Crystal structure of 1-(2,3-dimethylphenyl)piperazinium dihydrogentriphosphate trihydrate, [C~12~H~19~N~2~]~3~[H~2~P~3~O~10~] · 3H~2~O
Mechergui, Jalloul; Belam, Wahid; Rzaigui, Mohamed; Zeitschrift für Kristallographie - New Crystal Structures 222 (2007) 409–411; doi:

data_8102199
_publ_section_title
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Crystal structure of 1-(2,3-dimethylphenyl)piperazinium dihydrogentriphosphate 
trihydrate, [C~12~H~19~N~2~]~3~[H~2~P~3~O~10~] &#x00B7; 3H~2~O
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_journal_issue                   4
_journal_name_full
'Zeitschrift f\"ur Kristallographie - New Crystal Structures'
_journal_page_first              409
_journal_page_last               411
_journal_volume                  222
_journal_year                    2007
_chemical_compound_source        'synthesis as described'
_chemical_formula_moiety         'C36 H113 N6 O13 P3'
_chemical_formula_structural     '[C12H19N2]3[H2P3O10] &#x00B7; 3H2O'
_chemical_formula_sum            'C36 H65 N6 O13 P3'
_chemical_formula_weight         882.85
_chemical_name_systematic
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1-(2,3-dimethylphenyl)piperazine dihydrogentriphosphate 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_date             2007-12-02T12:21:48-00:00
_audit_creation_method           'WinGX routine CIF_UPDATE'
_cell_angle_alpha                96.72(2)
_cell_angle_beta                 111.050(10)
_cell_angle_gamma                78.55(2)
_cell_formula_units_Z            2
_cell_length_a                   15.036(3)
_cell_length_b                   7.660(2)
_cell_length_c                   20.327(4)
_cell_measurement_reflns_used    25
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      26.97
_cell_measurement_theta_min      2.1
_cell_measurement_wavelength     0.71073
_cell_volume                     2138.8(8)
_computing_cell_refinement       'CAD4 Express (Enraf Nonius, 1994)[2]'
_computing_data_collection       'CAD4 Express (Enraf Nonius, 1994)[2]'
_computing_data_reduction        'XCAD4 (Harms & Wocadlo, 1995)[3]'
_computing_molecular_graphics
'Ortep-3 for Windows (Farrugia, 1997)[6], DIAMOND Version 2.0[7]'
_computing_publication_material  'WinGX (Farrugia, 1999)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)[5]'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1997)[4]'
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 1
_diffrn_measured_fraction_theta_max 1
_diffrn_measurement_device       '\k-geometry diffractometer'
_diffrn_measurement_device_type  'Enraf-Nonius MACH 3'
_diffrn_measurement_method       'non-profiled omega scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0328
_diffrn_reflns_av_unetI/netI     0.0497
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -19
_diffrn_reflns_limit_k_max       9
_diffrn_reflns_limit_k_min       -9
_diffrn_reflns_limit_l_max       25
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_number            9578
_diffrn_reflns_theta_full        26.97
_diffrn_reflns_theta_max         26.97
_diffrn_reflns_theta_min         2.1
_diffrn_standards_decay_%        1
_diffrn_standards_interval_time  120
_diffrn_standards_number         2
_exptl_absorpt_coefficient_mu    0.208
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.371
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             944
_exptl_crystal_size_max          0.8
_exptl_crystal_size_mid          0.3
_exptl_crystal_size_min          0.1
_refine_diff_density_max         0.475
_refine_diff_density_min         -0.448
_refine_diff_density_rms         0.069
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.023
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     523
_refine_ls_number_reflns         9312
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.023
_refine_ls_R_factor_all          0.0972
_refine_ls_R_factor_gt           0.0578
_refine_ls_shift/su_max          0.009
_refine_ls_shift/su_mean         0.001
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0920P)^2^+1.0281P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1493
_refine_ls_wR_factor_ref         0.1706
_reflns_number_gt                6407
_reflns_number_total             9312
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            1267-2126.cff
_cod_data_source_block           global
_cod_depositor_comments
;
 Moving the '_geom_hbond_site_symmetry_A' data name to the end of the
 '_geom_hbond' loop based on loop values.

 Antanas Vaitkus,
 2017-03-07
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_cod_original_sg_symbol_H-M      P-1
_cod_database_code               8102199