#------------------------------------------------------------------------------
#$Date: 2016-03-23 04:05:21 +0200 (Wed, 23 Mar 2016) $
#$Revision: 179276 $
#$URL: svn://www.crystallography.net/cod/cif/4/31/96/4319699.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_4319699
loop_
_publ_author_name
'Robert C. Finn'
'Jon Zubieta'
_publ_section_title
;
 A New Class of Organic-Inorganic Hybrid Materials: Hydrothermal Synthesis
 and Structural Characterization of Bimetallic Organophosphonate Oxide
 Phases of the Mo/Cu/O/RPO32-Family
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              2466
_journal_page_last               2467
_journal_paper_doi               10.1021/ic0100018
_journal_volume                  40
_journal_year                    2001
_chemical_formula_sum            'C13 H14 Cu Mo2 N2 O11 P'
_chemical_formula_weight         660.65
_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                101.1370(10)
_cell_angle_beta                 104.176(2)
_cell_angle_gamma                110.0660(10)
_cell_formula_units_Z            2
_cell_length_a                   7.9401(7)
_cell_length_b                   10.4771(9)
_cell_length_c                   12.8953(11)
_cell_measurement_temperature    293(2)
_cell_volume                     930.60(14)
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 0.932
_diffrn_measured_fraction_theta_max 0.932
_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  0.0205
_diffrn_reflns_av_sigmaI/netI    0.0430
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -6
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            6279
_diffrn_reflns_theta_full        28.32
_diffrn_reflns_theta_max         28.32
_diffrn_reflns_theta_min         1.71
_exptl_absorpt_coefficient_mu    2.610
_exptl_crystal_density_diffrn    2.358
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             644
_refine_diff_density_max         1.745
_refine_diff_density_min         -1.096
_refine_diff_density_rms         0.212
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.146
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     279
_refine_ls_number_reflns         4314
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.146
_refine_ls_R_factor_all          0.0598
_refine_ls_R_factor_gt           0.0480
_refine_ls_shift/su_max          6.456
_refine_ls_shift/su_mean         0.023
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[σ²(Fo²)+(0.0001P)²+17.8147P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1104
_refine_ls_wR_factor_ref         0.1141
_reflns_number_gt                3601
_reflns_number_total             4314
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic0100018_2.cif
_cod_data_source_block           p-1
_cod_database_code               4319699
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
Mo1 Mo 0.51795(8) 0.53028(6) 0.38186(5) 0.00740(13) Uani 1 1 d . . .
Mo2 Mo 0.28601(9) 0.19207(6) 0.31970(5) 0.00832(13) Uani 1 1 d . . .
Cu1 Cu 0.38572(12) 0.84637(9) 0.29452(7) 0.00831(18) Uani 1 1 d . . .
P1 P 0.2545(2) 0.97493(18) 0.48074(14) 0.0058(3) Uani 1 1 d . . .
O1 O 0.3302(7) 1.1096(5) 0.4457(4) 0.0109(10) Uani 1 1 d . . .
O2 O 0.3670(7) 1.0089(5) 0.6046(4) 0.0091(9) Uani 1 1 d . . .
O3 O 0.2593(7) 0.8461(5) 0.4048(4) 0.0089(9) Uani 1 1 d . . .
O4 O 0.4235(7) 0.6356(5) 0.3231(4) 0.0128(10) Uani 1 1 d . . .
O5 O 0.7390(7) 0.5735(5) 0.3706(4) 0.0137(10) Uani 1 1 d . . .
O6 O 0.5776(8) 0.6215(5) 0.5400(4) 0.0165(11) Uani 1 1 d . . .
O7 O 0.3720(8) 0.3523(5) 0.2635(4) 0.0134(10) Uani 1 1 d . . .
O8 O 0.0576(8) 0.1682(6) 0.3054(5) 0.0250(13) Uani 1 1 d . . .
O9 O 0.2567(11) 0.0517(6) 0.2134(5) 0.0351(17) Uani 1 1 d . . .
O10 O 0.6099(10) 0.2364(8) 0.3546(6) 0.0305(15) Uani 1 1 d . . .
O100 O 0.8694(10) 0.4254(7) 0.5580(6) 0.0388(17) Uani 1 1 d . . .
N1 N 0.1346(8) 0.7309(6) 0.1693(5) 0.0082(11) Uani 1 1 d . . .
N2 N 0.4827(8) 0.8504(6) 0.1653(5) 0.0100(11) Uani 1 1 d . . .
C1 C -0.0405(10) 0.6747(7) 0.1738(6) 0.0122(14) Uani 1 1 d . . .
H1 H -0.0556 0.6806 0.2436 0.015 Uiso 1 1 calc R . .
C2 C -0.2037(11) 0.6065(8) 0.0763(6) 0.0159(15) Uani 1 1 d . . .
