#------------------------------------------------------------------------------
#$Date: 2019-11-28 20:47:44 +0200 (Thu, 28 Nov 2019) $
#$Revision: 244576 $
#$URL: file:///home/coder/svn-repositories/cod/cif/7/23/91/7239161.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_7239161
loop_
_publ_author_name
'Ma, Yun-Sheng'
'Yin, Wen-Yu'
'Cai, Wang-Shui'
'Zhu, Ping-Zhou'
'Tang, Xiao-Yan'
'Yuan, Rong-Xin'
'Roy, Soumyajit'
_publ_section_title
;
 Eight novel metal diphosphonates based on
 2-(4-pyridinyl)-1-hydroxyl-1,1-ethylidenediphosphonate: syntheses,
 structures, and magnetic properties
;
_journal_issue                   40
_journal_name_full               'RSC Advances'
_journal_page_first              18430
_journal_paper_doi               10.1039/c3ra43137a
_journal_volume                  3
_journal_year                    2013
_chemical_formula_moiety         'C7 H9 Cu N O7 P2'
_chemical_formula_sum            'C7 H9 Cu N O7 P2'
_chemical_formula_weight         344.63
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_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                94.13(3)
_cell_angle_beta                 103.16(3)
_cell_angle_gamma                102.49(3)
_cell_formula_units_Z            2
_cell_length_a                   5.5056(11)
_cell_length_b                   9.820(2)
_cell_length_c                   9.839(2)
_cell_measurement_temperature    293(2)
_cell_volume                     501.6(2)
_computing_cell_refinement       CrystalClear
_computing_data_collection       'CrystalClear (Rigaku, 2005)'
_computing_data_reduction        CrystalClear
_computing_molecular_graphics    'Bruker SHELXTL/PC (Sheldrick, 1999)'
_computing_publication_material  'Bruker SHELXTL/PC and PLATON (Spek, 2003)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 0.992
_diffrn_measured_fraction_theta_max 0.992
_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  0.0731
_diffrn_reflns_av_sigmaI/netI    0.0955
_diffrn_reflns_limit_h_max       6
_diffrn_reflns_limit_h_min       -6
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       12
_diffrn_reflns_limit_l_min       -12
_diffrn_reflns_number            4500
_diffrn_reflns_theta_full        26.00
_diffrn_reflns_theta_max         26.00
_diffrn_reflns_theta_min         3.22
_exptl_absorpt_coefficient_mu    2.525
_exptl_absorpt_correction_T_max  0.7723
_exptl_absorpt_correction_T_min  0.6381
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'CrystalClear (Rigaku, 2005)'
_exptl_crystal_density_diffrn    2.282
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             346
_exptl_crystal_size_max          0.20
_exptl_crystal_size_mid          0.15
_exptl_crystal_size_min          0.10
_refine_diff_density_max         1.539
_refine_diff_density_min         -0.788
_refine_diff_density_rms         0.162
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.120
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     167
_refine_ls_number_reflns         1945
_refine_ls_number_restraints     2
_refine_ls_restrained_S_all      1.121
_refine_ls_R_factor_all          0.1027
_refine_ls_R_factor_gt           0.0698
_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)+(0.0527P)²+1.5465P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1361
_refine_ls_wR_factor_ref         0.1455
_reflns_number_gt                1453
_reflns_number_total             1945
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c3ra43137a.txt
_cod_data_source_block           cu-4
_cod_original_sg_symbol_H-M      ' P -1'
_cod_database_code               7239161
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 -0.27038(18) 0.43948(10) -0.00896(9) 0.0173(3) Uani 1 1 d .
P1 P 0.0805(4) 0.5607(2) 0.27673(19) 0.0144(5) Uani 1 1 d .
P2 P -0.0664(4) 0.7566(2) 0.07254(19) 0.0147(4) Uani 1 1 d .
O1 O -0.1680(9) 0.4561(5) 0.1976(5) 0.0168(11) Uani 1 1 d .
O2 O 0.3052(9) 0.5550(5) 0.2118(5) 0.0157(11) Uani 1 1 d .
O3 O 0.1540(10) 0.5434(5) 0.4321(5) 0.0195(12) Uani 1 1 d .
O4 O -0.3110(9) 0.6382(5) 0.0109(5) 0.0166(12) Uani 1 1 d .
O5 O 0.1620(9) 0.7356(5) 0.0179(5) 0.0173(12) Uani 1 1 d .
O6 O -0.1185(10) 0.9011(5) 0.0545(5) 0.0201(12) Uani 1 1 d D
H6C H -0.1562 0.9101 -0.0326 0.030 Uiso 1 1 d RD
O7 O -0.1965(10) 0.7477(6) 0.3206(5) 0.0210(12) Uani 1 1 d .
H7 H -0.3264 0.6901 0.2757 0.032 Uiso 1 1 calc R
N1 N 0.4568(15) 1.2614(7) 0.2747(7) 0.0277(17) Uani 1 1 d D
C1 C 0.3127(14) 0.9897(8) 0.3204(7) 0.0170(16) Uani 1 1 d .
C2 C 0.2094(15) 1.0943(8) 0.3740(8) 0.0222(18) Uani 1 1 d .
H2 H 0.0877 1.0710 0.4257 0.027 Uiso 1 1 calc R
C3 C 0.2862(17) 1.2279(8) 0.3508(8) 0.0265(19) Uani 1 1 d .
H3 H 0.2199 1.2974 0.3880 0.032 Uiso 1 1 calc R
C4 C 0.5583(17) 1.1670(9) 0.2191(9) 0.030(2) Uani 1 1 d .
H4 H 0.6756 1.1944 0.1658 0.036 Uiso 1 1 calc R
C5 C 0.4905(16) 1.0309(9) 0.2404(8) 0.0252(19) Uani 1 1 d .
