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#$Date: 2019-03-05 10:52:05 +0200 (Tue, 05 Mar 2019) $
#$Revision: 213973 $
#$URL: file:///home/coder/svn-repositories/cod/cif/7/01/25/7012591.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_7012591
loop_
_publ_author_name
'Turner, Adele'
'Jaffrès, Paul-Alain'
'MacLean, Elizabeth J.'
'Villemin, Didier'
'McKee, Vickie'
'Hix, Gary B.'
_publ_section_title
;
 Hydrothermal synthesis and crystal structure of two Co phosphonates
 containing trifunctional phosphonate anions: Co3(O3PCH2NH2CH2PO3)2 and
 Co3(O3PCH2-NC4H7-CO2)2·5H2O
;
_journal_issue                   7
_journal_name_full               'Dalton Transactions'
_journal_page_first              1314
_journal_paper_doi               10.1039/b212266a
_journal_year                    2003
_chemical_formula_sum            'C12 H28 Co3 N2 O15 P2'
_chemical_formula_weight         679.02
_chemical_melting_point          decomposes
_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                90.238(5)
_cell_angle_beta                 106.810(5)
_cell_angle_gamma                111.346(4)
_cell_formula_units_Z            2
_cell_length_a                   9.985(2)
_cell_length_b                   10.378(3)
_cell_length_c                   11.942(3)
_cell_measurement_temperature    150(2)
_cell_volume                     1095.0(5)
_computing_molecular_graphics    'SHELXL-97 (Sheldrick, 1997)'
_computing_publication_material  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXL-97 (Sheldrick, 1997)'
_diffrn_ambient_temperature      0(2)
_diffrn_measured_fraction_theta_full 0.995
_diffrn_measured_fraction_theta_max 0.995
_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  0.0759
_diffrn_reflns_av_sigmaI/netI    0.1207
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       14
_diffrn_reflns_limit_l_min       -13
_diffrn_reflns_number            8099
_diffrn_reflns_theta_full        24.77
_diffrn_reflns_theta_max         24.77
_diffrn_reflns_theta_min         1.79
_exptl_absorpt_coefficient_mu    2.472
_exptl_absorpt_correction_T_max  0.7902
_exptl_absorpt_correction_T_min  0.7902
_exptl_absorpt_correction_type   multi-scan
_exptl_crystal_colour            purple
_exptl_crystal_density_diffrn    2.060
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             690
_exptl_crystal_size_max          0.05
_exptl_crystal_size_mid          0.05
_exptl_crystal_size_min          0.02
_refine_diff_density_max         0.820
_refine_diff_density_min         -0.644
_refine_diff_density_rms         0.146
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.924
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     307
_refine_ls_number_reflns         3736
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.924
_refine_ls_R_factor_all          0.0948
_refine_ls_R_factor_gt           0.0535
_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)+(0.0638P)²+0.0000P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1222
_refine_ls_wR_factor_ref         0.1384
_reflns_number_gt                2475
_reflns_number_total             3736
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            b212266a.txt
_cod_data_source_block           ejm48
_cod_original_sg_symbol_H-M      P-1
_cod_database_code               7012591
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
Co1 Co 0.02839(10) 0.58569(9) 0.88900(8) 0.0134(3) Uani 1 1 d . . .
Co2 Co 0.47778(11) 0.93956(10) 1.12339(9) 0.0171(3) Uani 1 1 d . . .
Co3 Co -0.10927(11) 0.84039(10) 0.98060(9) 0.0158(3) Uani 1 1 d . . .
P1 P -0.1435(2) 0.25761(18) 0.83656(17) 0.0142(4) Uani 1 1 d . . .
P2 P 0.1906(2) 0.92822(18) 0.88715(16) 0.0132(4) Uani 1 1 d . . .
O15 O 0.0846(5) 0.9631(5) 0.9421(4) 0.0171(11) Uani 1 1 d . . .
O7 O -0.1506(5) 0.6441(5) 0.8834(5) 0.0190(11) Uani 1 1 d . . .
O1 O 0.4364(6) 0.7455(6) 1.0314(6) 0.0442(17) Uani 1 1 d . . .
O9 O 0.3558(5) 0.9909(5) 0.9674(4) 0.0199(12) Uani 1 1 d . . .
O5 O -0.1031(5) 0.3813(5) 0.9289(4) 0.0166(11) Uani 1 1 d . . .
