Mixed 3,5-dinitrosalicylate(2‒) and partial 3,5-dinitrosalicylate(1‒) and picrate(1‒) species in tris(piperidinium) bis(3,5-dinitrosalicylate) picrate monohydrate
Graham Smith; Urs D. Wermuth; Peter C. Healy; Acta Crystallographica Section E 62 (2006) o610–o613; doi:10.1107/S1600536806000973

data_2208000
_publ_section_title
;
 Mixed 3,5-dinitrosalicylate(2--) and partial
 3,5-dinitrosalicylate(1--) and picrate(1--) species in
 tris(piperidinium) bis(3,5-dinitrosalicylate) picrate monohydrate
;
_journal_coeditor_code           CI6731
_journal_issue                   2
_journal_name_full               'Acta Crystallographica Section E'
_journal_page_first              o610
_journal_page_last               o613
_journal_paper_doi               10.1107/S1600536806000973
_journal_volume                  62
_journal_year                    2006
_chemical_formula_iupac
'3C5 H12 N + , C7 H2 N2 O7 2- , 0.79C7 H3 N2 O7 - , 0.21C6 H2 N3 O7 - , H2 O'
_chemical_formula_moiety
'3C5 H12 N + , C7 H2 N2 O7 2- , 0.79C7 H3 N2 O7 - , 0.21C6 H2 N3 O7 - , H2 O'
_chemical_formula_sum            'C28.79 H42.79 N7.21 O15'
_chemical_formula_weight         729.91
_chemical_melting_point          422(3)
_chemical_name_common
'tris(piperidinium) bis(3,5-dinitrosalicylate) picrate monohydrate'
_chemical_name_systematic
;
tris(piperidinium) bis(3,5-dinitrosalicylate)
picrate monohydrate
;
_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           'SHELXL97 (Sheldrick, 1997)'
_cell_angle_alpha                67.630(10)
_cell_angle_beta                 89.012(10)
_cell_angle_gamma                64.410(10)
_cell_formula_units_Z            2
_cell_length_a                   12.5457(15)
_cell_length_b                   12.903(2)
_cell_length_c                   13.1415(17)
_cell_measurement_reflns_used    17
_cell_measurement_temperature    297(2)
_cell_measurement_theta_max      16.3
_cell_measurement_theta_min      10.1
_cell_volume                     1746.4(5)
_computing_cell_refinement       'MSC/AFC Diffractometer Control Software'
_computing_data_collection
;
MSC/AFC Diffractometer Control Software (Molecular Structure
Corporation, 1999)
;
_computing_data_reduction
;
TEXSAN for Windows (Molecular Structure Corporation, 1999)
;
_computing_molecular_graphics    'PLATON (Spek, 2003)'
_computing_publication_material  PLATON
_computing_structure_refinement  'SHELXL97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS97 (Sheldrick, 1997)'
_diffrn_ambient_temperature      297(2)
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measurement_device_type  'Rigaku AFC-7R'
_diffrn_measurement_method       \w/2\q
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'Rigaku rotating anode'
_diffrn_radiation_type           'MoK\a '
_diffrn_radiation_wavelength     0.71069
_diffrn_reflns_av_R_equivalents  0.0262
_diffrn_reflns_av_sigmaI/netI    0.1376
_diffrn_reflns_limit_h_max       7
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_number            7072
_diffrn_reflns_theta_full        25.01
_diffrn_reflns_theta_max         25.01
_diffrn_reflns_theta_min         2.71
_diffrn_standards_decay_%        2.4
_diffrn_standards_interval_time  150
_diffrn_standards_number         3
_exptl_absorpt_coefficient_mu    0.113
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.388
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             772
_exptl_crystal_size_max          0.30
_exptl_crystal_size_mid          0.25
_exptl_crystal_size_min          0.20
_refine_diff_density_max         0.224
_refine_diff_density_min         -0.180
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.889
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     507
_refine_ls_number_reflns         6147
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.889
_refine_ls_R_factor_all          0.2190
_refine_ls_R_factor_gt           0.0553
_refine_ls_shift/su_max          0.003
_refine_ls_shift/su_mean         0.001
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w = 1/[\s^2^(Fo^2^)+(0.1P)^2^ + 0.2218P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1417
_refine_ls_wR_factor_ref         0.2110
_reflns_number_gt                2203
_reflns_number_total             6147
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            ci6731.cif
_cod_data_source_block           I
_cod_depositor_comments
;
The following automatic conversions were performed:

'_chemical_melting_point' value '419--424' was changed to '422(3)' -
the average value was taken and precision was estimated.

Automatic conversion script
Id: cif_fix_values 1646 2011-03-28 12:23:43Z adriana 

The following automatic conversions were performed:

'_chemical_melting_point' value '419--424' was changed to '422(3)' -
the average value was taken and precision was estimated.

Automatic conversion script
Id: cif_fix_values 1715 2011-07-08 13:25:40Z adriana 
;
_cod_database_code               2208000
_cod_database_fobs_code          2208000