Molecular crystals of 2-amino-1,3,4-thiadiazole with inorganic oxyacids ‒ crystal engineering, phase transformations and NLO properties
Matulková, I.; Cihelka, J.; Pojarová, M.; Fejfarová, K.; Dušek, M.; Císařová, I.; Vaněk, P.; Kroupa, J.; Němec, P.; Tesařová, N.; Němec, I.; CrystEngComm 16 (2014) 1763–; doi:10.1039/c3ce42306a

data_7214026
_publ_section_title
;
 Molecular crystals of 2-amino-1,3,4-thiadiazole with inorganic oxyacids
 -- crystal engineering, phase transformations and NLO properties
;
_journal_issue                   9
_journal_name_full               CrystEngComm
_journal_page_first              1763
_journal_paper_doi               10.1039/c3ce42306a
_journal_volume                  16
_journal_year                    2014
_chemical_formula_moiety         'C2 H4 N3 S, H O3 P'
_chemical_formula_sum            'C2 H5 N3 O3 P S'
_chemical_formula_weight         182.12
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2yab'
_symmetry_space_group_name_H-M   'P 1 21/a 1'
_atom_sites_solution_hydrogens   direct
_atom_sites_solution_primary     geom
_cell_angle_alpha                90
_cell_angle_beta                 96.820(6)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   6.2442(5)
_cell_length_b                   13.1523(12)
_cell_length_c                   8.5929(5)
_cell_measurement_reflns_used    3719
_cell_measurement_temperature    120(2)
_cell_measurement_theta_max      62.9787
_cell_measurement_theta_min      3.3575
_cell_volume                     700.70(9)
_computing_cell_refinement       'CrysAlis Pro (Oxford Diffraction, 2009)'
_computing_data_collection       'CrysAlis Pro (Oxford Diffraction, 2009)'
_computing_data_reduction        'CrysAlis Pro (Oxford Diffraction, 2009)'
_computing_molecular_graphics    none
_computing_publication_material
; CRYSTALS (Betteridge et al., 2003),
publCIF(MacMahon, 2008)
;
_computing_structure_refinement  'CRYSTALS (Betteridge et al., 2003)'
_computing_structure_solution    'SIR92 (Altomare et al., 1994)'
_diffrn_ambient_temperature      120(2)
_diffrn_detector_area_resol_mean 10.3784
_diffrn_measured_fraction_theta_full 0.996
_diffrn_measured_fraction_theta_max 0.993
_diffrn_measurement_device_type  'Xcalibur, Atlas, Gemini ultra'
_diffrn_measurement_method       \w/2\q
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_source         'Enhance Ultra (Cu) X-ray Source'
_diffrn_radiation_type           'Cu K\a'
_diffrn_radiation_wavelength     1.54180
_diffrn_reflns_av_R_equivalents  0.061
_diffrn_reflns_limit_h_max       6
_diffrn_reflns_limit_h_min       -7
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       9
_diffrn_reflns_limit_l_min       -9
_diffrn_reflns_number            5609
_diffrn_reflns_theta_full        61.808
_diffrn_reflns_theta_max         63.069
_diffrn_reflns_theta_min         5.184
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    5.973
_exptl_absorpt_correction_T_max  0.916
_exptl_absorpt_correction_T_min  0.784
_exptl_absorpt_correction_type   analytical
_exptl_absorpt_process_details   'CrysAlis Pro (Oxford Diffraction, 2009)'
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.726
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             372
_exptl_crystal_size_max          0.3920
_exptl_crystal_size_mid          0.2247
_exptl_crystal_size_min          0.1274
_refine_diff_density_max         1.11
_refine_diff_density_min         -0.63
_refine_ls_extinction_method     None
_refine_ls_goodness_of_fit_ref   1.1054
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     91
_refine_ls_number_reflns         962
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0834
_refine_ls_R_factor_gt           0.0769
_refine_ls_shift/su_max          0.0001533
_refine_ls_shift/su_mean         0.0431998
_refine_ls_structure_factor_coef F
_refine_ls_weighting_details
;
Method, part 1, Chebychev polynomial, (Watkin, 1994, Prince, 1982)
[weight] = 1.0/[A~0~*T~0~(x)+A~1~*T~1~(x) ... +A~n-1~]*T~n-1~(x)]
where A~i~ are the Chebychev coefficients listed below and x= Fcalc/Fmax
Method = Robust Weighting (Prince, 1982)
W = [weight] * [1-(deltaF/6*sigmaF)^2^]^2^
A~i~ are:
24.3 24.3 22.8 10.0
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.0679
_refine_ls_wR_factor_gt          0.0662
_refine_ls_wR_factor_ref         0.0662
_reflns_limit_h_max              7
_reflns_limit_h_min              -7
_reflns_limit_k_max              15
_reflns_limit_k_min              0
_reflns_limit_l_max              9
_reflns_limit_l_min              0
_reflns_number_gt                962
_reflns_number_total             1123
_reflns_threshold_expression     I>2.0\s(I)
_oxford_diffrn_Wilson_B_factor   2.27
_oxford_diffrn_Wilson_scale      0.07
_oxford_refine_ls_r_factor_ref   0.0769
_oxford_refine_ls_scale          3.75(2)
_oxford_reflns_number_all        1118
_oxford_reflns_threshold_expression_ref I>2.0\s(I)
_cod_data_source_file            c3ce42306a.txt
_cod_data_source_block           1
_cod_original_sg_symbol_H-M      'P 21/a '
_cod_original_formula_sum        'C2 H5 N3 O3 P1 S1'
_cod_database_code               7214026