O6 O 0.2009(6) 0.5131(6) 0.8879(5) 0.0260(13) Uani 1 1 d . . .
O2 O -0.5271(6) 0.8689(6) 0.7895(5) 0.0300(13) Uani 1 1 d . . .
N2 N 0.3241(7) 1.0467(6) 0.7218(5) 0.0207(14) Uani 1 1 d . . .
N1 N -0.1176(6) 0.4868(6) 0.7139(5) 0.0151(13) Uani 1 1 d . . .
O14 O 0.1411(5) 0.7746(5) 0.8472(4) 0.0172(11) Uani 1 1 d . . .
O11 O 0.0310(6) 0.8125(5) 1.1336(4) 0.0232(12) Uani 1 1 d . . .
O12 O -0.3060(6) 0.1570(5) 0.8093(4) 0.0236(12) Uani 1 1 d . . .
O8 O -0.3991(6) 0.5252(6) 0.8310(6) 0.0414(16) Uani 1 1 d . . .
C6 C -0.1214(9) 0.3407(7) 0.7042(6) 0.0168(16) Uani 1 1 d . . .
H6A H -0.0264 0.3433 0.6923 0.020 Uiso 1 1 calc R . .
H6B H -0.2066 0.2845 0.6346 0.020 Uiso 1 1 calc R . .
C1 C -0.2746(8) 0.5560(8) 0.8140(7) 0.0226(18) Uani 1 1 d . . .
C3 C -0.0685(9) 0.5604(8) 0.6173(7) 0.0228(17) Uani 1 1 d . . .
H3A H -0.0997 0.4943 0.5460 0.027 Uiso 1 1 calc R . .
H3B H 0.0427 0.6112 0.6422 0.027 Uiso 1 1 calc R . .
C2 C -0.2707(8) 0.4880(8) 0.7027(7) 0.0237(18) Uani 1 1 d . . .
H2 H -0.3479 0.3903 0.6833 0.028 Uiso 1 1 calc R . .
C12 C -0.6204(10) 0.8353(9) 0.6845(8) 0.035(2) Uani 1 1 d . . .
O13 O -0.6486(9) 0.7304(7) 0.6175(6) 0.060(2) Uani 1 1 d . . .
C11 C 0.3539(10) 1.1717(9) 0.6554(8) 0.031(2) Uani 1 1 d . . .
H11A H 0.2594 1.1869 0.6178 0.037 Uiso 1 1 calc R . .
H11B H 0.4287 1.2568 0.7084 0.037 Uiso 1 1 calc R . .
C7 C 0.1942(8) 1.0293(8) 0.7646(6) 0.0189(16) Uani 1 1 d . . .
H7A H 0.0990 0.9828 0.6991 0.023 Uiso 1 1 calc R . .
H7B H 0.1985 1.1224 0.7890 0.023 Uiso 1 1 calc R . .
C4 C -0.1501(10) 0.6614(9) 0.5949(8) 0.037(2) Uani 1 1 d . . .
H4A H -0.0997 0.7429 0.6565 0.044 Uiso 1 1 calc R . .
H4B H -0.1550 0.6943 0.5167 0.044 Uiso 1 1 calc R . .
C5 C -0.3063(10) 0.5723(10) 0.6002(8) 0.037(2) Uani 1 1 d . . .
H5A H -0.3690 0.5103 0.5255 0.044 Uiso 1 1 calc R . .
H5B H -0.3592 0.6306 0.6171 0.044 Uiso 1 1 calc R . .
C10 C 0.4143(12) 1.1356(10) 0.5659(9) 0.049(3) Uani 1 1 d . . .
H10A H 0.5201 1.1435 0.6013 0.059 Uiso 1 1 calc R . .
H10B H 0.4093 1.1954 0.5016 0.059 Uiso 1 1 calc R . .
C8 C 0.2880(10) 0.9246(9) 0.6364(7) 0.032(2) Uani 1 1 d . . .
H8 H 0.1786 0.8646 0.6200 0.038 Uiso 1 1 calc R . .
C9 C 0.3073(14) 0.9848(11) 0.5220(8) 0.058(3) Uani 1 1 d . . .
H9A H 0.3522 0.9353 0.4822 0.069 Uiso 1 1 calc R . .
H9B H 0.2092 0.9792 0.4670 0.069 Uiso 1 1 calc R . .
