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_7215310
_publ_section_title
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 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         'C5 H6 N O3 P'
_chemical_formula_sum            'C5 H6 N O3 P'
_chemical_formula_weight         159.08
_chemical_melting_point          524(2)
_space_group_IT_number           33
_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_Hall  'P 2c -2n'
_symmetry_space_group_name_H-M   'P n a 21'
_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            4
_cell_length_a                   7.5460(15)
_cell_length_b                   10.948(2)
_cell_length_c                   7.8040(16)
_cell_measurement_reflns_used    837
_cell_measurement_temperature    295(2)
_cell_measurement_theta_max      29.30
_cell_measurement_theta_min      3.21
_cell_volume                     644.7(2)
_computing_cell_refinement
;
Oxford Diffration Poland (2006). CrysAlis Red, Version 171.31.6;
Wroc\/law, Poland
;
_computing_data_collection
;
Oxford Diffration Poland (2006). CrysAlis CCD, Version 171.31.6;
Wroc\/law, Poland
;
_computing_data_reduction
;
Oxford Diffration Poland (2006). CrysAlis Red, Version 171.31.6;
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 bocks 2x2'
_diffrn_measured_fraction_theta_full 0.989
_diffrn_measured_fraction_theta_max 0.958
_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  0.0176
_diffrn_reflns_av_sigmaI/netI    0.0165
_diffrn_reflns_limit_h_max       8
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       10
_diffrn_reflns_limit_l_min       -10
_diffrn_reflns_number            8140
_diffrn_reflns_theta_full        28.80
_diffrn_reflns_theta_max         29.30
_diffrn_reflns_theta_min         3.21
_exptl_absorpt_coefficient_mu    0.365
_exptl_absorpt_correction_T_max  0.9302
_exptl_absorpt_correction_T_min  0.9181
_exptl_absorpt_correction_type   numerical
_exptl_absorpt_process_details
;
Oxford Diffration Poland (2006). CrysAlis Red, Version 171.31.6;
Wroc\/law, Poland
;
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.639
_exptl_crystal_density_meas      1.63
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       paralellepiped
_exptl_crystal_F_000             328
_exptl_crystal_size_max          0.26
_exptl_crystal_size_mid          0.24
_exptl_crystal_size_min          0.22
_refine_diff_density_max         0.162
_refine_diff_density_min         -0.174
_refine_diff_density_rms         0.034
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   0.12(7)
_refine_ls_extinction_coef       0.046(3)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     SHELXL
_refine_ls_goodness_of_fit_ref   0.955
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     98
_refine_ls_number_reflns         1643
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.955
_refine_ls_R_factor_all          0.0254
_refine_ls_R_factor_gt           0.0209
_refine_ls_shift/su_max          0.008
_refine_ls_shift/su_mean         0.001
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0380P)^2^+0.0168P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0516
_refine_ls_wR_factor_ref         0.0531
_reflns_number_gt                1466
_reflns_number_total             1643
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            c1ce05140g.txt
_cod_data_source_block           Compound_1
_cod_depositor_comments
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The following automatic conversions were performed:

'_chemical_melting_point' value '249-253 C' was changed to '524(2)' -
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 
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_cod_database_code               7215310