R
C4 C 1.0269(3) 0.5856(3) 0.8813(3) 0.0504(13) Uani 1 1 d .
C5 C 1.1227(4) 0.5386(4) 0.9103(3) 0.0693(18) Uani 1 1 d .
H5 H 1.1916 0.5609 0.9303 0.083 Uiso 1 1 calc R
C6 C 1.1152(4) 0.4643(4) 0.9093(4) 0.0721(19) Uani 1 1 d .
H6 H 1.1788 0.4360 0.9285 0.087 Uiso 1 1 calc R
C7 C 1.0121(4) 0.4272(3) 0.8795(3) 0.0516(13) Uani 1 1 d .
C8 C 0.9968(5) 0.3504(3) 0.8749(3) 0.0626(16) Uani 1 1 d .
H8 H 1.0574 0.3187 0.8919 0.075 Uiso 1 1 calc R
C9 C 0.8939(5) 0.3212(3) 0.8458(3) 0.0600(14) Uani 1 1 d .
H9 H 0.8835 0.2696 0.8440 0.072 Uiso 1 1 calc R
C10 C 0.8042(4) 0.3686(3) 0.8187(3) 0.0484(11) Uani 1 1 d .
H10 H 0.7341 0.3480 0.7990 0.058 Uiso 1 1 calc R
C11 C 0.9175(3) 0.4706(3) 0.8514(3) 0.0395(10) Uani 1 1 d .
C12 C 0.9253(3) 0.5503(3) 0.8520(3) 0.0384(10) Uani 1 1 d .
C13 C 0.2588(3) 0.6879(2) 0.4836(3) 0.0336(9) Uani 1 1 d .
H13 H 0.3229 0.7117 0.5113 0.040 Uiso 1 1 calc R
C14 C 0.1653(4) 0.7309(2) 0.4530(3) 0.0420(10) Uani 1 1 d .
H14 H 0.1676 0.7825 0.4603 0.050 Uiso 1 1 calc R
C15 C 0.0698(4) 0.6972(2) 0.4122(3) 0.0428(10) Uani 1 1 d .
H15 H 0.0073 0.7257 0.3909 0.051 Uiso 1 1 calc R
C16 C 0.0673(3) 0.6193(2) 0.4028(3) 0.0334(9) Uani 1 1 d .
C17 C -0.0280(3) 0.5770(3) 0.3643(3) 0.0423(11) Uani 1 1 d .
H17 H -0.0933 0.6020 0.3412 0.051 Uiso 1 1 calc R
C18 C -0.0256(3) 0.5018(3) 0.3607(3) 0.0404(10) Uani 1 1 d .
H18 H -0.0891 0.4760 0.3353 0.049 Uiso 1 1 calc R
C19 C 0.0730(3) 0.4609(2) 0.3953(3) 0.0347(9) Uani 1 1 d .
C20 C 0.0806(4) 0.3833(2) 0.3975(3) 0.0424(11) Uani 1 1 d .
H20 H 0.0198 0.3543 0.3736 0.051 Uiso 1 1 calc R
C21 C 0.1777(4) 0.3500(2) 0.4350(3) 0.0423(10) Uani 1 1 d .
H21 H 0.1829 0.2981 0.4374 0.051 Uiso 1 1 calc R
C22 C 0.2692(4) 0.3940(2) 0.4700(3) 0.0352(9) Uani 1 1 d .
H22 H 0.3349 0.3708 0.4954 0.042 Uiso 1 1 calc R
C23 C 0.1679(3) 0.5012(2) 0.4316(2) 0.0276(8) Uani 1 1 d .
C24 C 0.1649(3) 0.5805(2) 0.4350(2) 0.0278(8) Uani 1 1 d .
C25 C 0.4210(3) 0.53020(18) 0.7408(2) 0.0255(8) Uani 1 1 d .
H25A H 0.4310 0.5269 0.8093 0.031 Uiso 1 1 calc R
H25B H 0.3402 0.5321 0.7226 0.031 Uiso 1 1 calc R
H1W H 0.611(4) 0.541(2) 0.964(3) 0.038(14) Uiso 1 1 d D
H2W H 0.618(5) 0.470(3) 0.944(4) 0.09(2) Uiso 1 1 d 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
O1 Cu1 O6 97.42(10) . .
O1 Cu1 N1 164.19(12) . .
O6 Cu1 N1 90.36(12) . .
O1 Cu1 N2 87.43(12) . .
O6 Cu1 N2 166.76(13) . .
N1 Cu1 N2 82.16(14) . .
O1 Cu1 O1W 94.08(12) . .
O6 Cu1 O1W 99.64(12) . .
N1 Cu1 O1W 98.17(13) . .
N2 Cu1 O1W 92.27(13) . .
O4 Cu2 O3 92.03(10) . .
O4 Cu2 N3 91.52(11) . .
O3 Cu2 N3 166.86(11) . .
O4 Cu2 N4 163.45(12) . .
O3 Cu2 N4 91.66(11) . .
N3 Cu2 N4 81.51(12) . .
O4 Cu2 O3 90.72(10) . 3_666
O3 Cu2 O3 81.00(10) . 3_666
N3 Cu2 O3 111.60(10) . 3_666
N4 Cu2 O3 105.79(11) . 3_666
O8 V1 O7 107.99(16) . .
O8 V1 O9 112.81(15) . .
O7 V1 O9 109.07(14) . .
O8 V1 O2 108.04(14) . .
O7 V1 O2 109.96(13) . .
O9 V1 O2 108.94(12) . .
O10 V2 O11 109.37(16) . .
O10 V2 O9 110.16(14) . 2_556
O11 V2 O9 110.23(14) . 2_556
O10 V2 O5 108.67(13) . .
O11 V2 O5 106.65(13) . .
