#------------------------------------------------------------------------------
#$Date: 2019-11-28 20:47:44 +0200 (Thu, 28 Nov 2019) $
#$Revision: 244576 $
#$URL: file:///home/coder/svn-repositories/cod/cif/7/23/91/7239160.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_7239160
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         'C16 H18 Cu3 N2 O18 P4'
_chemical_formula_sum            'C16 H18 Cu3 N2 O18 P4'
_chemical_formula_weight         840.82
_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                109.44(3)
_cell_angle_beta                 99.01(3)
_cell_angle_gamma                110.06(3)
_cell_formula_units_Z            1
_cell_length_a                   8.6015(17)
_cell_length_b                   8.9334(18)
_cell_length_c                   9.6326(19)
_cell_measurement_temperature    293(2)
_cell_volume                     624.3(3)
_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 0.997
_diffrn_measured_fraction_theta_max 0.997
_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  0.0484
_diffrn_reflns_av_sigmaI/netI    0.0620
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_l_max       12
_diffrn_reflns_limit_l_min       -12
_diffrn_reflns_number            6538
_diffrn_reflns_theta_full        27.48
_diffrn_reflns_theta_max         27.48
_diffrn_reflns_theta_min         3.50
_exptl_absorpt_coefficient_mu    2.883
_exptl_absorpt_correction_T_max  0.56
_exptl_absorpt_correction_T_min  0.489
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'CrystalClear (Rigaku, 2005)'
_exptl_crystal_density_diffrn    2.236
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             419
_exptl_crystal_size_max          0.25
_exptl_crystal_size_mid          0.22
_exptl_crystal_size_min          0.20
_refine_diff_density_max         1.041
_refine_diff_density_min         -0.557
_refine_diff_density_rms         0.121
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.001
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     205
_refine_ls_number_reflns         2854
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.001
_refine_ls_R_factor_all          0.0641
_refine_ls_R_factor_gt           0.0448
_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)+(0.0453P)²+1.1085P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0963
_refine_ls_wR_factor_ref         0.1042
_reflns_number_gt                2269
_reflns_number_total             2854
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c3ra43137a.txt
_cod_data_source_block           cu-2
_cod_database_code               7239160
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
H2A H 0.124(7) -0.475(7) 0.640(7) 0.049(19) Uiso 1 1 d .
C8 C 0.5521(6) 0.2918(6) 0.9735(5) 0.0251(10) Uani 1 1 d .
H8 H 0.4994 0.2802 1.0488 0.030 Uiso 1 1 calc R
C7 C 0.6767(6) 0.4524(6) 0.9990(5) 0.0294(11) Uani 1 1 d .
H7 H 0.7084 0.5491 1.0916 0.035 Uiso 1 1 calc R
C6 C 0.7131(6) 0.3337(6) 0.7586(6) 0.0339(12) Uani 1 1 d .
H6 H 0.7680 0.3489 0.6853 0.041 Uiso 1 1 calc R
C5 C 0.5922(6) 0.1718(6) 0.7308(5) 0.0307(11) Uani 1 1 d .
H5 H 0.5683 0.0764 0.6396 0.037 Uiso 1 1 calc R
O9 O 0.5584(4) 0.5129(4) 0.3381(3) 0.0222(7) Uani 1 1 d .
O4 O -0.0913(4) -0.0162(4) 0.6271(3) 0.0186(6) Uani 1 1 d .
O1 O -0.1180(4) -0.3854(4) 0.5557(3) 0.0207(6) Uani 1 1 d .
Cu1 Cu 0.0000 0.0000 1.0000 0.01593(18) Uani 1 2 d S
Cu2 Cu 0.26198(6) 0.24830(6) 0.51962(6) 0.01796(15) Uani 1 1 d .
P1 P 0.03431(14) -0.28624(13) 0.70282(12) 0.0162(2) Uani 1 1 d .
P2 P 0.09728(13) 0.07171(13) 0.72973(12) 0.0150(2) Uani 1 1 d .
O5 O 0.2073(4) 0.2212(3) 0.6971(3) 0.0198(6) Uani 1 1 d .
O6 O 0.1140(4) 0.1377(4) 0.9007(3) 0.0201(6) Uani 1 1 d .
O3 O -0.0094(4) -0.2238(4) 0.8523(3) 0.0223(7) Uani 1 1 d .
O2 O 0.1304(4) -0.4032(4) 0.7174(4) 0.0235(7) Uani 1 1 d .
O8 O 0.3936(4) 0.2798(4) 0.3702(3) 0.0235(7) Uani 1 1 d .
O7 O 0.2123(4) -0.1414(4) 0.5403(3) 0.0228(7) Uani 1 1 d .
H7A H 0.1564 -0.1103 0.4878 0.034 Uiso 1 1 calc R
C2 C 0.1895(5) -0.0922(5) 0.6908(4) 0.0161(8) Uani 1 1 d .
C1 C 0.4853(5) 0.4396(5) 0.4151(5) 0.0189(9) Uani 1 1 d .
N1 N 0.7517(5) 0.4690(5) 0.8908(5) 0.0293(9) Uani 1 1 d D
C4 C 0.5051(5) 0.1476(6) 0.8359(5) 0.0206(9) Uani 1 1 d .
C3 C 0.3685(5) -0.0278(5) 0.8092(5) 0.0217(9) Uani 1 1 d .
