Synthesis, structural characterization and computational studies of layered metal phosphonates: [M(HO3P‒C5H4N‒PO3H)2(H2O)2]n [MII= Co, Zn, Cd]
Videnova-Adrabinska, Veneta Georgieva; Wilk, Magdalena; Jarzembska, Katarzyna Natalia; Janczak, Jan; Duczmal, Marek; Hoffmann, Józef; RSC Adv.  (2014) –; doi:10.1039/C4RA10257F

data_7218634
_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 N2 O14 P4 Zn'
_chemical_formula_sum            'C10 H16 N2 O14 P4 Zn'
_chemical_formula_weight         577.50
_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                 96.31(3)
_cell_angle_gamma                90.00
_cell_formula_units_Z            2
_cell_length_a                   9.1826(18)
_cell_length_b                   8.6841(17)
_cell_length_c                   11.656(2)
_cell_measurement_reflns_used    1966
_cell_measurement_temperature    295(2)
_cell_measurement_theta_max      29.20
_cell_measurement_theta_min      2.93
_cell_volume                     923.8(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 0.998
_diffrn_measured_fraction_theta_max 0.942
_diffrn_measurement_device_type  'KUMA KM-4 with area CCD detector'
_diffrn_measurement_method       \w-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  0.0247
_diffrn_reflns_av_sigmaI/netI    0.0219
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       10
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_number            12006
_diffrn_reflns_theta_full        28.00
_diffrn_reflns_theta_max         29.20
_diffrn_reflns_theta_min         2.93
_exptl_absorpt_coefficient_mu    1.758
_exptl_absorpt_correction_T_max  0.7816
_exptl_absorpt_correction_T_min  0.6488
_exptl_absorpt_correction_type   numerical
_exptl_absorpt_process_details
;
Oxford Diffraction Poland (2006). CrysAlis Red, Version 171.32.6
;
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    2.076
_exptl_crystal_density_meas      2.07
_exptl_crystal_density_method    floatation
_exptl_crystal_description       parallelepiped
_exptl_crystal_F_000             584
_exptl_crystal_size_max          0.28
_exptl_crystal_size_mid          0.18
_exptl_crystal_size_min          0.15
_refine_diff_density_max         0.437
_refine_diff_density_min         -0.325
_refine_diff_density_rms         0.068
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.002
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     154
_refine_ls_number_reflns         2357
_refine_ls_number_restraints     4
_refine_ls_restrained_S_all      1.001
_refine_ls_R_factor_all          0.0378
_refine_ls_R_factor_gt           0.0270
_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/[\s^2^(Fo^2^)+(0.0360P)^2^+0.7230P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0666
_refine_ls_wR_factor_ref         0.0701
_reflns_number_gt                1966
_reflns_number_total             2357
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            c4ra10257f2.cif
_cod_data_source_block           compound_2
_cod_original_sg_symbol_Hall     '-P 2yn '
_cod_original_sg_symbol_H-M      'P 21/n'
_cod_database_code               7218634