O9 V2 O5 111.68(12) 2_556 .
O1 P1 O3 111.99(14) . .
O1 P1 O2 111.11(15) . .
O3 P1 O2 109.09(14) . .
O1 P1 C25 108.87(16) . .
O3 P1 C25 107.71(15) . .
O2 P1 C25 107.94(15) . .
O6 P2 O4 114.33(15) . .
O6 P2 O5 109.04(14) . .
O4 P2 O5 109.26(15) . .
O6 P2 C25 107.56(15) . .
O4 P2 C25 107.97(15) . .
O5 P2 C25 108.52(15) . .
P1 O1 Cu1 126.93(15) . .
P1 O2 V1 132.64(16) . .
P1 O3 Cu2 122.48(14) . .
P1 O3 Cu2 128.00(14) . 3_666
Cu2 O3 Cu2 99.00(10) . 3_666
P2 O4 Cu2 123.41(14) . .
P2 O5 V2 129.88(15) . .
P2 O6 Cu1 129.67(15) . .
V1 O9 V2 128.41(16) . 2_546
C1 N1 C12 118.5(4) . .
C1 N1 Cu1 128.8(3) . .
C12 N1 Cu1 112.7(3) . .
C10 N2 C11 118.2(4) . .
C10 N2 Cu1 129.4(3) . .
C11 N2 Cu1 112.4(3) . .
C13 N3 C24 118.1(3) . .
C13 N3 Cu2 128.7(3) . .
C24 N3 Cu2 113.1(2) . .
C22 N4 C23 118.4(3) . .
C22 N4 Cu2 128.7(3) . .
C23 N4 Cu2 112.9(2) . .
N1 C1 C2 122.3(4) . .
C3 C2 C1 119.3(5) . .
C2 C3 C4 120.1(4) . .
C3 C4 C12 117.1(4) . .
C3 C4 C5 125.4(5) . .
C12 C4 C5 117.4(5) . .
C6 C5 C4 121.8(5) . .
C5 C6 C7 121.6(5) . .
C8 C7 C11 116.1(5) . .
C8 C7 C6 125.6(5) . .
C11 C7 C6 118.4(5) . .
C9 C8 C7 120.4(4) . .
C8 C9 C10 119.7(5) . .
N2 C10 C9 121.9(5) . .
N2 C11 C7 123.7(5) . .
N2 C11 C12 116.0(4) . .
C7 C11 C12 120.3(4) . .
N1 C12 C4 122.7(4) . .
N1 C12 C11 116.7(4) . .
C4 C12 C11 120.5(4) . .
N3 C13 C14 122.3(4) . .
C15 C14 C13 120.0(4) . .
C14 C15 C16 119.3(4) . .
C24 C16 C15 116.9(4) . .
C24 C16 C17 118.0(4) . .
C15 C16 C17 125.0(4) . .
C18 C17 C16 121.7(4) . .
C17 C18 C19 121.1(4) . .
C20 C19 C23 117.2(4) . .
C20 C19 C18 124.6(4) . .
C23 C19 C18 118.2(4) . .
C21 C20 C19 119.7(4) . .
C20 C21 C22 119.8(4) . .
N4 C22 C21 121.8(4) . .
N4 C23 C19 123.1(4) . .
N4 C23 C24 116.4(3) . .
C19 C23 C24 120.5(3) . .
N3 C24 C16 123.3(3) . .
N3 C24 C23 116.1(3) . .
C16 C24 C23 120.5(3) . .
P1 C25 P2 108.22(18) . .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
Cu1 O1 1.934(2) .
Cu1 O6 1.952(2) .
Cu1 N1 1.992(3) .
Cu1 N2 2.013(3) .
Cu1 O1W 2.247(3) .
Cu2 O4 1.948(2) .
Cu2 O3 1.981(2) .
Cu2 N3 2.004(3) .
Cu2 N4 2.013(3) .
Cu2 O3 2.280(2) 3_666
V1 O8 1.606(3) .
V1 O7 1.613(3) .
V1 O9 1.791(3) .
V1 O2 1.872(2) .
V2 O10 1.608(3) .
V2 O11 1.621(3) .
V2 O9 1.798(3) 2_556
V2 O5 1.866(2) .
P1 O1 1.501(3) .
P1 O3 1.519(2) .
P1 O2 1.535(3) .
P1 C25 1.798(3) .
P2 O6 1.505(2) .
P2 O4 1.511(3) .
P2 O5 1.545(2) .
P2 C25 1.799(3) .
O3 Cu2 2.280(2) 3_666
O9 V2 1.798(3) 2_546
O2WA O2WB 0.58(2) .
N1 C1 1.322(5) .
N1 C12 1.355(5) .
N2 C10 1.314(5) .
N2 C11 1.354(5) .
N3 C13 1.318(5) .
N3 C24 1.361(4) .
N4 C22 1.327(5) .
N4 C23 1.355(5) .
C1 C2 1.384(6) .
C2 C3 1.366(7) .
C3 C4 1.388(7) .
C4 C12 1.392(6) .
C4 C5 1.445(7) .
C5 C6 1.333(8) .
C6 C7 1.422(8) .
C7 C8 1.386(7) .
C7 C11 1.394(6) .
C8 C9 1.359(8) .
C9 C10 1.388(6) .
C11 C12 1.429(6) .
C13 C14 1.387(5) .
C14 C15 1.369(6) .
C15 C16 1.399(6) .
C16 C24 1.393(5) .
C16 C17 1.431(6) .
C17 C18 1.346(6) .
C18 C19 1.431(6) .
C19 C20 1.390(6) .
C19 C23 1.398(5) .
C20 C21 1.364(6) .
C21 C22 1.398(5) .
C23 C24 1.421(5) .