H3A H 0.3504 -0.0218 0.9075 0.026 Uiso 1 1 calc R
H3B H 0.4134 -0.1150 0.7745 0.026 Uiso 1 1 calc R
H1A H 0.810(5) 0.572(3) 0.906(5) 0.023(13) 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'
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
C7 C8 C4 120.2(4) . .
C7 C8 H8 119.9 . .
C4 C8 H8 119.9 . .
N1 C7 C8 119.8(4) . .
N1 C7 H7 120.1 . .
C8 C7 H7 120.1 . .
N1 C6 C5 119.6(4) . .
N1 C6 H6 120.2 . .
C5 C6 H6 120.2 . .
C6 C5 C4 121.0(4) . .
C6 C5 H5 119.5 . .
C4 C5 H5 119.5 . .
C1 O9 Cu2 109.2(3) . 2_666
P2 O4 Cu2 138.55(18) . 2_556
P1 O1 Cu2 120.00(16) . 2_556
O6 Cu1 O6 180.000(1) 2_557 .
O6 Cu1 O3 94.78(12) 2_557 2_557
O6 Cu1 O3 85.22(12) . 2_557
O6 Cu1 O3 85.22(12) 2_557 .
O6 Cu1 O3 94.78(12) . .
O3 Cu1 O3 180.000(1) 2_557 .
O5 Cu2 O4 95.03(12) . 2_556
O5 Cu2 O9 87.64(12) . 2_666
O4 Cu2 O9 177.28(11) 2_556 2_666
O5 Cu2 O8 160.80(13) . .
O4 Cu2 O8 93.05(12) 2_556 .
O9 Cu2 O8 84.24(12) 2_666 .
O5 Cu2 O1 108.42(12) . 2_556
O4 Cu2 O1 94.34(11) 2_556 2_556
O9 Cu2 O1 85.32(12) 2_666 2_556
O8 Cu2 O1 88.26(12) . 2_556
O1 P1 O3 115.95(17) . .
O1 P1 O2 110.07(17) . .
O3 P1 O2 106.81(18) . .
O1 P1 C2 108.40(18) . .
O3 P1 C2 107.69(17) . .
O2 P1 C2 107.62(18) . .
O5 P2 O6 109.34(17) . .
O5 P2 O4 111.66(17) . .
O6 P2 O4 112.66(17) . .
O5 P2 C2 108.00(17) . .
O6 P2 C2 105.98(18) . .
O4 P2 C2 108.94(18) . .
P2 O5 Cu2 135.91(17) . .
P2 O6 Cu1 125.64(17) . .
P1 O3 Cu1 137.07(18) . .
P1 O2 H2A 117(4) . .
C1 O8 Cu2 108.4(3) . .
C2 O7 H7A 109.5 . .
O7 C2 C3 107.1(3) . .
O7 C2 P1 109.4(3) . .
C3 C2 P1 108.2(3) . .
O7 C2 P2 111.9(3) . .
C3 C2 P2 113.4(3) . .
P1 C2 P2 106.7(2) . .
O9 C1 O8 126.7(4) . .
O9 C1 C1 116.3(4) . 2_666
O8 C1 C1 117.0(4) . 2_666
C7 N1 C6 122.0(4) . .
C7 N1 H1A 115(3) . .
C6 N1 H1A 122(3) . .
C8 C4 C5 117.2(4) . .
C8 C4 C3 119.8(4) . .
C5 C4 C3 123.0(4) . .
C4 C3 C2 116.1(4) . .
C4 C3 H3A 108.3 . .
C2 C3 H3A 108.3 . .
C4 C3 H3B 108.3 . .
C2 C3 H3B 108.3 . .
H3A C3 H3B 107.4 . .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
C8 C7 1.377(6) .
C8 C4 1.384(6) .
C8 H8 0.9300 .
C7 N1 1.330(6) .
C7 H7 0.9300 .
C6 N1 1.327(6) .
C6 C5 1.367(6) .
C6 H6 0.9300 .
C5 C4 1.381(6) .
C5 H5 0.9300 .
O9 C1 1.250(5) .
O9 Cu2 1.987(3) 2_666
O4 P2 1.527(3) .
O4 Cu2 1.940(3) 2_556
O1 P1 1.515(3) .
O1 Cu2 2.217(3) 2_556
Cu1 O6 1.907(3) 2_557
Cu1 O6 1.907(3) .
Cu1 O3 1.997(3) 2_557
Cu1 O3 1.997(3) .
Cu2 O5 1.911(3) .
Cu2 O4 1.940(3) 2_556
Cu2 O9 1.987(3) 2_666
Cu2 O8 1.998(3) .
Cu2 O1 2.217(3) 2_556
P1 O3 1.518(3) .
P1 O2 1.565(3) .
P1 C2 1.843(4) .
P2 O5 1.511(3) .
P2 O6 1.517(3) .
P2 C2 1.854(4) .
O2 H2A 0.79(6) .
O8 C1 1.248(5) .
O7 C2 1.434(5) .
O7 H7A 0.8200 .
C2 C3 1.551(6) .
C1 C1 1.553(8) 2_666
N1 H1A 0.830(19) .
C4 C3 1.509(6) .
C3 H3A 0.9700 .
C3 H3B 0.9700 .