O16 O -0.2320(6) 0.8858(5) 0.8188(5) 0.0252(12) Uani 1 1 d . . .
O17 O -0.3096(6) 0.7152(6) 1.0141(5) 0.0325(14) Uani 1 1 d . . .
O18 O 0.3036(7) 0.4902(7) 0.7123(6) 0.0435(16) 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'
Co Co 0.3494 0.9721 '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'
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
O14 Co1 O5 101.94(19) . 2_567 ?
O14 Co1 O7 89.98(19) . . ?
O5 Co1 O7 91.06(19) 2_567 . ?
O14 Co1 O6 92.7(2) . . ?
O5 Co1 O6 91.1(2) 2_567 . ?
O7 Co1 O6 176.1(2) . . ?
O14 Co1 N1 98.7(2) . . ?
O5 Co1 N1 158.0(2) 2_567 . ?
O7 Co1 N1 81.3(2) . . ?
O6 Co1 N1 95.5(2) . . ?
O14 Co1 O5 177.46(19) . . ?
O5 Co1 O5 79.7(2) 2_567 . ?
O7 Co1 O5 88.00(18) . . ?
O6 Co1 O5 89.27(19) . . ?
N1 Co1 O5 79.43(19) . . ?
O12 Co2 O2 92.5(2) 2_567 2_577 ?
O12 Co2 O9 99.5(2) 2_567 . ?
O2 Co2 O9 90.6(2) 2_577 . ?
O12 Co2 O1 90.1(2) 2_567 . ?
O2 Co2 O1 177.3(2) 2_577 . ?
O9 Co2 O1 89.5(2) . . ?
O12 Co2 O9 170.3(2) 2_567 2_677 ?
O2 Co2 O9 97.1(2) 2_577 2_677 ?
O9 Co2 O9 78.53(19) . 2_677 ?
O1 Co2 O9 80.3(2) . 2_677 ?
O12 Co2 N2 99.8(2) 2_567 2_677 ?
O2 Co2 N2 79.4(2) 2_577 2_677 ?
O9 Co2 N2 158.6(2) . 2_677 ?
O1 Co2 N2 99.6(2) . 2_677 ?
O9 Co2 N2 84.0(2) 2_677 2_677 ?
O11 Co3 O15 87.1(2) . . ?
O11 Co3 O17 94.5(2) . . ?
O15 Co3 O17 178.2(2) . . ?
O11 Co3 O16 173.5(2) . . ?
O15 Co3 O16 86.4(2) . . ?
O17 Co3 O16 92.0(2) . . ?
O11 Co3 O15 91.22(19) . 2_577 ?
O15 Co3 O15 82.04(19) . 2_577 ?
O17 Co3 O15 98.5(2) . 2_577 ?
O16 Co3 O15 87.16(19) . 2_577 ?
O11 Co3 O7 95.3(2) . . ?
O15 Co3 O7 98.08(18) . . ?
O17 Co3 O7 81.2(2) . . ?
O16 Co3 O7 86.37(19) . . ?
O15 Co3 O7 173.51(19) 2_577 . ?
O11 P1 O12 113.4(3) 2_567 . ?
O11 P1 O5 112.8(3) 2_567 . ?
O12 P1 O5 112.2(3) . . ?
O11 P1 C6 105.8(3) 2_567 . ?
O12 P1 C6 108.4(3) . . ?
O5 P1 C6 103.4(3) . . ?
O14 P2 O15 114.4(3) . . ?
O14 P2 O9 111.7(3) . . ?
O15 P2 O9 111.6(3) . . ?
O14 P2 C7 111.3(3) . . ?
O15 P2 C7 104.1(3) . . ?
O9 P2 C7 102.7(3) . . ?
P2 O15 Co3 132.8(3) . . ?
P2 O15 Co3 129.0(3) . 2_577 ?
Co3 O15 Co3 97.96(18) . 2_577 ?
C1 O7 Co1 110.9(4) . . ?
C1 O7 Co3 129.0(4) . . ?
Co1 O7 Co3 120.0(2) . . ?
P2 O9 Co2 134.2(3) . . ?
P2 O9 Co2 115.1(3) . 2_677 ?
Co2 O9 Co2 101.47(19) . 2_677 ?
P1 O5 Co1 134.5(3) . 2_567 ?
P1 O5 Co1 115.1(3) . . ?
