#------------------------------------------------------------------------------
#$Date: 2016-03-23 00:40:34 +0200 (Wed, 23 Mar 2016) $
#$Revision: 179122 $
#$URL: svn://www.crystallography.net/cod/cif/4/30/84/4308456.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_4308456
loop_
_publ_author_name
'Bing-Ping Yang'
'Jiang-Gao Mao'
_publ_contact_author_address
;
     Fujian Institute of Research  
        on the Structure of Matter,
        Chinese Academy of Sciences,
        Fuzhou, Fujian 350002, 
    P.R.China
;
_publ_contact_author_email       mjg@ms.fjirsm.ac.cn
_publ_contact_author_fax         0086-0591-3704836
_publ_contact_author_name        'Dr. Jiang-Gao Mao'
_publ_contact_author_phone       0086-0591-3704836
_publ_section_title
;
New Types of Metal Squarato-phosphonates: Condensation of
Aminodiphosphonate with Squaric Acid under Hydrothermal Conditions
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              566
_journal_page_last               571
_journal_paper_doi               10.1021/ic048685h
_journal_volume                  44
_journal_year                    2005
_chemical_formula_moiety         'C26 H26 Cu2 N5 O11 P2'
_chemical_formula_sum            'C26 H26 Cu2 N5 O11 P2'
_chemical_formula_weight         773.54
_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                77.8860(10)
_cell_angle_beta                 65.2130(10)
_cell_angle_gamma                63.5380(10)
_cell_formula_units_Z            2
_cell_length_a                   11.7680(4)
_cell_length_b                   12.1790(4)
_cell_length_c                   12.6422(4)
_cell_measurement_reflns_used    5025
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      25.00
_cell_measurement_theta_min      1.77
_cell_volume                     1472.05(9)
_computing_cell_refinement       'Siemens SMART'
_computing_data_collection       'Siemens SMART'
_computing_data_reduction        'Siemens SHELXTL'
_computing_molecular_graphics    'Siemens SHELXTL'
_computing_publication_material  'Siemens SHELXTL'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 0.973
_diffrn_measured_fraction_theta_max 0.973
_diffrn_measurement_device_type  'Siemens Smart 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  0.0191
_diffrn_reflns_av_sigmaI/netI    0.0274
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_limit_l_min       -7
_diffrn_reflns_number            7469
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         25.00
_diffrn_reflns_theta_min         1.77
_diffrn_standards_decay_%        <1.0%
_exptl_absorpt_coefficient_mu    1.624
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.62785
_exptl_absorpt_correction_type   SADABS
_exptl_crystal_colour            brown
_exptl_crystal_density_diffrn    1.745
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       brick
_exptl_crystal_F_000             786
_exptl_crystal_size_max          0.38
_exptl_crystal_size_mid          0.34
_exptl_crystal_size_min          0.30
_refine_diff_density_max         0.655
_refine_diff_density_min         -0.672
_refine_diff_density_rms         0.081
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.069
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     415
_refine_ls_number_reflns         5025
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.069
_refine_ls_R_factor_all          0.0498
_refine_ls_R_factor_gt           0.0441
_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)+(0.0510P)²+3.1495P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1107
_refine_ls_wR_factor_ref         0.1172
_reflns_number_gt                4525
_reflns_number_total             5025
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic048685hsi20040920_050314.cif
_cod_data_source_block           Cu
_cod_original_cell_volume        1472.05(8)
_cod_database_code               4308456
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 1.02413(5) -0.10495(4) 0.18211(5) 0.04334(16) Uani 1 1 d . . .
Cu2 Cu 0.02090(4) 0.65724(4) 0.43853(4) 0.04149(16) Uani 1 1 d . . .
P1 P 1.23082(9) 0.32987(8) -0.11000(8) 0.0275(2) Uani 1 1 d . . .
P2 P 0.92088(9) 0.37677(8) 0.30111(7) 0.0274(2) Uani 1 1 d . . .
N1 N 1.1474(3) 0.2527(3) 0.1177(2) 0.0290(6) Uani 1 1 d . . .
N2 N 0.2001(3) 0.5294(3) 0.3783(3) 0.0335(7) Uani 1 1 d . . .
N3 N 0.8480(3) 0.0242(3) 0.2219(3) 0.0366(7) Uani 1 1 d . . .
N4 N 1.1863(3) -0.2465(3) 0.1239(3) 0.0362(7) Uani 1 1 d . . .
N5 N -0.1623(3) 0.7770(3) 0.4616(3) 0.0346(7) Uani 1 1 d . . .
