#------------------------------------------------------------------------------
#$Date: 2019-11-28 20:47:44 +0200 (Thu, 28 Nov 2019) $
#$Revision: 244576 $
#$URL: file:///home/coder/svn-repositories/cod/cif/7/23/91/7239156.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_7239156
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 H20 Co3 N2 O20 P4'
_chemical_formula_sum            'C16 H20 Co3 N2 O20 P4'
_chemical_formula_weight         861.01
_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                98.89(3)
_cell_angle_beta                 108.72(3)
_cell_angle_gamma                110.34(3)
_cell_formula_units_Z            1
_cell_length_a                   8.8776(18)
_cell_length_b                   8.9196(18)
_cell_length_c                   9.984(2)
_cell_measurement_temperature    293(2)
_cell_volume                     669.8(4)
_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  0.0639
_diffrn_reflns_av_sigmaI/netI    0.0786
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       10
_diffrn_reflns_limit_k_min       -10
_diffrn_reflns_limit_l_max       11
_diffrn_reflns_limit_l_min       -11
_diffrn_reflns_number            5637
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         25.00
_diffrn_reflns_theta_min         3.40
_exptl_absorpt_coefficient_mu    2.173
_exptl_absorpt_correction_T_max  0.8120
_exptl_absorpt_correction_T_min  0.6126
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'CrystalClear (Rigaku, 2005)'
_exptl_crystal_density_diffrn    2.134
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             431
_exptl_crystal_size_max          0.25
_exptl_crystal_size_mid          0.15
_exptl_crystal_size_min          0.10
_refine_diff_density_max         0.619
_refine_diff_density_min         -0.493
_refine_diff_density_rms         0.114
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.096
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     209
_refine_ls_number_reflns         2346
_refine_ls_number_restraints     3
_refine_ls_restrained_S_all      1.097
_refine_ls_R_factor_all          0.0872
_refine_ls_R_factor_gt           0.0586
_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)+(0.0322P)²+1.2965P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0966
_refine_ls_wR_factor_ref         0.1042
_reflns_number_gt                1797
_reflns_number_total             2346
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c3ra43137a.txt
_cod_data_source_block           Co-3
_cod_original_cell_volume        669.8(2)
_cod_database_code               7239156
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
O10 O 0.5164(5) -0.0720(5) 0.6545(4) 0.0264(10) Uani 1 1 d .
O6 O 1.2305(5) 0.7177(5) 0.7003(4) 0.0187(9) Uani 1 1 d .
O2 O 0.7614(5) 0.4742(5) 0.8358(4) 0.0210(10) Uani 1 1 d .
Co1 Co 1.0000 0.5000 1.0000 0.0155(3) Uani 1 2 d S
Co2 Co 0.74823(10) 0.26425(10) 0.48424(9) 0.0178(2) Uani 1 1 d .
P1 P 0.71355(19) 0.52994(19) 0.69900(16) 0.0151(4) Uani 1 1 d .
P2 P 1.08333(18) 0.60419(19) 0.73368(16) 0.0144(4) Uani 1 1 d .
O5 O 0.9956(5) 0.4248(4) 0.6310(4) 0.0171(9) Uani 1 1 d .
O4 O 1.1487(5) 0.6158(5) 0.8970(4) 0.0184(9) Uani 1 1 d .
O9 O 0.7280(5) 0.1017(5) 0.6044(4) 0.0229(10) Uani 1 1 d .
O7 O 0.8667(6) 0.7090(6) 0.5489(5) 0.0294(11) Uani 1 1 d .
H7 H 0.8935 0.6511 0.4972 0.044 Uiso 1 1 calc R
O3 O 0.6227(5) 0.3906(5) 0.5521(4) 0.0178(9) Uani 1 1 d .
O1 O 0.5913(5) 0.6169(6) 0.7090(4) 0.0220(11) Uani 1 1 d .
O8 O 1.0192(5) 0.7343(5) 1.1168(4) 0.0265(10) Uani 1 1 d D
H8A H 1.1120 0.7797 1.1964 0.040 Uiso 1 1 d RD
H8B H 0.9301 0.7168 1.1375 0.040 Uiso 1 1 d RD
C7 C 0.9135(7) 0.6855(7) 0.6957(6) 0.0174(13) Uani 1 1 d .
C4 C 1.2827(8) 1.0460(8) 0.9657(7) 0.0315(16) Uani 1 1 d .
H4 H 1.2669 1.0007 1.0407 0.038 Uiso 1 1 calc R
C6 C 0.9686(7) 0.8554(7) 0.8018(7) 0.0231(14) Uani 1 1 d .
H6A H 0.8793 0.8950 0.7635 0.028 Uiso 1 1 calc R
H6B H 0.9705 0.8399 0.8963 0.028 Uiso 1 1 calc R
C3 C 1.1445(8) 0.9909(7) 0.8294(7) 0.0208(14) Uani 1 1 d .
N1 N 1.4703(7) 1.2365(7) 0.8841(7) 0.0373(15) Uani 1 1 d .
C1 C 1.3361(10) 1.1880(9) 0.7520(8) 0.0392(18) Uani 1 1 d .
H1 H 1.3528 1.2375 0.6794 0.047 Uiso 1 1 calc R
C2 C 1.1750(8) 1.0661(8) 0.7236(7) 0.0303(16) Uani 1 1 d .
H2 H 1.0840 1.0330 0.6311 0.036 Uiso 1 1 calc R
C5 C 1.4457(9) 1.1692(9) 0.9915(8) 0.043(2) Uani 1 1 d .
H5 H 1.5385 1.2054 1.0836 0.051 Uiso 1 1 calc R
C8 C 0.5691(8) 0.0067(7) 0.5752(6) 0.0216(14) Uani 1 1 d .