H2 H -0.3238 0.5691 0.0828 0.019 Uiso 1 1 calc R . .
C3 C -0.1863(10) 0.5952(8) -0.0281(6) 0.0156(15) Uani 1 1 d . . .
H3 H -0.2936 0.5501 -0.0925 0.019 Uiso 1 1 calc R . .
C4 C -0.0015(10) 0.6533(7) -0.0361(6) 0.0133(14) Uani 1 1 d . . .
C5 C 0.1533(10) 0.7212(7) 0.0663(5) 0.0077(12) Uani 1 1 d . . .
C6 C 0.0370(12) 0.6475(8) -0.1395(6) 0.0168(15) Uani 1 1 d . . .
H6 H -0.0642 0.6034 -0.2071 0.020 Uiso 1 1 calc R . .
C7 C 0.2176(11) 0.7049(8) -0.1412(6) 0.0157(15) Uani 1 1 d . . .
H7 H 0.2383 0.6973 -0.2097 0.019 Uiso 1 1 calc R . .
C8 C 0.3769(11) 0.7771(8) -0.0383(6) 0.0127(14) Uani 1 1 d . . .
C9 C 0.3420(10) 0.7832(7) 0.0641(6) 0.0100(13) Uani 1 1 d . . .
C10 C 0.5698(11) 0.8448(8) -0.0318(6) 0.0172(15) Uani 1 1 d . . .
H10 H 0.6007 0.8421 -0.0970 0.021 Uiso 1 1 calc R . .
C11 C 0.7080(11) 0.9133(8) 0.0701(6) 0.0162(15) Uani 1 1 d . . .
H11 H 0.8339 0.9589 0.0747 0.019 Uiso 1 1 calc R . .
C12 C 0.6626(10) 0.9159(7) 0.1691(6) 0.0118(13) Uani 1 1 d . . .
H12 H 0.7592 0.9639 0.2383 0.014 Uiso 1 1 calc R . .
C13 C 0.0112(9) 0.9343(7) 0.4681(5) 0.0086(13) Uani 1 1 d . . .
H13A H -0.0652 0.9038 0.3894 0.010 Uiso 1 1 calc R . .
H13B H -0.0351 0.8562 0.4983 0.010 Uiso 1 1 calc R . .
H10A H 0.654(11) 0.284(8) 0.426(7) 0.000(18) Uiso 1 1 d . . .
H10B H 0.631(14) 0.181(11) 0.398(9) 0.03(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 0.0033 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'
Cu Cu 0.3201 1.2651 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Mo Mo -1.6832 0.6857 '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
O5 Mo1 O4 107.0(2) . . ?
O5 Mo1 O7 101.6(2) . . ?
O4 Mo1 O7 99.0(2) . . ?
O5 Mo1 O6 102.1(2) . . ?
O4 Mo1 O6 100.5(2) . . ?
O7 Mo1 O6 143.2(2) . . ?
O5 Mo1 O6 119.0(2) . 2_666 ?
O4 Mo1 O6 134.0(2) . 2_666 ?
O7 Mo1 O6 74.2(2) . 2_666 ?
O6 Mo1 O6 69.8(2) . 2_666 ?
O5 Mo1 Mo2 112.00(17) . . ?
O4 Mo1 Mo2 122.55(17) . . ?
O7 Mo1 Mo2 33.78(14) . . ?
O6 Mo1 Mo2 110.30(15) . . ?
O6 Mo1 Mo2 40.55(14) 2_666 . ?
O8 Mo2 O9 102.5(3) . . ?
O8 Mo2 O7 102.1(2) . . ?
O9 Mo2 O7 102.8(2) . . ?
O8 Mo2 O1 97.5(2) . 1_545 ?
O9 Mo2 O1 98.2(3) . 1_545 ?
O7 Mo2 O1 147.3(2) . 1_545 ?
O8 Mo2 O6 97.5(3) . 2_666 ?
O9 Mo2 O6 160.0(3) . 2_666 ?
O7 Mo2 O6 72.9(2) . 2_666 ?
O1 Mo2 O6 78.8(2) 1_545 2_666 ?
O8 Mo2 O10 175.4(3) . . ?
O9 Mo2 O10 81.8(3) . . ?
O7 Mo2 O10 78.4(2) . . ?
O1 Mo2 O10 80.1(2) 1_545 . ?
O6 Mo2 O10 78.2(2) 2_666 . ?
O8 Mo2 Mo1 104.9(2) . . ?
O9 Mo2 Mo1 132.3(2) . . ?
O7 Mo2 Mo1 33.61(14) . . ?
O1 Mo2 Mo1 115.68(14) 1_545 . ?
O6 Mo2 Mo1 39.47(13) 2_666 . ?
