Design, synthesis and noncentrosymmetric solid state organization of three novel pyridylphosphonic acids
Zon, Jerzy; Videnova-Adrabinska, Veneta; Janczak, Jan; Wilk, Magdalena; Samoc, Anna; Gancarz, Roman; Samoc, Marek; CrystEngComm 13 (2011) 3474–; doi:10.1039/c1ce05140g

data_7215311
_publ_section_title
;
 Design, synthesis and noncentrosymmetric solid state organization of
 three novel pyridylphosphonic acids
;
_journal_issue                   10
_journal_name_full               CrystEngComm
_journal_page_first              3474
_journal_paper_doi               10.1039/c1ce05140g
_journal_volume                  13
_journal_year                    2011
_chemical_formula_moiety         'C6 H6 N O5 P'
_chemical_formula_sum            'C6 H6 N O5 P'
_chemical_formula_weight         203.09
_chemical_melting_point          581(3)
_chemical_name_systematic
;
5-(dihydroxyphosphoryl)nicotinic acid
;
_space_group_IT_number           43
_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_Hall  'F 2 -2d'
_symmetry_space_group_name_H-M   'F d d 2'
_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                 90.00
_cell_angle_gamma                90.00
_cell_formula_units_Z            16
_cell_length_a                   19.948(3)
_cell_length_b                   28.534(4)
_cell_length_c                   5.3040(10)
_cell_measurement_reflns_used    724
_cell_measurement_temperature    295(2)
_cell_measurement_theta_max      29.36
_cell_measurement_theta_min      3.51
_cell_volume                     3019.0(8)
_computing_cell_refinement
;
Oxford Diffraction Poland (2006). CrysAlis CCD,
Version 171.32.6, Wroc\/law, Poland
;
_computing_data_collection
;
Oxford Diffraction Poland (2006). CrysAlis CCD,
Version 171.32.6, Wroc\/law, Poland
;
_computing_data_reduction
;
Oxford Diffraction Poland (2006). CrysAlis CCD,
Version 171.32.6, Wroc\/law, Poland
;
_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 0.995
_diffrn_measured_fraction_theta_max 0.957
_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  0.0262
_diffrn_reflns_av_sigmaI/netI    0.0238
_diffrn_reflns_limit_h_max       26
_diffrn_reflns_limit_h_min       -26
_diffrn_reflns_limit_k_max       38
_diffrn_reflns_limit_k_min       -38
_diffrn_reflns_limit_l_max       7
_diffrn_reflns_limit_l_min       -4
_diffrn_reflns_number            9629
_diffrn_reflns_theta_full        28.50
_diffrn_reflns_theta_max         29.31
_diffrn_reflns_theta_min         2.49
_exptl_absorpt_coefficient_mu    0.352
_exptl_absorpt_correction_T_max  0.9491
_exptl_absorpt_correction_T_min  0.9210
_exptl_absorpt_correction_type   numerical
_exptl_absorpt_process_details
;
Oxford Diffraction Poland (2006). CrysAlis Red,
Version 171.32.6, Wroc\/law, Poland
;
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.787
_exptl_crystal_density_meas      1.79
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       paralellepiped
_exptl_crystal_F_000             1664
_exptl_crystal_size_max          0.27
_exptl_crystal_size_mid          0.16
_exptl_crystal_size_min          0.14
_refine_diff_density_max         0.248
_refine_diff_density_min         -0.192
_refine_diff_density_rms         0.045
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   -0.02(8)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.001
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     130
_refine_ls_number_reflns         1680
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.001
_refine_ls_R_factor_all          0.0301
_refine_ls_R_factor_gt           0.0249
_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^)+(0.0367P)^2^+0.9858P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0576
_refine_ls_wR_factor_ref         0.0592
_reflns_number_gt                1525
_reflns_number_total             1680
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c1ce05140g.txt
_cod_data_source_block           Compound_2
_cod_depositor_comments
;
The following automatic conversions were performed:

'_chemical_melting_point' value '305-310 C' was changed to '581(3)' -
it was converted from degrees Celsius(C) to Kelvins(K), the average
value was taken and precision was estimated.

Automatic conversion script
Id: cif_fix_values 2281 2013-09-26 08:29:07Z andrius 
;
_cod_database_code               7215311