#------------------------------------------------------------------------------
#$Date: 2016-03-26 22:45:49 +0200 (Sat, 26 Mar 2016) $
#$Revision: 180517 $
#$URL: svn://www.crystallography.net/cod/cif/7/21/86/7218633.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_7218633
loop_
_publ_author_name
'Videnova-Adrabinska, Veneta Georgieva'
'Wilk, Magdalena'
'Jarzembska, Katarzyna Natalia'
'Janczak, Jan'
'Duczmal, Marek'
'Hoffmann, Józef'
_publ_section_title
;
 Synthesis, structural characterization and computational studies of
 layered metal phosphonates: [M(HO3P--C5H4N--PO3H)2(H2O)2]n [MII= Co, Zn,
 Cd]
;
_journal_name_full               'RSC Adv.'
_journal_paper_doi               10.1039/C4RA10257F
_journal_year                    2014
_chemical_formula_moiety         'C10 H16 Co N2 O14 P4'
_chemical_formula_sum            'C10 H16 Co N2 O14 P4'
_chemical_formula_weight         571.06
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 95.980(10)
_cell_angle_gamma                90.00
_cell_formula_units_Z            2
_cell_length_a                   9.151(2)
_cell_length_b                   8.6680(10)
_cell_length_c                   11.631(2)
_cell_measurement_reflns_used    1773
_cell_measurement_temperature    295(2)
_cell_measurement_theta_max      29.35
_cell_measurement_theta_min      2.70
_cell_volume                     917.6(3)
_computing_cell_refinement
;
Oxford Diffraction Poland (2006). CrysAlis Red, Version 171.32.6
;
_computing_data_collection
;
Oxford Diffraction Poland (2006). CrysAlis CCD, Version 171.32.6
;
_computing_data_reduction
;
Oxford Diffraction Poland (2006). CrysAlis Red, Version 171.32.6
;
_computing_molecular_graphics
;
Brandenburg & Putz (2006). Diamond 3.0. Crystal and Molecular
Structure Visualisation, University of Bonn, Germany
;
_computing_publication_material  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      295(2)
_diffrn_detector_area_resol_mean '1024x1024 with blocks 2x2'
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.939
_diffrn_measurement_device_type  'KUMA KM-4 with area CCD detector'
_diffrn_measurement_method       ω-scan
_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  0.0284
_diffrn_reflns_av_sigmaI/netI    0.0294
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_limit_l_min       -10
_diffrn_reflns_number            12177
_diffrn_reflns_theta_full        28.00
_diffrn_reflns_theta_max         29.35
_diffrn_reflns_theta_min         2.70
_exptl_absorpt_coefficient_mu    1.366
_exptl_absorpt_correction_T_max  0.7988
_exptl_absorpt_correction_T_min  0.7722
_exptl_absorpt_correction_type   numerical
_exptl_absorpt_process_details
;
Oxford Diffraction Poland (2006). CrysAlis Red, Version 171.32.6
;
_exptl_crystal_colour            pink
_exptl_crystal_density_diffrn    2.067
_exptl_crystal_density_meas      2.06
_exptl_crystal_density_method    floatation
_exptl_crystal_description       parallelepiped
_exptl_crystal_F_000             578
_exptl_crystal_preparation       'Magnetic properties'
_exptl_crystal_size_max          0.25
_exptl_crystal_size_mid          0.21
_exptl_crystal_size_min          0.18
_refine_diff_density_max         0.359
_refine_diff_density_min         -0.361
_refine_diff_density_rms         0.069
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.006
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     157
_refine_ls_number_reflns         2364
_refine_ls_number_restraints     4
_refine_ls_restrained_S_all      1.006
_refine_ls_R_factor_all          0.0485
_refine_ls_R_factor_gt           0.0258
_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)+(0.0360P)²+0.0000P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0552
_refine_ls_wR_factor_ref         0.0611
_reflns_number_gt                1773
_reflns_number_total             2364
_reflns_threshold_expression     I>2σ(I)
_cod_data_source_file            c4ra10257f2.cif
_cod_data_source_block           compound_1
_cod_original_sg_symbol_H-M      'P 21/n'
_cod_database_code               7218633
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x+1/2, y+1/2, -z+1/2'
'-x, -y, -z'
'x-1/2, -y-1/2, z-1/2'
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
Co Co 0.0000 0.0000 0.0000 0.01531(9) Uani 1 2 d S
N1 N 0.55838(16) -0.27391(17) 0.03769(12) 0.0212(3) Uani 1 1 d .
H1N H 0.579(2) -0.278(2) 0.1074(17) 0.025 Uiso 1 1 d .
C2 C 0.44272(19) -0.1903(2) -0.00648(14) 0.0191(4) Uani 1 1 d .
H2 H 0.3897 -0.1318 0.0418 0.023 Uiso 1 1 calc R
C3 C 0.40285(16) -0.19155(18) -0.12454(14) 0.0152(3) Uani 1 1 d .
C4 C 0.48545(17) -0.28050(17) -0.19384(14) 0.0152(3) Uani 1 1 d .
H4 H 0.4612 -0.2810 -0.2735 0.018 Uiso 1 1 calc R
C5 C 0.60383(17) -0.36872(18) -0.14588(14) 0.0170(3) Uani 1 1 d .
C6 C 0.63835(19) -0.3606(2) -0.02692(14) 0.0217(4) Uani 1 1 d .
H6 H 0.7179 -0.4162 0.0080 0.026 Uiso 1 1 calc R
P3 P 0.23809(4) -0.09417(5) -0.18547(4) 0.01406(10) Uani 1 1 d .
