#------------------------------------------------------------------------------
#$Date: 2016-03-23 00:50:43 +0200 (Wed, 23 Mar 2016) $
#$Revision: 179131 $
#$URL: svn://www.crystallography.net/cod/cif/4/30/93/4309347.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_4309347
loop_
_publ_author_name
'Sebastian Bauer'
'Thomas Bein'
'Norbert Stock'
_publ_contact_author_address
;
Christian-Albrechts-Universität zu Kiel
Institut für Anorganische Chemie
Otto-Hahn Platz 6/7
24118 Kiel
Germany
;
_publ_contact_author_email       stock@ac.uni-kiel.de
_publ_contact_author_fax         +49-(0)431-880-1520
_publ_contact_author_name        'Norbert Stock'
_publ_contact_author_phone       +49-(0)431-880-1675
_publ_section_title
;
High-Throughput Investigation and Characterization of Cobalt Carboxy
Phosphonates
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              5882
_journal_page_last               5889
_journal_paper_doi               10.1021/ic0505089
_journal_volume                  44
_journal_year                    2005
_chemical_formula_sum            'C10 H12 Co N O7 P'
_chemical_formula_weight         348.11
_chemical_name_systematic
; 
 ? 
;
_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                92.555(10)
_cell_angle_beta                 96.132(10)
_cell_angle_gamma                107.771(9)
_cell_formula_units_Z            2
_cell_length_a                   5.3903(4)
_cell_length_b                   5.4687(4)
_cell_length_c                   21.1156(18)
_cell_measurement_reflns_used    4591
_cell_measurement_temperature    200(2)
_cell_measurement_theta_max      28.0
_cell_measurement_theta_min      2.9
_cell_volume                     587.39(9)
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      200(2)
_diffrn_measured_fraction_theta_full 0.923
_diffrn_measured_fraction_theta_max 0.923
_diffrn_measurement_device_type  STOE-IPDS
_diffrn_measurement_method       'area detection'
_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  0.0474
_diffrn_reflns_av_sigmaI/netI    0.0601
_diffrn_reflns_limit_h_max       7
_diffrn_reflns_limit_h_min       -7
_diffrn_reflns_limit_k_max       6
_diffrn_reflns_limit_k_min       -7
_diffrn_reflns_limit_l_max       27
_diffrn_reflns_limit_l_min       -27
_diffrn_reflns_number            5444
_diffrn_reflns_theta_full        27.99
_diffrn_reflns_theta_max         27.99
_diffrn_reflns_theta_min         2.92
_exptl_absorpt_coefficient_mu    1.631
_exptl_absorpt_correction_T_max  0.9820
_exptl_absorpt_correction_T_min  0.9026
_exptl_absorpt_correction_type   numerical
_exptl_absorpt_process_details
; 
 Absorption correction with XRed, rev 1.09, STOE (Darmstadt, Germany) 
;
_exptl_crystal_colour            pink
_exptl_crystal_density_diffrn    1.968
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       platelet
_exptl_crystal_F_000             354
_exptl_crystal_size_max          0.20
_exptl_crystal_size_mid          0.08
_exptl_crystal_size_min          0.03
_refine_diff_density_max         0.812
_refine_diff_density_min         -1.020
_refine_diff_density_rms         0.107
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.953
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     190
_refine_ls_number_reflns         2615
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      0.952
_refine_ls_R_factor_all          0.0464
_refine_ls_R_factor_gt           0.0338
_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)+(0.0484P)²+0.0000P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0817
_refine_ls_wR_factor_ref         0.0855
_reflns_number_gt                2068
_reflns_number_total             2615
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic0505089si20050609_083347.cif
_cod_data_source_block           '[Co(O3PCH2)(OCH)N-CH2C6H4-COOH]_H2O'
_cod_original_cell_volume        587.39(8)
_cod_database_code               4309347
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 0.64523(7) 0.69338(7) 0.560503(18) 0.00509(11) Uani 1 1 d . . .
P1 P 0.73613(13) 0.90967(12) 0.42294(3) 0.00447(15) Uani 1 1 d . . .
O1 O 1.0304(4) 0.9825(3) 0.42167(9) 0.0078(4) Uani 1 1 d . . .
O2 O 0.6445(4) 1.1338(3) 0.44303(9) 0.0073(4) Uani 1 1 d . . .
O3 O 0.6393(4) 0.6730(3) 0.46070(9) 0.0065(4) Uani 1 1 d . . .
O4 O 0.3786(4) 0.3039(4) 0.33392(10) 0.0140(4) Uani 1 1 d . . .
O5 O 0.3621(6) 1.2155(6) 0.03338(14) 0.0383(7) Uani 1 1 d . . .
O6 O 0.7753(6) 1.4796(6) 0.04692(14) 0.0384(7) Uani 1 1 d D . .
H6 H 0.741(10) 1.575(8) 0.0193(18) 0.046 Uiso 1 1 d D . .