C1 C 1.2103(3) 0.0321(3) 0.2020(3) 0.0304(7) Uani 1 1 d . . .
C2 C 1.3575(4) -0.0271(3) 0.1819(3) 0.0318(8) Uani 1 1 d . . .
C3 C 1.3748(3) 0.0848(3) 0.1184(3) 0.0294(7) Uani 1 1 d . . .
C4 C 1.2288(3) 0.1412(3) 0.1420(3) 0.0265(7) Uani 1 1 d . . .
C5 C 1.2072(4) 0.3367(3) 0.0397(3) 0.0308(7) Uani 1 1 d . . .
H5A H 1.2950 0.3164 0.0438 0.037 Uiso 1 1 calc R . .
H5B H 1.1480 0.4199 0.0661 0.037 Uiso 1 1 calc R . .
C6 C 0.9985(3) 0.2932(3) 0.1677(3) 0.0278(7) Uani 1 1 d . . .
H6A H 0.9761 0.2222 0.1843 0.033 Uiso 1 1 calc R . .
H6B H 0.9605 0.3456 0.1111 0.033 Uiso 1 1 calc R . .
C11 C 0.3028(4) 0.5245(3) 0.4035(3) 0.0345(8) Uani 1 1 d . . .
H11A H 0.2867 0.5880 0.4450 0.041 Uiso 1 1 calc R . .
C12 C 0.4313(3) 0.4292(3) 0.3705(3) 0.0330(8) Uani 1 1 d . . .
H12A H 0.4986 0.4298 0.3904 0.040 Uiso 1 1 calc R . .
C13 C 0.4602(3) 0.3327(3) 0.3079(3) 0.0278(7) Uani 1 1 d . . .
C14 C 0.3544(4) 0.3415(3) 0.2778(3) 0.0354(8) Uani 1 1 d . . .
H14A H 0.3692 0.2813 0.2330 0.042 Uiso 1 1 calc R . .
C15 C 0.2291(4) 0.4385(4) 0.3142(4) 0.0397(9) Uani 1 1 d . . .
H15A H 0.1608 0.4415 0.2933 0.048 Uiso 1 1 calc R . .
C16 C 0.5936(3) 0.2258(3) 0.2771(3) 0.0285(7) Uani 1 1 d . . .
C17 C 0.6787(3) 0.1992(3) 0.3368(3) 0.0306(7) Uani 1 1 d . . .
H17A H 0.6520 0.2485 0.3972 0.037 Uiso 1 1 calc R . .
C18 C 0.8026(3) 0.1001(3) 0.3069(3) 0.0340(8) Uani 1 1 d . . .
H18A H 0.8579 0.0848 0.3480 0.041 Uiso 1 1 calc R . .
C19 C 0.7632(4) 0.0480(4) 0.1657(4) 0.0480(11) Uani 1 1 d . . .
H19A H 0.7901 -0.0051 0.1085 0.058 Uiso 1 1 calc R . .
C20 C 0.6393(4) 0.1472(4) 0.1894(4) 0.0425(10) Uani 1 1 d . . .
H20A H 0.5861 0.1615 0.1465 0.051 Uiso 1 1 calc R . .
C21 C 1.2955(4) -0.2740(3) 0.1504(3) 0.0377(9) Uani 1 1 d . . .
H21A H 1.2877 -0.2250 0.2026 0.045 Uiso 1 1 calc R . .
C22 C 1.4183(4) -0.3711(3) 0.1040(3) 0.0354(8) Uani 1 1 d . . .
H22A H 1.4908 -0.3863 0.1252 0.042 Uiso 1 1 calc R . .
C23 C 1.4349(3) -0.4468(3) 0.0257(3) 0.0282(7) Uani 1 1 d . . .
C24 C 1.3209(4) -0.4175(3) -0.0018(4) 0.0371(8) Uani 1 1 d . . .
H24A H 1.3264 -0.4645 -0.0543 0.045 Uiso 1 1 calc R . .
C25 C 1.2009(4) -0.3195(4) 0.0486(4) 0.0422(9) Uani 1 1 d . . .
H25A H 1.1263 -0.3029 0.0298 0.051 Uiso 1 1 calc R . .
C26 C -0.2364(4) 0.7694(4) 0.4095(4) 0.0503(11) Uani 1 1 d . . .
H26A H -0.1972 0.7040 0.3608 0.060 Uiso 1 1 calc R . .
C27 C -0.3671(4) 0.8527(4) 0.4236(4) 0.0479(11) Uani 1 1 d . . .
