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#$Date: 2019-11-28 20:47:44 +0200 (Thu, 28 Nov 2019) $
#$Revision: 244576 $
#$URL: file:///home/coder/svn-repositories/cod/cif/7/23/91/7239158.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_7239158
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         'C8 H12 Co N O10 P2, H2 O'
_chemical_formula_sum            'C8 H14 Co N O11 P2'
_chemical_formula_weight         421.07
_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                93.03(3)
_cell_angle_beta                 107.48(3)
_cell_angle_gamma                110.72(3)
_cell_formula_units_Z            2
_cell_length_a                   7.2146(14)
_cell_length_b                   9.3580(19)
_cell_length_c                   11.945(2)
_cell_measurement_temperature    293(2)
_cell_volume                     707.9(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 0.999
_diffrn_measured_fraction_theta_max 0.999
_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  0.0711
_diffrn_reflns_av_sigmaI/netI    0.0897
_diffrn_reflns_limit_h_max       8
_diffrn_reflns_limit_h_min       -8
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_l_max       14
_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_number            6120
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         25.00
_diffrn_reflns_theta_min         3.10
_exptl_absorpt_coefficient_mu    1.499
_exptl_absorpt_correction_T_max  0.738
_exptl_absorpt_correction_T_min  0.639
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'CrystalClear (Rigaku, 2005)'
_exptl_crystal_density_diffrn    1.975
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             428
_exptl_crystal_size_max          0.3
_exptl_crystal_size_mid          0.25
_exptl_crystal_size_min          0.20
_refine_diff_density_max         0.538
_refine_diff_density_min         -0.568
_refine_diff_density_rms         0.147
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.088
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     230
_refine_ls_number_reflns         2495
_refine_ls_number_restraints     6
_refine_ls_restrained_S_all      1.088
_refine_ls_R_factor_all          0.0872
_refine_ls_R_factor_gt           0.0547
_refine_ls_shift/su_max          0.073
_refine_ls_shift/su_mean         0.003
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[σ²(Fo²)+(0.0696P)²+1.5500P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1287
_refine_ls_wR_factor_ref         0.1566
_reflns_number_gt                1784
_reflns_number_total             2495
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c3ra43137a.txt
_cod_data_source_block           co_2
_cod_database_code               7239158
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
Co1 Co 0.10495(14) 0.27295(10) -0.04085(8) 0.0173(3) Uani 1 1 d .
P1 P 0.2224(3) 0.0763(2) 0.17913(15) 0.0165(4) Uani 1 1 d .
P2 P -0.1344(3) 0.1928(2) 0.15694(15) 0.0180(4) Uani 1 1 d .
O1 O 0.2358(7) 0.1331(5) 0.0641(4) 0.0187(10) Uani 1 1 d .
O2 O 0.0932(7) -0.0912(5) 0.1711(4) 0.0229(11) Uani 1 1 d .
O3 O 0.4480(7) 0.1121(6) 0.2692(4) 0.0235(11) Uani 1 1 d .
H3A H 0.556(11) 0.161(8) 0.252(6) 0.028 Uiso 1 1 d .
O4 O -0.0865(7) 0.2736(5) 0.0562(4) 0.0200(10) Uani 1 1 d .
O5 O -0.2912(7) 0.0192(5) 0.1126(4) 0.0227(11) Uani 1 1 d D
H5A H -0.277(11) -0.023(8) 0.057(4) 0.027 Uiso 1 1 d D
O6 O -0.2200(7) 0.2705(5) 0.2304(4) 0.0216(11) Uani 1 1 d .
O7 O 0.2676(8) 0.3530(5) 0.2909(4) 0.0275(12) Uani 1 1 d .
H7 H 0.2915 0.3864 0.2324 0.041 Uiso 1 1 calc R
O8 O 0.3366(7) 0.4713(5) 0.0851(4) 0.0227(11) Uani 1 1 d .
O9 O 0.6532(7) 0.6567(5) 0.1172(4) 0.0242(11) Uani 1 1 d .