H5 H 0.5619 0.9646 0.2020 0.030 Uiso 1 1 calc R
C6 C 0.2539(14) 0.8423(7) 0.3544(7) 0.0166(17) Uani 1 1 d .
H6A H 0.2360 0.8461 0.4504 0.020 Uiso 1 1 calc R
H6B H 0.4023 0.8046 0.3527 0.020 Uiso 1 1 calc R
C7 C 0.0156(13) 0.7364(7) 0.2612(7) 0.0130(16) Uani 1 1 d .
H1A H 0.502(14) 1.346(3) 0.260(8) 0.020 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'
Cu Cu 0.3201 1.2651 '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'
H H 0.0000 0.0000 '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 O1 89.2(2) 2_565 .
O5 Cu1 O2 91.4(2) 2_565 2_565
O1 Cu1 O2 168.9(2) . 2_565
O5 Cu1 O4 169.1(2) 2_565 .
O1 Cu1 O4 87.8(2) . .
O2 Cu1 O4 89.6(2) 2_565 .
O5 Cu1 O4 101.45(19) 2_565 2_465
O1 Cu1 O4 91.39(19) . 2_465
O2 Cu1 O4 99.36(19) 2_565 2_465
O4 Cu1 O4 89.08(19) . 2_465
O5 Cu1 Cu1 82.52(15) 2_565 2_565
O1 Cu1 Cu1 85.95(15) . 2_565
O2 Cu1 Cu1 83.13(15) 2_565 2_565
O4 Cu1 Cu1 86.83(15) . 2_565
O4 Cu1 Cu1 175.21(14) 2_465 2_565
O5 Cu1 Cu1 142.65(15) 2_565 2_465
O1 Cu1 Cu1 89.59(15) . 2_465
O2 Cu1 Cu1 96.64(15) 2_565 2_465
O4 Cu1 Cu1 47.81(14) . 2_465
O4 Cu1 Cu1 41.27(13) 2_465 2_465
Cu1 Cu1 Cu1 134.59(7) 2_565 2_465
O3 P1 O1 112.3(3) . .
O3 P1 O2 109.9(3) . .
O1 P1 O2 113.0(3) . .
O3 P1 C7 108.4(3) . .
O1 P1 C7 105.6(3) . .
O2 P1 C7 107.3(3) . .
O6 P2 O5 112.6(3) . .
O6 P2 O4 111.5(3) . .
O5 P2 O4 113.0(3) . .
O6 P2 C7 109.7(3) . .
O5 P2 C7 106.0(3) . .
O4 P2 C7 103.6(3) . .
P1 O1 Cu1 119.1(3) . .
P1 O2 Cu1 121.0(3) . 2_565
P2 O4 Cu1 117.7(3) . .
P2 O4 Cu1 144.5(3) . 2_465
Cu1 O4 Cu1 90.92(19) . 2_465
P2 O5 Cu1 124.6(3) . 2_565
P2 O6 H6C 109.5 . .
C7 O7 H7 109.5 . .
C4 N1 C3 122.7(7) . .
C4 N1 H1A 118(5) . .
C3 N1 H1A 119(5) . .
C5 C1 C2 117.2(7) . .
C5 C1 C6 120.3(7) . .
C2 C1 C6 122.3(7) . .
C3 C2 C1 120.0(7) . .
C3 C2 H2 120.0 . .
C1 C2 H2 120.0 . .
N1 C3 C2 120.2(8) . .
N1 C3 H3 119.9 . .
C2 C3 H3 119.9 . .
N1 C4 C5 119.7(8) . .
N1 C4 H4 120.1 . .
C5 C4 H4 120.1 . .
C4 C5 C1 120.1(8) . .
C4 C5 H5 119.9 . .
C1 C5 H5 119.9 . .
C1 C6 C7 118.6(6) . .
C1 C6 H6A 107.7 . .
C7 C6 H6A 107.7 . .
C1 C6 H6B 107.7 . .
C7 C6 H6B 107.7 . .
H6A C6 H6B 107.1 . .
O7 C7 C6 106.6(6) . .
O7 C7 P2 109.8(5) . .
C6 C7 P2 116.6(5) . .
O7 C7 P1 109.8(4) . .
C6 C7 P1 106.2(5) . .
P2 C7 P1 107.7(4) . .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
Cu1 O5 1.941(5) 2_565
Cu1 O1 1.966(5) .
Cu1 O2 1.967(5) 2_565
Cu1 O4 2.013(5) .
Cu1 O4 2.261(5) 2_465
Cu1 Cu1 2.917(2) 2_565
Cu1 Cu1 3.051(2) 2_465
P1 O3 1.521(5) .
P1 O1 1.525(5) .
P1 O2 1.526(5) .
P1 C7 1.846(7) .
P2 O6 1.522(5) .
P2 O5 1.522(5) .
P2 O4 1.543(5) .
P2 C7 1.844(7) .
O2 Cu1 1.967(5) 2_565
O4 Cu1 2.261(5) 2_465
O5 Cu1 1.941(5) 2_565
O6 H6C 0.8500 .
O7 C7 1.440(8) .
O7 H7 0.8200 .
N1 C4 1.327(11) .
N1 C3 1.331(10) .
N1 H1A 0.85(2) .
C1 C5 1.403(10) .
C1 C2 1.403(10) .
C1 C6 1.493(10) .
C2 C3 1.342(11) .
C2 H2 0.9300 .
C3 H3 0.9300 .
C4 C5 1.353(11) .
C4 H4 0.9300 .
C5 H5 0.9300 .
C6 C7 1.539(10) .
C6 H6A 0.9700 .
C6 H6B 0.9700 .