H27A H -0.4141 0.8413 0.3861 0.057 Uiso 1 1 calc R . .
C28 C -0.4298(3) 0.9527(3) 0.4923(3) 0.0264(7) Uani 1 1 d . . .
C29 C -0.3528(4) 0.9605(4) 0.5476(4) 0.0389(9) Uani 1 1 d . . .
H29A H -0.3894 1.0258 0.5956 0.047 Uiso 1 1 calc R . .
C30 C -0.2235(4) 0.8724(4) 0.5314(4) 0.0403(9) Uani 1 1 d . . .
H30A H -0.1759 0.8792 0.5709 0.048 Uiso 1 1 calc R . .
O1 O 1.1112(3) 0.0008(2) 0.2513(2) 0.0404(6) Uani 1 1 d . . .
O2 O 1.4324(3) -0.1279(2) 0.2118(2) 0.0429(7) Uani 1 1 d . . .
O3 O 1.4699(3) 0.1183(2) 0.0696(2) 0.0392(6) Uani 1 1 d . . .
O11 O 1.0897(2) 0.3691(2) -0.1138(2) 0.0383(6) Uani 1 1 d . . .
O12 O 1.3125(3) 0.1922(2) -0.1410(2) 0.0383(6) Uani 1 1 d . . .
H12B H 1.3946 0.1750 -0.1635 0.057 Uiso 1 1 calc R . .
O13 O 1.3065(2) 0.4087(2) -0.1820(2) 0.0355(6) Uani 1 1 d . . .
O21 O 0.9628(3) 0.2950(2) 0.3956(2) 0.0373(6) Uani 1 1 d . . .
O22 O 0.9604(2) 0.4869(2) 0.2709(2) 0.0328(5) Uani 1 1 d . . .
O23 O 0.7641(2) 0.4218(2) 0.3316(2) 0.0353(6) Uani 1 1 d . . .
H23A H 0.7410 0.4757 0.2844 0.053 Uiso 1 1 calc R . .
O1W O 1.1668(4) -0.1422(4) 0.4509(4) 0.0870(13) Uani 1 1 d . . .
O2W O 1.4558(4) -0.3083(3) 0.4027(3) 0.0612(9) Uani 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'
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
N3 Cu1 N4 167.36(14) . . ?
N3 Cu1 O1 93.13(11) . . ?
N4 Cu1 O1 99.18(11) . . ?
N2 Cu2 N5 164.35(13) . . ?
N2 Cu2 O21 98.38(11) . 2_666 ?
N5 Cu2 O21 97.25(11) . 2_666 ?
O13 P1 O11 115.29(14) . . ?
O13 P1 O12 113.29(15) . . ?
O11 P1 O12 107.19(15) . . ?
O13 P1 C5 107.07(16) . . ?
O11 P1 C5 107.55(16) . . ?
O12 P1 C5 105.91(15) . . ?
O21 P2 O22 113.31(15) . . ?
O21 P2 O23 111.26(15) . . ?
O22 P2 O23 110.10(14) . . ?
O21 P2 C6 111.05(15) . . ?
O22 P2 C6 107.27(15) . . ?
O23 P2 C6 103.32(15) . . ?
C4 N1 C6 121.0(3) . . ?
C4 N1 C5 119.7(3) . . ?
C6 N1 C5 119.3(3) . . ?
C15 N2 C11 116.7(3) . . ?
C15 N2 Cu2 122.9(2) . . ?
C11 N2 Cu2 120.4(2) . . ?
C18 N3 C19 116.3(3) . . ?
C18 N3 Cu1 120.4(2) . . ?
C19 N3 Cu1 123.3(3) . . ?
C21 N4 C25 116.9(3) . . ?
C21 N4 Cu1 121.1(3) . . ?
C25 N4 Cu1 121.8(2) . . ?
C26 N5 C30 116.0(3) . . ?
C26 N5 Cu2 121.8(3) . . ?
C30 N5 Cu2 122.2(2) . . ?
O1 C1 C4 135.7(3) . . ?
O1 C1 C2 135.3(3) . . ?
C4 C1 C2 89.0(3) . . ?
O2 C2 C1 134.0(3) . . ?
O2 C2 C3 135.9(3) . . ?
C1 C2 C3 90.1(3) . . ?
O3 C3 C4 135.3(3) . . ?
O3 C3 C2 136.3(3) . . ?
C4 C3 C2 88.4(3) . . ?
N1 C4 C1 135.5(3) . . ?
N1 C4 C3 132.0(3) . . ?
