2-Pyridylmethylphosphonic acid: a flexible, multi-dentate ligand for metal phosphonates
Zavras, Athanasios; Fry, Julie A.; Beavers, Christine M.; Talbo, Gert H.; Richards, Anne F.; CrystEngComm 13 (2011) 3551–; doi:10.1039/c0ce00969e

data_7205882
_publ_section_title
;
 2-Pyridylmethylphosphonic acid: a flexible, multi-dentate ligand for
 metal phosphonates
;
_journal_issue                   10
_journal_name_full               CrystEngComm
_journal_page_first              3551
_journal_paper_doi               10.1039/c0ce00969e
_journal_volume                  13
_journal_year                    2011
_chemical_formula_moiety         'C24 H52 Fe4 N4 O24 P4, Cl, 7(ClO4),(H2O)'
_chemical_formula_sum            'C24 H54 Cl8 Fe4 N4 O53 P4'
_chemical_formula_weight         1877.59
_chemical_name_common            (Fe4(PyHCH2PO3)4(H2O)12(Cl)(ClO4)7xH2O)
_chemical_name_systematic
;
?
;
_space_group_IT_number           13
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2yac'
_symmetry_space_group_name_H-M   'P 1 2/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                 92.526(6)
_cell_angle_gamma                90.00
_cell_formula_units_Z            2
_cell_length_a                   11.051(3)
_cell_length_b                   14.563(4)
_cell_length_c                   20.651(6)
_cell_measurement_reflns_used    6557
_cell_measurement_temperature    213(2)
_cell_measurement_theta_max      29.2322
_cell_measurement_theta_min      2.4166
_cell_volume                     3320.3(16)
_computing_cell_refinement       'CrysAlisPro, V. 171.34.40'
_computing_data_collection       'CrysAlisPro, V. 1.171.34.40'
_computing_data_reduction        'CrysAlisPro, V. 1.171.34.40'
_computing_molecular_graphics    'SHELXTL 5.1, XP (Sheldrick, 1994)'
_computing_publication_material  SHELXL-97
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      213(2)
_diffrn_detector_area_resol_mean 10.3281
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.867
_diffrn_measurement_device_type  'Oxford Gemini'
_diffrn_measurement_method       \w
_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  0.0316
_diffrn_reflns_av_sigmaI/netI    0.0489
_diffrn_reflns_limit_h_max       7
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       27
_diffrn_reflns_limit_l_min       -27
_diffrn_reflns_number            19115
_diffrn_reflns_theta_full        26.25
_diffrn_reflns_theta_max         29.15
_diffrn_reflns_theta_min         2.42
_exptl_absorpt_coefficient_mu    1.393
_exptl_absorpt_correction_T_max  0.9862
_exptl_absorpt_correction_T_min  0.9727
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS: SAINT+, 2001'
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.878
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             1900
_exptl_crystal_size_max          0.02
_exptl_crystal_size_mid          0.02
_exptl_crystal_size_min          0.01
_refine_diff_density_max         1.418
_refine_diff_density_min         -1.050
_refine_diff_density_rms         0.136
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.996
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     684
_refine_ls_number_reflns         7772
_refine_ls_number_restraints     2215
_refine_ls_restrained_S_all      1.082
_refine_ls_R_factor_all          0.0971
_refine_ls_R_factor_gt           0.0666
_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^)+(0.1088P)^2^+14.1672P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1756
_refine_ls_wR_factor_ref         0.2009
_reflns_number_gt                5667
_reflns_number_total             7772
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            c0ce00969e.txt
_cod_data_source_block           3cb2
_cod_original_cell_volume        3320.4(17)
_cod_original_sg_symbol_H-M      'P 2/n'
_cod_original_formula_sum        'C24 H54 Cl8 Fe4 N4 O53 P4 '
_cod_database_code               7205882