Crystal structure of poly[[di-μ~2~-aqua-aquasodium] 4-amino-3,5,6-trichloropyridine-2-carboxylate trihydrate], the sodium salt of the herbicide picloram
Smith, Graham; Acta Crystallographica Section E 71 (2015) 931–933; doi:10.1107/S2056989015012633

data_2240931
_publ_section_title
;
 Crystal structure of poly[[di-\m~2~-aqua-aquasodium]
 4-amino-3,5,6-trichloropyridine-2-carboxylate trihydrate], the sodium
 salt of the herbicide picloram
;
_journal_coeditor_code           WM5173
_journal_issue                   8
_journal_name_full               'Acta Crystallographica Section E'
_journal_page_first              931
_journal_page_last               933
_journal_paper_doi               10.1107/S2056989015012633
_journal_volume                  71
_journal_year                    2015
_chemical_formula_iupac          '[Na (H2 O)3] (C6 H2 Cl3 N2 O2), 3H2 O'
_chemical_formula_moiety         'C6 H2 Cl3 N2 O2 +, H6 Na O3 -, 3(H2 O)'
_chemical_formula_sum            'C6 H14 Cl3 N2 Na O8'
_chemical_formula_weight         371.53
_chemical_name_common            'sodium picloramate hexahydrate'
_chemical_name_systematic
;
Poly[[di-\m~2~-aqua-aquasodium]
4-amino-3,5,6-trichloropyridine-2-carboxylate trihydrate]
;
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                78.747(6)
_cell_angle_beta                 79.374(6)
_cell_angle_gamma                88.864(6)
_cell_formula_units_Z            2
_cell_length_a                   6.5625(5)
_cell_length_b                   8.4574(6)
_cell_length_c                   13.8553(10)
_cell_measurement_reflns_used    2548
_cell_measurement_temperature    200(2)
_cell_measurement_theta_max      28.8
_cell_measurement_theta_min      3.75
_cell_volume                     741.17(10)
_computing_cell_refinement
;
CrysAlis PRO (Agilent, 2014)
;
_computing_data_collection
;
CrysAlis PRO (Agilent, 2014)
;
_computing_data_reduction
;
CrysAlis PRO (Agilent, 2014)
;
_computing_molecular_graphics
;
PLATON (Spek, 2009)
;
_computing_publication_material
;
PLATON (Spek, 2009)
;
_computing_structure_refinement
;
SHELXL97 (Sheldrick, 2008) within WinGX (Farrugia, 2012)
;
_computing_structure_solution
;
SIR92 (Altomare <i>et al.</i>, 1993)
;
_diffrn_ambient_temperature      200(2)
_diffrn_detector_area_resol_mean 16.077
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measurement_device_type  'Oxford Diffraction Gemini-S CCD-detector'
_diffrn_measurement_method       '\w scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'Enhance (Mo) X-ray source'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0246
_diffrn_reflns_av_sigmaI/netI    0.0363
_diffrn_reflns_limit_h_max       7
_diffrn_reflns_limit_h_min       -8
_diffrn_reflns_limit_k_max       10
_diffrn_reflns_limit_k_min       -10
_diffrn_reflns_limit_l_max       13
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            6040
_diffrn_reflns_theta_full        26.00
_diffrn_reflns_theta_max         26.00
_diffrn_reflns_theta_min         3.25
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.682
_exptl_absorpt_correction_T_max  0.980
_exptl_absorpt_correction_T_min  0.947
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
(<i>CrysAlis PRO</i>; Agilent, 2014)
;
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.665
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             380
_exptl_crystal_size_max          0.35
_exptl_crystal_size_mid          0.35
_exptl_crystal_size_min          0.22
_refine_diff_density_max         0.299
_refine_diff_density_min         -0.280
_refine_ls_extinction_coef       0.050(3)
_refine_ls_extinction_method
;
SHELXL97 (Sheldrick, 2008) within WinGX (Farrugia, 2012)
;
_refine_ls_goodness_of_fit_ref   1.001
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     182
_refine_ls_number_reflns         2905
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.001
_refine_ls_R_factor_all          0.0394
_refine_ls_R_factor_gt           0.0306
_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^)+(0.0478P)^2^+0.2264P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0818
_refine_ls_wR_factor_ref         0.0879
_reflns_number_gt                2487
_reflns_number_total             2905
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            wm5173sup1.cf
_cod_data_source_block           I
_cod_original_cell_volume        741.17(9)
_cod_database_code               2240931
_cod_database_fobs_code 2240931