C1 C4 C3 92.5(3) . . ?
N1 C5 P1 112.5(2) . . ?
N1 C6 P2 112.1(2) . . ?
N2 C11 C12 123.0(3) . . ?
C11 C12 C13 120.5(3) . . ?
C12 C13 C14 116.0(3) . . ?
C12 C13 C16 122.0(3) . . ?
C14 C13 C16 122.0(3) . . ?
C15 C14 C13 120.2(3) . . ?
N2 C15 C14 123.5(3) . . ?
C17 C16 C20 116.7(3) . . ?
C17 C16 C13 120.7(3) . . ?
C20 C16 C13 122.6(3) . . ?
C18 C17 C16 120.0(3) . . ?
N3 C18 C17 123.7(3) . . ?
N3 C19 C20 123.0(4) . . ?
C19 C20 C16 120.1(4) . . ?
N4 C21 C22 123.1(3) . . ?
C21 C22 C23 120.5(3) . . ?
C22 C23 C24 116.2(3) . . ?
C22 C23 C23 122.3(4) . 2_845 ?
C24 C23 C23 121.5(4) . 2_845 ?
C25 C24 C23 120.3(3) . . ?
N4 C25 C24 123.1(3) . . ?
N5 C26 C27 123.6(4) . . ?
C26 C27 C28 121.1(4) . . ?
C27 C28 C29 115.4(3) . . ?
C27 C28 C28 123.0(4) . 2_476 ?
C29 C28 C28 121.6(4) . 2_476 ?
C30 C29 C28 120.4(3) . . ?
N5 C30 C29 123.5(3) . . ?
C1 O1 Cu1 132.2(2) . . ?
C2 O2 O12 121.4(2) . 2_855 ?
C2 O2 O2W 145.1(2) . . ?
O12 O2 O2W 87.65(12) 2_855 . ?
P1 O11 O22 116.49(15) . 2_765 ?
P1 O13 O23 125.68(14) . 2_765 ?
P1 O13 O2W 118.29(16) . 2_855 ?
O23 O13 O2W 78.95(11) 2_765 2_855 ?
P2 O21 Cu2 130.22(16) . 2_666 ?
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 N3 1.891(3) . ?
Cu1 N4 1.891(3) . ?
Cu1 O1 2.423(3) . ?
Cu2 N2 1.917(3) . ?
Cu2 N5 1.926(3) . ?
Cu2 O21 2.392(3) 2_666 ?
P1 O13 1.503(3) . ?
P1 O11 1.529(2) . ?
P1 O12 1.553(3) . ?
P1 C5 1.809(4) . ?
P2 O21 1.490(2) . ?
P2 O22 1.534(3) . ?
P2 O23 1.564(2) . ?
P2 C6 1.821(3) . ?
N1 C4 1.330(4) . ?
N1 C6 1.465(4) . ?
N1 C5 1.467(4) . ?
N2 C15 1.345(5) . ?
N2 C11 1.347(5) . ?
N3 C18 1.338(5) . ?
N3 C19 1.353(5) . ?
N4 C21 1.344(5) . ?
N4 C25 1.345(5) . ?
N5 C26 1.336(5) . ?
N5 C30 1.341(5) . ?
C1 O1 1.258(4) . ?
C1 C4 1.443(5) . ?
C1 C2 1.476(5) . ?
C2 O2 1.244(4) . ?
C2 C3 1.481(5) . ?
C3 O3 1.233(4) . ?
C3 C4 1.455(5) . ?
C11 C12 1.384(5) . ?
C12 C13 1.389(5) . ?
C13 C14 1.403(5) . ?
C13 C16 1.480(5) . ?
C14 C15 1.375(5) . ?
C16 C17 1.386(5) . ?
C16 C20 1.387(5) . ?
C17 C18 1.373(5) . ?
C19 C20 1.375(5) . ?
C21 C22 1.374(5) . ?
C22 C23 1.388(5) . ?
C23 C24 1.400(5) . ?
C23 C23 1.483(6) 2_845 ?
C24 C25 1.373(5) . ?
C26 C27 1.372(5) . ?
C27 C28 1.374(5) . ?
C28 C29 1.398(5) . ?
C28 C28 1.490(6) 2_476 ?
C29 C30 1.373(5) . ?
O2 O12 2.524(4) 2_855 ?
O2 O2W 2.919(4) . ?
O11 O22 2.443(3) 2_765 ?
O13 O23 2.583(3) 2_765 ?
O13 O2W 2.990(4) 2_855 ?
O21 Cu2 2.392(3) 2_666 ?