O7 O 0.9101(4) 0.4945(4) 0.57711(11) 0.0121(4) Uani 1 1 d . . .
H71 H 1.062(8) 0.578(7) 0.5704(18) 0.015 Uiso 1 1 d . . .
H72 H 0.892(7) 0.329(7) 0.5657(17) 0.015 Uiso 1 1 d . . .
N1 N 0.6741(5) 0.6319(4) 0.30552(11) 0.0082(5) Uani 1 1 d . . .
C1 C 0.5783(6) 0.8124(5) 0.34090(13) 0.0083(5) Uani 1 1 d . . .
H1B H 0.3912 0.7348 0.3418 0.010 Uiso 1 1 calc R . .
H1A H 0.6022 0.9658 0.3178 0.010 Uiso 1 1 calc R . .
C2 C 0.5663(5) 0.3844(5) 0.30163(12) 0.0043(5) Uani 1 1 d . . .
H2A H 0.6238 0.2734 0.2766 0.005 Uiso 1 1 calc R . .
C3 C 0.8891(6) 0.7304(6) 0.26719(14) 0.0129(6) Uani 1 1 d . . .
H3B H 0.9448 0.5885 0.2516 0.016 Uiso 1 1 calc R . .
H3A H 1.0373 0.8509 0.2940 0.016 Uiso 1 1 calc R . .
C4 C 0.8088(6) 0.8636(6) 0.21107(14) 0.0143(6) Uani 1 1 d . . .
C5 C 0.5574(7) 0.7799(7) 0.17806(17) 0.0241(8) Uani 1 1 d . . .
H5A H 0.4346 0.6340 0.1897 0.029 Uiso 1 1 calc R . .
C6 C 0.4859(7) 0.9115(7) 0.12749(17) 0.0245(7) Uani 1 1 d . . .
H6A H 0.3165 0.8547 0.1058 0.029 Uiso 1 1 calc R . .
C7 C 0.6711(7) 1.1284(6) 0.11007(15) 0.0198(7) Uani 1 1 d . . .
C8 C 0.9244(7) 1.2064(7) 0.14141(17) 0.0245(8) Uani 1 1 d . . .
H8A H 1.0497 1.3479 0.1287 0.029 Uiso 1 1 calc R . .
C9 C 0.9934(7) 1.0750(6) 0.19173(16) 0.0211(7) Uani 1 1 d . . .
H9A H 1.1643 1.1291 0.2125 0.025 Uiso 1 1 calc R . .
C10 C 0.5955(7) 1.2824(7) 0.05961(16) 0.0235(8) 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
_geom_angle_publ_flag
O7 Co1 O2 170.56(8) . 2_676 ?
O7 Co1 O1 84.90(8) . 2_776 ?
O2 Co1 O1 99.19(8) 2_676 2_776 ?
O7 Co1 O3 95.36(8) . . ?
O2 Co1 O3 92.73(7) 2_676 . ?
O1 Co1 O3 95.38(8) 2_776 . ?
O7 Co1 O3 85.62(8) . 2_666 ?
O2 Co1 O3 90.69(8) 2_676 2_666 ?
O1 Co1 O3 169.94(7) 2_776 2_666 ?
O3 Co1 O3 82.15(8) . 2_666 ?
O7 Co1 O4 86.20(8) . 2_666 ?
O2 Co1 O4 85.41(8) 2_676 2_666 ?
O1 Co1 O4 88.57(8) 2_776 2_666 ?
O3 Co1 O4 175.85(8) . 2_666 ?
O3 Co1 O4 94.16(8) 2_666 2_666 ?
O2 P1 O1 113.59(11) . . ?
O2 P1 O3 113.97(10) . . ?
O1 P1 O3 110.83(10) . . ?
O2 P1 C1 104.16(11) . . ?
O1 P1 C1 107.50(12) . . ?
O3 P1 C1 106.07(12) . . ?
P1 O1 Co1 138.34(11) . 2_776 ?
P1 O2 Co1 149.39(13) . 2_676 ?
P1 O3 Co1 123.58(11) . . ?
P1 O3 Co1 134.29(12) . 2_666 ?
Co1 O3 Co1 97.85(7) . 2_666 ?
C2 O4 Co1 132.9(2) . 2_666 ?
C2 N1 C1 123.6(2) . . ?
C2 N1 C3 116.6(2) . . ?
C1 N1 C3 119.6(2) . . ?
N1 C1 P1 115.37(19) . . ?
O4 C2 N1 115.6(2) . . ?
N1 C3 C4 111.9(2) . . ?
C9 C4 C5 119.1(3) . . ?
C9 C4 C3 118.8(3) . . ?
C5 C4 C3 122.1(3) . . ?
C4 C5 C6 121.0(3) . . ?
C7 C6 C5 119.2(4) . . ?
C8 C7 C6 119.8(3) . . ?
C8 C7 C10 119.8(3) . . ?