O10 Mo2 Mo1 72.82(17) . . ?
O3 Cu1 O2 95.8(2) . 2_676 ?
O3 Cu1 N2 171.1(2) . . ?
O2 Cu1 N2 89.8(2) 2_676 . ?
O3 Cu1 N1 91.2(2) . . ?
O2 Cu1 N1 166.2(2) 2_676 . ?
N2 Cu1 N1 81.9(2) . . ?
O3 Cu1 O4 89.25(18) . . ?
O2 Cu1 O4 99.51(19) 2_676 . ?
N2 Cu1 O4 96.6(2) . . ?
N1 Cu1 O4 92.5(2) . . ?
O3 P1 O2 113.2(3) . . ?
O3 P1 O1 112.2(3) . . ?
O2 P1 O1 108.1(3) . . ?
O3 P1 C13 107.4(3) . . ?
O2 P1 C13 107.8(3) . . ?
O1 P1 C13 108.0(3) . . ?
P1 O1 Mo2 143.2(3) . 1_565 ?
P1 O2 Cu1 133.7(3) . 2_676 ?
P1 O3 Cu1 127.1(3) . . ?
Mo1 O4 Cu1 159.9(3) . . ?
Mo1 O6 Mo1 110.2(2) . 2_666 ?
Mo1 O6 Mo2 149.6(3) . 2_666 ?
Mo1 O6 Mo2 100.0(2) 2_666 2_666 ?
Mo1 O7 Mo2 112.6(2) . . ?
C1 N1 C5 117.9(6) . . ?
C1 N1 Cu1 129.8(5) . . ?
C5 N1 Cu1 112.1(4) . . ?
C12 N2 C9 119.1(6) . . ?
C12 N2 Cu1 127.7(5) . . ?
C9 N2 Cu1 113.0(4) . . ?
N1 C1 C2 122.2(7) . . ?
C3 C2 C1 120.4(7) . . ?
C2 C3 C4 118.9(7) . . ?
C5 C4 C3 116.7(6) . . ?
C5 C4 C6 118.7(7) . . ?
C3 C4 C6 124.6(7) . . ?
N1 C5 C4 124.0(6) . . ?
N1 C5 C9 116.6(6) . . ?
C4 C5 C9 119.4(6) . . ?
C7 C6 C4 121.6(7) . . ?
C6 C7 C8 120.6(7) . . ?
C9 C8 C10 116.9(6) . . ?
C9 C8 C7 118.5(7) . . ?
C10 C8 C7 124.6(7) . . ?
N2 C9 C8 122.8(6) . . ?
N2 C9 C5 116.2(6) . . ?
C8 C9 C5 121.0(6) . . ?
C11 C10 C8 119.4(7) . . ?
C10 C11 C12 120.6(7) . . ?
N2 C12 C11 121.1(7) . . ?
C13 C13 P1 111.2(6) 2_576 . ?
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
Mo1 O5 1.706(5) . ?
Mo1 O4 1.723(5) . ?
Mo1 O7 1.924(5) . ?
Mo1 O6 1.939(5) . ?
Mo1 O6 2.071(5) 2_666 ?
Mo1 Mo2 3.2082(8) . ?
Mo2 O8 1.701(6) . ?
Mo2 O9 1.710(6) . ?
Mo2 O7 1.932(5) . ?
Mo2 O1 1.995(5) 1_545 ?
Mo2 O6 2.118(5) 2_666 ?
Mo2 O10 2.359(6) . ?
Cu1 O3 1.931(5) . ?
Cu1 O2 1.947(5) 2_676 ?
Cu1 N2 2.001(6) . ?
Cu1 N1 2.015(6) . ?
Cu1 O4 2.411(5) . ?
P1 O3 1.524(5) . ?
P1 O2 1.529(5) . ?
P1 O1 1.534(5) . ?
P1 C13 1.787(7) . ?
O1 Mo2 1.995(5) 1_565 ?
O2 Cu1 1.947(5) 2_676 ?
O6 Mo1 2.071(5) 2_666 ?
O6 Mo2 2.118(5) 2_666 ?
N1 C1 1.332(9) . ?
N1 C5 1.361(8) . ?
N2 C12 1.340(9) . ?
N2 C9 1.356(9) . ?
C1 C2 1.411(10) . ?
C2 C3 1.374(11) . ?
C3 C4 1.421(11) . ?
C4 C5 1.415(10) . ?
C4 C6 1.434(10) . ?
C5 C9 1.424(9) . ?
C6 C7 1.359(11) . ?
C7 C8 1.438(10) . ?
C8 C9 1.408(9) . ?
C8 C10 1.423(11) . ?
C10 C11 1.355(11) . ?
C11 C12 1.406(10) . ?
C13 C13 1.552(13) 2_576 ?
