A new series of 3,5-diamino-1,2,4-triazolium(1+) inorganic salts and their potential in crystal engineering of novel NLO materials
Matulková, Irena; Cihelka, Jaroslav; Pojarová, Michaela; Fejfarová, Karla; Dušek, Michal; Vaněk, Přemysl; Kroupa, Jan; Krupková, Radmila; Fábry, Jan; Němec, Ivan; CrystEngComm 14 (2012) 4625–; doi:10.1039/c2ce00024e

data_7215002
_publ_section_title
;
 A new series of 3,5-diamino-1,2,4-triazolium(1+) inorganic salts and
 their potential in crystal engineering of novel NLO materials
;
_journal_issue                   14
_journal_name_full               CrystEngComm
_journal_page_first              4625
_journal_paper_doi               10.1039/c2ce00024e
_journal_volume                  14
_journal_year                    2012
_chemical_absolute_configuration ad
_chemical_formula_moiety         'C2 H6 N5, H2 O4 P '
_chemical_formula_sum            'C2 H8 N5 O4 P'
_chemical_formula_weight         197.1
_space_group_IT_number           43
_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_Hall  'F 2 -2d'
_symmetry_space_group_name_H-M   'F d d 2'
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            16
_cell_length_a                   13.3492(4)
_cell_length_b                   37.1096(12)
_cell_length_c                   6.0702(2)
_cell_measurement_reflns_used    7644
_cell_measurement_temperature    120
_cell_measurement_theta_max      66.6468
_cell_measurement_theta_min      4.7671
_cell_volume                     3007.08(17)
_computing_cell_refinement       'Crysalis RED (Oxford diffraction, 2009)'
_computing_data_collection       'Crysalis CCD (Oxford diffraction, 2009)'
_computing_data_reduction        'Crysalis RED'
_computing_molecular_graphics    'Diamond (Brandenburg & Putz, 2005)'
_computing_publication_material  Jana2006
_computing_structure_refinement
'Jana2006 (Pet\<r\'i\<cek, Du\<sek & Palatinus, 2006)'
_computing_structure_solution    'SIR2002 (Burla et al., 2003)'
_diffrn_ambient_temperature      120
_diffrn_detector_area_resol_mean 10.3784
_diffrn_measured_fraction_theta_full 0.99
_diffrn_measured_fraction_theta_max 0.99
_diffrn_measurement_device       'four-cycle diffractometer'
_diffrn_measurement_device_type
'Goniometer Xcalibur, detector: Atlas (Gemini ultra Cu)'
_diffrn_measurement_method
'Rotation method data acquisition using \w scans'
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_source         'X-ray tube'
_diffrn_radiation_type           'Cu K\a'
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0247
_diffrn_reflns_av_sigmaI/netI    0.0055
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       44
_diffrn_reflns_limit_k_min       -42
_diffrn_reflns_limit_l_max       6
_diffrn_reflns_limit_l_min       -7
_diffrn_reflns_number            8122
_diffrn_reflns_reduction_process
;
Integration of the CCD images was done by program Crysalis RED
(Oxford diffraction, 2008). The same program was used for indexing of the
crystal shape and absorption correction.
;
_diffrn_reflns_theta_full        66.79
_diffrn_reflns_theta_max         66.79
_diffrn_reflns_theta_min         7.05
_exptl_absorpt_coefficient_mu    3.270
_exptl_absorpt_correction_T_max  0.686
_exptl_absorpt_correction_T_min  0.485
_exptl_absorpt_correction_type   analytical
_exptl_absorpt_process_details
;
CrysAlisPro, Oxford Diffraction Ltd.,
Version 1.171.33.51 (release 27-10-2009 CrysAlis171 .NET)
Analytical numeric absorption correction using a multifaceted crystal
model based on expressions derived by R.C. Clark & J.S. Reid.
;
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.7408
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       'irregular shape'
_exptl_crystal_F_000             1632
_exptl_crystal_size_max          0.3851
_exptl_crystal_size_mid          0.2734
_exptl_crystal_size_min          0.1800
_refine_diff_density_max         0.09
_refine_diff_density_min         -0.11
_refine_ls_abs_structure_details 'Flack (1983)'
_refine_ls_abs_structure_Flack   0.034(16)
_refine_ls_extinction_coef       1900(200)
_refine_ls_extinction_method
'B-C type 1 Lorentzian isotropic (Becker & Coppens, 1974)'
_refine_ls_goodness_of_fit_gt    1.52
_refine_ls_goodness_of_fit_ref   1.52
_refine_ls_hydrogen_treatment    refxyz
_refine_ls_number_constraints    9
_refine_ls_number_parameters     133
_refine_ls_number_reflns         1295
_refine_ls_number_restraints     8
_refine_ls_R_factor_all          0.0190
_refine_ls_R_factor_gt           0.0189
_refine_ls_shift/su_max          0.0100
_refine_ls_shift/su_mean         0.0013
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details     w=1/(\s^2^(I)+0.0016I^2^)
_refine_ls_weighting_scheme      sigma
_refine_ls_wR_factor_gt          0.0615
_refine_ls_wR_factor_ref         0.0617
_reflns_number_gt                1290
_reflns_number_total             1295
_reflns_threshold_expression     I>3\s(I)
_cod_data_source_file            c2ce00024e.txt
_cod_data_source_block           III
_cod_original_formula_sum        'C2 H8 N5 O4 P1'
_cod_database_code               7215002