C6 C7 C10 120.3(3) . . ?
C7 C8 C9 120.5(3) . . ?
C4 C9 C8 120.3(3) . . ?
O5 C10 O6 124.3(3) . . ?
O5 C10 C7 119.2(3) . . ?
O6 C10 C7 116.5(3) . . ?
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 O7 2.054(2) . ?
Co1 O2 2.0545(18) 2_676 ?
Co1 O1 2.061(2) 2_776 ?
Co1 O3 2.1017(19) . ?
Co1 O3 2.113(2) 2_666 ?
Co1 O4 2.246(2) 2_666 ?
P1 O2 1.5145(18) . ?
P1 O1 1.5166(19) . ?
P1 O3 1.5335(18) . ?
P1 C1 1.826(3) . ?
O1 Co1 2.061(2) 2_776 ?
O2 Co1 2.0545(18) 2_676 ?
O3 Co1 2.1131(19) 2_666 ?
O4 C2 1.259(3) . ?
O4 Co1 2.246(2) 2_666 ?
O5 C10 1.255(5) . ?
O6 C10 1.272(4) . ?
N1 C2 1.295(3) . ?
N1 C1 1.458(3) . ?
N1 C3 1.465(3) . ?
C3 C4 1.511(4) . ?
C4 C9 1.385(4) . ?
C4 C5 1.387(5) . ?
C5 C6 1.399(5) . ?
C6 C7 1.390(5) . ?
C7 C8 1.382(5) . ?
C7 C10 1.486(4) . ?
C8 C9 1.389(5) . ?
loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
O2 P1 O1 Co1 -0.2(2) . . . 2_776 ?
O3 P1 O1 Co1 -130.01(16) . . . 2_776 ?
C1 P1 O1 Co1 114.49(18) . . . 2_776 ?
O1 P1 O2 Co1 151.9(2) . . . 2_676 ?
O3 P1 O2 Co1 -79.9(2) . . . 2_676 ?
C1 P1 O2 Co1 35.3(3) . . . 2_676 ?
O2 P1 O3 Co1 -44.55(17) . . . . ?
O1 P1 O3 Co1 85.07(14) . . . . ?
C1 P1 O3 Co1 -158.54(13) . . . . ?
O2 P1 O3 Co1 106.67(16) . . . 2_666 ?
O1 P1 O3 Co1 -123.71(15) . . . 2_666 ?
C1 P1 O3 Co1 -7.32(18) . . . 2_666 ?
O7 Co1 O3 P1 -115.55(14) . . . . ?
O2 Co1 O3 P1 69.32(14) 2_676 . . . ?
O1 Co1 O3 P1 -30.18(14) 2_776 . . . ?
O3 Co1 O3 P1 159.64(17) 2_666 . . . ?
O4 Co1 O3 P1 132.5(9) 2_666 . . . ?
O7 Co1 O3 Co1 84.81(8) . . . 2_666 ?
O2 Co1 O3 Co1 -90.32(8) 2_676 . . 2_666 ?
O1 Co1 O3 Co1 170.18(7) 2_776 . . 2_666 ?
O3 Co1 O3 Co1 0.0 2_666 . . 2_666 ?
O4 Co1 O3 Co1 -27.2(10) 2_666 . . 2_666 ?
C2 N1 C1 P1 94.1(3) . . . . ?
C3 N1 C1 P1 -91.5(3) . . . . ?
O2 P1 C1 N1 168.39(19) . . . . ?
O1 P1 C1 N1 47.6(2) . . . . ?
O3 P1 C1 N1 -71.0(2) . . . . ?
Co1 O4 C2 N1 -66.6(3) 2_666 . . . ?
C1 N1 C2 O4 -4.1(4) . . . . ?
C3 N1 C2 O4 -178.7(2) . . . . ?
C2 N1 C3 C4 108.2(3) . . . . ?
C1 N1 C3 C4 -66.6(3) . . . . ?
N1 C3 C4 C9 145.3(3) . . . . ?
N1 C3 C4 C5 -35.3(4) . . . . ?
C9 C4 C5 C6 -2.5(5) . . . . ?
C3 C4 C5 C6 178.0(3) . . . . ?
C4 C5 C6 C7 0.4(5) . . . . ?
C5 C6 C7 C8 2.0(5) . . . . ?
C5 C6 C7 C10 -175.7(3) . . . . ?
C6 C7 C8 C9 -2.2(5) . . . . ?
C10 C7 C8 C9 175.5(3) . . . . ?
C5 C4 C9 C8 2.3(5) . . . . ?
C3 C4 C9 C8 -178.3(3) . . . . ?
C7 C8 C9 C4 0.1(5) . . . . ?
C8 C7 C10 O5 -177.0(3) . . . . ?
C6 C7 C10 O5 0.6(5) . . . . ?
C8 C7 C10 O6 1.5(5) . . . . ?
C6 C7 C10 O6 179.2(3) . . . . ?