H1A H 0.536(9) 0.616(9) 0.644(7) 0.032 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'
Co Co 0.3494 0.9721 '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
C8 O10 Co2 107.4(4) . 2_656
P2 O6 Co2 132.1(2) . 2_766
P1 O2 Co1 135.2(2) . .
O4 Co1 O4 180.000(1) 2_767 .
O4 Co1 O2 93.46(14) 2_767 2_767
O4 Co1 O2 86.54(14) . 2_767
O4 Co1 O2 86.54(14) 2_767 .
O4 Co1 O2 93.46(14) . .
O2 Co1 O2 180.000(1) 2_767 .
O4 Co1 O8 88.32(16) 2_767 .
O4 Co1 O8 91.68(16) . .
O2 Co1 O8 93.15(16) 2_767 .
O2 Co1 O8 86.85(16) . .
O4 Co1 O8 91.68(16) 2_767 2_767
O4 Co1 O8 88.32(15) . 2_767
O2 Co1 O8 86.85(16) 2_767 2_767
O2 Co1 O8 93.15(16) . 2_767
O8 Co1 O8 180.000(1) . 2_767
O6 Co2 O9 140.02(17) 2_766 .
O6 Co2 O3 115.48(16) 2_766 .
O9 Co2 O3 99.91(16) . .
O6 Co2 O5 100.12(15) 2_766 .
O9 Co2 O5 93.01(15) . .
O3 Co2 O5 97.06(16) . .
O6 Co2 O10 85.70(16) 2_766 2_656
O9 Co2 O10 79.68(15) . 2_656
O3 Co2 O10 84.27(16) . 2_656
O5 Co2 O10 172.69(15) . 2_656
O2 P1 O3 115.2(2) . .
O2 P1 O1 107.5(2) . .
O3 P1 O1 109.1(2) . .
O2 P1 C7 109.9(2) . .
O3 P1 C7 106.8(2) . .
O1 P1 C7 108.1(3) . .
O4 P2 O6 110.4(2) . .
O4 P2 O5 113.4(2) . .
O6 P2 O5 112.1(2) . .
O4 P2 C7 107.1(2) . .
O6 P2 C7 106.8(2) . .
O5 P2 C7 106.7(2) . .
P2 O5 Co2 135.7(2) . .
P2 O4 Co1 125.8(2) . .
C8 O9 Co2 112.6(4) . .
C7 O7 H7 109.5 . .
P1 O3 Co2 121.7(2) . .
P1 O1 H1A 116(6) . .
Co1 O8 H8A 109.5 . .
Co1 O8 H8B 109.5 . .
H8A O8 H8B 109.5 . .
O7 C7 C6 105.0(5) . .
O7 C7 P1 107.7(4) . .
C6 C7 P1 109.7(4) . .
O7 C7 P2 111.0(4) . .
C6 C7 P2 114.6(4) . .
P1 C7 P2 108.7(3) . .
C3 C4 C5 120.3(7) . .
C3 C4 H4 119.9 . .
C5 C4 H4 119.9 . .
C3 C6 C7 116.4(5) . .
C3 C6 H6A 108.2 . .
C7 C6 H6A 108.2 . .
C3 C6 H6B 108.2 . .
C7 C6 H6B 108.2 . .
H6A C6 H6B 107.3 . .
C4 C3 C2 117.1(6) . .
C4 C3 C6 119.9(6) . .
C2 C3 C6 123.0(6) . .
C1 N1 C5 120.1(6) . .
N1 C1 C2 120.4(7) . .
N1 C1 H1 119.8 . .
C2 C1 H1 119.8 . .
C1 C2 C3 121.5(6) . .
C1 C2 H2 119.2 . .
C3 C2 H2 119.2 . .
N1 C5 C4 120.5(6) . .
N1 C5 H5 119.7 . .
C4 C5 H5 119.7 . .
O10 C8 O9 126.3(5) . .
O10 C8 C8 118.3(7) . 2_656
O9 C8 C8 115.4(6) . 2_656
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
O10 C8 1.233(7) .
O10 Co2 2.181(4) 2_656
O6 P2 1.519(4) .
O6 Co2 1.936(4) 2_766
O2 P1 1.509(4) .
O2 Co1 2.131(4) .
Co1 O4 2.030(4) 2_767
Co1 O4 2.030(4) .
Co1 O2 2.131(4) 2_767
Co1 O8 2.152(4) .
Co1 O8 2.152(4) 2_767
Co2 O6 1.936(4) 2_766
Co2 O9 2.016(4) .
Co2 O3 2.024(4) .
Co2 O5 2.030(4) .
Co2 O10 2.181(4) 2_656
P1 O3 1.525(4) .
P1 O1 1.556(4) .
P1 C7 1.848(6) .
P2 O4 1.518(4) .
P2 O5 1.527(4) .
P2 C7 1.849(6) .
O9 C8 1.274(7) .
O7 C7 1.460(7) .
O7 H7 0.8200 .
O1 H1A 0.67(6) .
O8 H8A 0.8500 .
O8 H8B 0.8499 .
C7 C6 1.522(8) .
C4 C3 1.379(8) .
C4 C5 1.392(9) .
C4 H4 0.9300 .
C6 C3 1.511(8) .
C6 H6A 0.9700 .
C6 H6B 0.9700 .
C3 C2 1.384(8) .
N1 C1 1.342(9) .
N1 C5 1.347(9) .
C1 C2 1.368(9) .
C1 H1 0.9300 .
C2 H2 0.9300 .
C5 H5 0.9300 .
C8 C8 1.559(12) 2_656