O31 O 0.18550(12) 0.00823(12) -0.09570(10) 0.0195(3) Uani 1 1 d .
O32 O 0.13642(12) -0.22024(12) -0.23514(9) 0.0190(3) Uani 1 1 d .
O33 O 0.28572(13) -0.00417(13) -0.29231(10) 0.0200(3) Uani 1 1 d D
H33 H 0.307(2) 0.0854(13) -0.2751(16) 0.030 Uiso 1 1 d D
P5 P 0.71432(4) -0.48951(5) -0.23095(4) 0.01483(10) Uani 1 1 d .
O51 O 0.63791(14) -0.50555(14) -0.34933(10) 0.0256(3) Uani 1 1 d .
O52 O 0.74953(13) -0.63428(13) -0.16327(10) 0.0240(3) Uani 1 1 d .
O53 O 0.86044(13) -0.39258(14) -0.23211(11) 0.0259(3) Uani 1 1 d D
H53 H 0.847(2) -0.3053(14) -0.2565(17) 0.039 Uiso 1 1 d D
O1W O 0.01061(15) -0.25023(16) 0.00494(11) 0.0275(3) Uani 1 1 d D
H1W H 0.0832(16) -0.293(2) 0.0407(17) 0.041 Uiso 1 1 d D
H2W H 0.009(2) -0.290(2) -0.0593(11) 0.041 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'
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
O51 Co O51 180.00(4) 4_556 2_554
O51 Co O31 90.41(5) 4_556 3
O51 Co O31 89.59(5) 2_554 3
O51 Co O31 89.59(5) 4_556 .
O51 Co O31 90.41(5) 2_554 .
O31 Co O31 180.00(8) 3 .
O51 Co O1W 91.21(5) 4_556 3
O51 Co O1W 88.79(5) 2_554 3
O31 Co O1W 90.65(5) 3 3
O31 Co O1W 89.35(5) . 3
O51 Co O1W 88.80(5) 4_556 .
O51 Co O1W 91.20(5) 2_554 .
O31 Co O1W 89.35(5) 3 .
O31 Co O1W 90.65(5) . .
O1W Co O1W 180.00(7) 3 .
C6 N1 C2 123.13(15) . .
C6 N1 H1N 116.9(14) . .
C2 N1 H1N 119.9(14) . .
N1 C2 C3 119.48(16) . .
N1 C2 H2 120.3 . .
C3 C2 H2 120.3 . .
C2 C3 C4 118.40(15) . .
C2 C3 P3 120.56(13) . .
C4 C3 P3 120.81(12) . .
C3 C4 C5 121.18(15) . .
C3 C4 H4 119.4 . .
C5 C4 H4 119.4 . .
C6 C5 C4 117.24(15) . .
C6 C5 P5 119.31(12) . .
C4 C5 P5 123.44(12) . .
N1 C6 C5 120.56(15) . .
N1 C6 H6 119.7 . .
C5 C6 H6 119.7 . .
O31 P3 O32 117.94(7) . .
O31 P3 O33 113.36(7) . .
O32 P3 O33 105.55(6) . .
O31 P3 C3 108.73(7) . .
O32 P3 C3 105.52(7) . .
O33 P3 C3 104.71(7) . .
P3 O31 Co 132.97(7) . .
P3 O33 H33 110.9(14) . .
O51 P5 O52 117.62(7) . .
O51 P5 O53 111.05(7) . .
O52 P5 O53 108.29(7) . .
O51 P5 C5 108.89(7) . .
O52 P5 C5 107.32(7) . .
O53 P5 C5 102.56(7) . .
P5 O51 Co 168.23(8) . 2_544
P5 O53 H53 113.4(16) . .
Co O1W H1W 119.4(15) . .
Co O1W H2W 113.3(16) . .
H1W O1W H2W 102(2) . .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
Co O51 2.0507(12) 4_556
Co O51 2.0507(12) 2_554
Co O31 2.1258(12) 3
Co O31 2.1258(12) .
Co O1W 2.1717(14) 3
Co O1W 2.1717(14) .
N1 C6 1.334(2) .
N1 C2 1.340(2) .
N1 H1N 0.815(19) .
C2 C3 1.384(2) .
C2 H2 0.9300 .
C3 C4 1.394(2) .
C3 P3 1.8070(16) .
C4 C5 1.394(2) .
C4 H4 0.9300 .
C5 C6 1.389(2) .
C5 P5 1.8182(17) .
C6 H6 0.9300 .
P3 O31 1.4881(12) .
P3 O32 1.5105(11) .
P3 O33 1.5671(12) .
O33 H33 0.819(9) .
P5 O51 1.4843(12) .
P5 O52 1.4984(12) .
P5 O53 1.5805(13) .
O51 Co 2.0507(12) 2_544
O53 H53 0.813(9) .
O1W H1W 0.834(9) .
O1W H2W 0.821(9) .
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
N1 H1N O32 0.815(19) 1.851(19) 2.6648(19) 177(2) 4_656
O33 H33 O32 0.819(9) 1.764(10) 2.5728(16) 169(2) 2_554
O53 H53 O52 0.813(9) 1.916(12) 2.6929(17) 159(2) 2_654
O1W H1W O52 0.834(9) 2.078(11) 2.8929(18) 166(2) 3_645
O1W H2W O53 0.821(9) 2.474(14) 3.1973(19) 147(2) 1_455
O1W H2W O32 0.821(9) 2.528(17) 3.1400(18) 132.3(19) .