O10 O -0.0323(8) 0.4154(6) -0.1452(4) 0.0257(11) Uani 1 1 d D
H1OB H 0.023(12) 0.513(9) -0.110(7) 0.039 Uiso 1 1 d .
H10A H -0.157(5) 0.370(9) -0.163(7) 0.039 Uiso 1 1 d D
O1W O 0.4718(11) -0.2108(7) 0.2671(6) 0.0506(16) Uani 1 1 d D
H1WA H 0.511(16) -0.252(10) 0.221(7) 0.076 Uiso 1 1 d D
H1WB H 0.437(15) -0.132(8) 0.260(8) 0.076 Uiso 1 1 d D
N1 N 0.0423(14) 0.4035(11) 0.6383(7) 0.058(2) Uani 1 1 d D
H1A H 0.034(15) 0.454(10) 0.696(6) 0.069 Uiso 1 1 d D
C1 C 0.0750(11) 0.2302(8) 0.4619(6) 0.0256(16) Uani 1 1 d .
C2 C -0.1119(13) 0.1883(10) 0.4853(7) 0.037(2) Uani 1 1 d .
H2 H -0.2286 0.1007 0.4400 0.044 Uiso 1 1 calc R
C3 C -0.1233(14) 0.2769(12) 0.5760(8) 0.049(3) Uani 1 1 d .
H3 H -0.2471 0.2484 0.5938 0.059 Uiso 1 1 calc R
C4 C 0.2200(15) 0.4479(11) 0.6184(7) 0.048(2) Uani 1 1 d .
H4 H 0.3315 0.5386 0.6634 0.058 Uiso 1 1 calc R
C5 C 0.2440(13) 0.3614(9) 0.5308(7) 0.036(2) Uani 1 1 d .
H5 H 0.3725 0.3911 0.5182 0.044 Uiso 1 1 calc R
C6 C 0.1007(12) 0.1274(8) 0.3679(6) 0.0285(17) Uani 1 1 d .
H6A H 0.2262 0.1072 0.4050 0.034 Uiso 1 1 calc R
H6B H -0.0188 0.0286 0.3446 0.034 Uiso 1 1 calc R
C7 C 0.1178(10) 0.1927(8) 0.2549(6) 0.0194(15) Uani 1 1 d .
C8 C 0.4989(11) 0.5380(8) 0.0588(6) 0.0206(15) 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'
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
O2 Co1 O4 99.94(18) 2 .
O2 Co1 O8 173.59(18) 2 .
O4 Co1 O8 86.32(17) . .
O2 Co1 O1 92.48(18) 2 .
O4 Co1 O1 93.01(17) . .
O8 Co1 O1 88.55(18) . .
O2 Co1 O9 95.60(18) 2 2_665
O4 Co1 O9 162.86(18) . 2_665
O8 Co1 O9 78.01(17) . 2_665
O1 Co1 O9 93.49(18) . 2_665
O2 Co1 O10 87.79(19) 2 .
O4 Co1 O10 85.73(18) . .
O8 Co1 O10 91.32(19) . .
O1 Co1 O10 178.74(18) . .
O9 Co1 O10 87.70(19) 2_665 .
O2 P1 O1 117.8(3) . .
O2 P1 O3 107.3(3) . .
O1 P1 O3 110.4(3) . .
O2 P1 C7 107.6(3) . .
O1 P1 C7 109.0(3) . .
O3 P1 C7 104.0(3) . .
O6 P2 O4 114.5(3) . .
O6 P2 O5 107.7(3) . .
O4 P2 O5 112.7(3) . .
O6 P2 C7 108.4(3) . .
O4 P2 C7 106.1(3) . .
O5 P2 C7 107.0(3) . .
P1 O1 Co1 134.0(3) . .
P1 O2 Co1 136.7(3) . 2
P1 O3 H3A 121(5) . .
P2 O4 Co1 134.0(3) . .
P2 O5 H5A 113(5) . .
C7 O7 H7 109.5 . .
C8 O8 Co1 114.6(4) . .
C8 O9 Co1 113.7(4) . 2_665
Co1 O10 H1OB 113(5) . .
Co1 O10 H10A 105(6) . .