Co1 O5 Co1 100.34(19) 2_567 . ?
C12 O2 Co2 118.2(5) . 2_577 ?
C7 N2 C8 110.6(6) . . ?
C7 N2 C11 109.4(6) . . ?
C8 N2 C11 106.3(6) . . ?
C7 N2 Co2 108.4(4) . 2_677 ?
C8 N2 Co2 108.5(5) . 2_677 ?
C11 N2 Co2 113.7(5) . 2_677 ?
C3 N1 C2 107.0(6) . . ?
C3 N1 C6 110.0(5) . . ?
C2 N1 C6 111.9(5) . . ?
C3 N1 Co1 114.1(4) . . ?
C2 N1 Co1 107.0(4) . . ?
C6 N1 Co1 106.9(4) . . ?
P2 O14 Co1 140.2(3) . . ?
P1 O11 Co3 135.1(3) 2_567 . ?
P1 O12 Co2 145.6(3) . 2_567 ?
N1 C6 P1 111.6(5) . . ?
O8 C1 O7 123.6(7) . . ?
O8 C1 C2 118.1(7) . . ?
O7 C1 C2 118.3(6) . . ?
N1 C3 C4 103.2(6) . . ?
N1 C2 C1 112.4(6) . . ?
N1 C2 C5 106.4(6) . . ?
C1 C2 C5 109.2(6) . . ?
O13 C12 O2 125.1(8) . . ?
O13 C12 C8 115.4(8) . 1_455 ?
O2 C12 C8 119.4(7) . 1_455 ?
C10 C11 N2 103.8(7) . . ?
N2 C7 P2 113.0(5) . . ?
C5 C4 C3 102.4(7) . . ?
C4 C5 C2 102.5(6) . . ?
C11 C10 C9 101.6(8) . . ?
N2 C8 C12 113.0(7) . 1_655 ?
N2 C8 C9 105.5(7) . . ?
C12 C8 C9 115.4(8) 1_655 . ?
C10 C9 C8 102.7(8) . . ?
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
Co1 O14 2.021(5) . ?
Co1 O5 2.067(5) 2_567 ?
Co1 O7 2.070(5) . ?
Co1 O6 2.119(5) . ?
Co1 N1 2.163(6) . ?
Co1 O5 2.189(5) . ?
Co2 O12 2.036(5) 2_567 ?
Co2 O2 2.062(5) 2_577 ?
Co2 O9 2.099(5) . ?
Co2 O1 2.133(6) . ?
Co2 O9 2.152(5) 2_677 ?
Co2 N2 2.243(6) 2_677 ?
Co3 O11 2.050(5) . ?
Co3 O15 2.075(5) . ?
Co3 O17 2.103(5) . ?
Co3 O16 2.125(5) . ?
Co3 O15 2.135(5) 2_577 ?
Co3 O7 2.182(5) . ?
P1 O11 1.511(5) 2_567 ?
P1 O12 1.512(5) . ?
P1 O5 1.543(5) . ?
P1 C6 1.834(7) . ?
P2 O14 1.516(5) . ?
P2 O15 1.536(5) . ?
P2 O9 1.537(5) . ?
P2 C7 1.805(7) . ?
O15 Co3 2.135(5) 2_577 ?
O7 C1 1.278(9) . ?
O9 Co2 2.152(5) 2_677 ?
O5 Co1 2.067(5) 2_567 ?
O2 C12 1.283(10) . ?
O2 Co2 2.062(5) 2_577 ?
N2 C7 1.480(9) . ?
N2 C8 1.491(10) . ?
N2 C11 1.505(9) . ?
N2 Co2 2.243(6) 2_677 ?
N1 C3 1.489(9) . ?
N1 C2 1.500(9) . ?
N1 C6 1.506(8) . ?
O11 P1 1.511(5) 2_567 ?
O12 Co2 2.036(5) 2_567 ?
O8 C1 1.244(9) . ?
C1 C2 1.519(11) . ?
C3 C4 1.527(11) . ?
C2 C5 1.541(11) . ?
C12 O13 1.242(10) . ?
C12 C8 1.531(12) 1_455 ?
C11 C10 1.477(12) . ?
C4 C5 1.517(12) . ?
C10 C9 1.522(14) . ?
C8 C12 1.531(12) 1_655 ?
C8 C9 1.538(12) . ?
