4-(3,5-Dimethyl-1<i>H</i>-pyrazol-4-ylmethyl)-3,5-dimethyl-1<i>H</i>-pyrazol-2-ium dihydrogen phosphate: a combined X-ray and DFT study
Hazra, Dipak K.; Chatterjee, Rajarshi; Ali, Mahammad; Mukherjee, Monika; Acta Crystallographica Section C 66 (2010) o190–o193; doi:10.1107/S0108270110007134

data_2017626
_publ_section_title
;
 4-(3,5-Dimethyl-1<i>H</i>-pyrazol-4-ylmethyl)-3,5-dimethyl-1<i>H</i>-pyrazol-2-ium
 dihydrogen phosphate: a combined X-ray and DFT study
;
_journal_coeditor_code           SK3363
_journal_issue                   4
_journal_name_full               'Acta Crystallographica Section C'
_journal_page_first              o190
_journal_page_last               o193
_journal_paper_doi               10.1107/S0108270110007134
_journal_volume                  66
_journal_year                    2010
_chemical_formula_iupac          'C11 H17 N4 + , H2 O4 P -'
_chemical_formula_moiety         'C11 H17 N4 + , H2 O4 P -'
_chemical_formula_sum            'C11 H19 N4 O4 P'
_chemical_formula_weight         302.27
_chemical_name_systematic
;
4-(3,5-dimethyl-1<i>H</i>-pyrazol-4-ylmethyl)-3,5-dimethyl-1<i>H</i>-
pyrazol-2-ium dihydrogen phosphate
;
_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
_cell_angle_alpha                117.624(3)
_cell_angle_beta                 104.576(4)
_cell_angle_gamma                94.663(4)
_cell_formula_units_Z            2
_cell_length_a                   7.649(4)
_cell_length_b                   10.504(2)
_cell_length_c                   10.538(2)
_cell_measurement_reflns_used    1408
_cell_measurement_temperature    298(2)
_cell_measurement_theta_max      24.18
_cell_measurement_theta_min      2.28
_cell_volume                     706.4(4)
_computing_cell_refinement
;
APEX2 (Bruker, 2007) and SAINT (Bruker, 2007)
;
_computing_data_collection       'APEX2 (Bruker, 2007)'
_computing_data_reduction
;
SAINT (Bruker, 2007) and XPREP (Bruker, 2007)
;
_computing_molecular_graphics
;
ORTEP-3 for Windows (Farrugia, 1997), DIAMOND (Brandenburg,
1999) and
Mercury (Macrae <i>et al.</i>, 2006)
;
_computing_publication_material  'PLATON (Spek, 2009)'
_computing_structure_refinement  'SHELXL97 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      298(2)
_diffrn_measured_fraction_theta_full 0.990
_diffrn_measured_fraction_theta_max 0.990
_diffrn_measurement_device_type  'Bruker APEXII Kappa CCD area-detector'
_diffrn_measurement_method       '\w and \f'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
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_diffrn_reflns_av_sigmaI/netI    0.0602
_diffrn_reflns_limit_h_max       8
_diffrn_reflns_limit_h_min       -8
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       12
_diffrn_reflns_limit_l_min       -12
_diffrn_reflns_number            4686
_diffrn_reflns_theta_full        24.18
_diffrn_reflns_theta_max         24.18
_diffrn_reflns_theta_min         2.28
_exptl_absorpt_coefficient_mu    0.214
_exptl_absorpt_correction_T_max  0.986
_exptl_absorpt_correction_T_min  0.933
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   '(SADABS; Bruker, 2001)'
_exptl_crystal_colour            brown
_exptl_crystal_density_diffrn    1.421
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       flake
_exptl_crystal_F_000             320
_exptl_crystal_size_max          0.35
_exptl_crystal_size_mid          0.23
_exptl_crystal_size_min          0.02
_refine_diff_density_max         0.203
_refine_diff_density_min         -0.380
_refine_ls_extinction_method     none
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_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     189
_refine_ls_number_reflns         2239
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.032
_refine_ls_R_factor_all          0.0830
_refine_ls_R_factor_gt           0.0516
_refine_ls_shift/su_max          0.017
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w = 1/[\s^2^(Fo^2^)+(0.0706P)^2^+0.0452P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1206
_refine_ls_wR_factor_ref         0.1357
_reflns_number_gt                1536
_reflns_number_total             2239
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            sk3363.cif
_cod_data_source_block           I
_cod_depositor_comments
;
The following automatic conversions were performed:
'_geom_bond_publ_flag' value 'Y' changed to 'y' according to
'/home/saulius/struct/CIF-dictionaries/cif_core.dic' dictionary named
'cif_core.dic' version 2.4.1 from 2010-06-29 (10
times).

'_geom_torsion_publ_flag' value 'Y' changed to 'y' according to
'/home/saulius/struct/CIF-dictionaries/cif_core.dic' dictionary named
'cif_core.dic' version 2.4.1 from 2010-06-29 (2 times).

Automatic conversion script
Id: cif_fix_enum 1527 2010-12-29 10:47:43Z saulius 
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_cod_original_cell_volume        706.4(5)
_cod_database_code               2017626
_cod_database_fobs_code          2017626