H1OB O10 H10A 118(8) . .
H1WA O1W H1WB 127(6) . .
C4 N1 C3 122.7(8) . .
C4 N1 H1A 119(7) . .
C3 N1 H1A 118(7) . .
C5 C1 C2 118.5(7) . .
C5 C1 C6 120.2(7) . .
C2 C1 C6 121.1(7) . .
C3 C2 C1 119.3(8) . .
C3 C2 H2 120.3 . .
C1 C2 H2 120.3 . .
N1 C3 C2 119.9(8) . .
N1 C3 H3 120.1 . .
C2 C3 H3 120.0 . .
N1 C4 C5 120.3(9) . .
N1 C4 H4 119.8 . .
C5 C4 H4 119.8 . .
C1 C5 C4 119.2(8) . .
C1 C5 H5 120.4 . .
C4 C5 H5 120.4 . .
C7 C6 C1 116.2(6) . .
C7 C6 H6A 108.2 . .
C1 C6 H6A 108.2 . .
C7 C6 H6B 108.2 . .
C1 C6 H6B 108.2 . .
H6A C6 H6B 107.4 . .
O7 C7 C6 108.0(5) . .
O7 C7 P2 107.3(4) . .
C6 C7 P2 112.7(5) . .
O7 C7 P1 109.4(4) . .
C6 C7 P1 106.8(4) . .
P2 C7 P1 112.5(3) . .
O9 C8 O8 126.4(6) . .
O9 C8 C8 118.1(8) . 2_665
O8 C8 C8 115.5(7) . 2_665
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
Co1 O2 2.005(5) 2
Co1 O4 2.054(4) .
Co1 O8 2.122(5) .
Co1 O1 2.124(4) .
Co1 O9 2.125(5) 2_665
Co1 O10 2.163(5) .
P1 O2 1.494(5) .
P1 O1 1.517(4) .
P1 O3 1.563(5) .
P1 C7 1.861(7) .
P2 O6 1.503(5) .
P2 O4 1.517(5) .
P2 O5 1.565(5) .
P2 C7 1.844(7) .
O2 Co1 2.005(5) 2
O3 H3A 0.84(7) .
O5 H5A 0.81(6) .
O7 C7 1.452(8) .
O7 H7 0.8200 .
O8 C8 1.259(8) .
O9 C8 1.240(8) .
O9 Co1 2.125(5) 2_665
O10 H1OB 0.88(8) .
O10 H10A 0.80(3) .
O1W H1WA 0.83(11) .
O1W H1WB 0.86(8) .
N1 C4 1.300(12) .
N1 C3 1.325(12) .
N1 H1A 0.84(8) .
C1 C5 1.379(10) .
C1 C2 1.384(10) .
C1 C6 1.535(10) .
C2 C3 1.369(12) .
C2 H2 0.9300 .
C3 H3 0.9300 .
C4 C5 1.378(11) .
C4 H4 0.9300 .
C5 H5 0.9300 .
C6 C7 1.532(9) .
C6 H6A 0.9700 .
C6 H6B 0.9700 .
C8 C8 1.547(13) 2_665
loop_
_geom_hbond_atom_site_label_D
_geom_hbond_atom_site_label_H
_geom_hbond_atom_site_label_A
_geom_hbond_distance_DH
_geom_hbond_distance_HA
_geom_hbond_distance_DA
_geom_hbond_angle_DHA
_geom_hbond_site_symmetry_A
O3 H3A O6 0.84(7) 1.68(8) 2.525(6) 175(7) 1_655
O5 H5A O1 0.81(6) 1.89(6) 2.690(6) 175(7) 2
O7 H7 O8 0.82 2.04 2.854(7) 177.0 .
O10 H10A O8 0.80(3) 2.59(8) 2.995(7) 113(7) 2_565
O10 H1OB O4 0.88(8) 1.91(8) 2.774(7) 168(7) 2_565
N1 H1A O10 0.84(8) 2.11(7) 2.799(9) 139(9) 1_556
N1 H1A O6 0.84(8) 2.42(8) 2.988(10) 126(8) 2_566
