Crystal structures and phase transitions of imidazolium hypodiphosphates
Budzikur, Daria; Szklarz, Przemysław; Kinzhybalo, Vasyl; Ślepokura, Katarzyna A.; Acta Crystallographica Section B 76 (2020) –; doi:10.1107/S2052520620011439

data_2108671
_publ_section_title
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 Crystal structures and phase transitions of imidazolium hypodiphosphates
;
_journal_coeditor_code           YB5027
_journal_issue                   5
_journal_name_full               'Acta Crystallographica Section B'
_journal_page_first
;
;
_journal_paper_doi               10.1107/S2052520620011439
_journal_volume                  76
_journal_year                    2020
_chemical_formula_moiety         '(C3 H5 N2), (H3 O6 P2)'
_chemical_formula_sum            'C3 H8 N2 O6 P2'
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_space_group_name_Hall           '-P 2a 2bc'
_space_group_name_H-M_alt        'P n n a'
_atom_sites_solution_hydrogens   mixed
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_atom_sites_solution_secondary   difmap
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_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   6.962(3)
_cell_length_b                   8.368(3)
_cell_length_c                   14.388(4)
_cell_measurement_reflns_used    4526
_cell_measurement_temperature    291(2)
_cell_measurement_theta_max      29.0850
_cell_measurement_theta_min      4.7210
_cell_volume                     838.2(5)
_computing_cell_refinement       'CrysAlisPro 1.171.39.46 (Rigaku OD, 2018)'
_computing_data_collection       'CrysAlisPro 1.171.39.46 (Rigaku OD, 2018)'
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_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2015)'
_diffrn_ambient_temperature      291(2)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 10.6249
_diffrn_detector_type            Atlas
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.984
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'Agilent Technologies, Xcalibur R'
_diffrn_measurement_method       'omega scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0261
_diffrn_reflns_av_unetI/netI     0.0142
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.984
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_h_min       -9
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_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -19
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_diffrn_reflns_point_group_measured_fraction_full 1.000
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_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         29.226
_diffrn_reflns_theta_min         2.816
_diffrn_source                   'fine-focus sealed X-ray tube'
_diffrn_source_type              'Enhance (Mo) X-ray Source'
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_exptl_absorpt_process_details
;
CrysAlisPro 1.171.39.46 (Rigaku Oxford Diffraction, 2018)
Analytical numeric absorption correction using a multifaceted crystal
   model based on expressions derived by R.C. Clark & J.S. Reid.
(Clark, R. C. & Reid, J. S. (1995). Acta Cryst. A51, 887-897)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.823
_exptl_crystal_description       plate
_exptl_crystal_F_000             472
_exptl_crystal_size_max          0.350
_exptl_crystal_size_mid          0.210
_exptl_crystal_size_min          0.100
_refine_diff_density_max         0.235
_refine_diff_density_min         -0.395
_refine_diff_density_rms         0.057
_refine_ls_extinction_coef       0.065(4)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     'SHELXL-2014/7 (Sheldrick 2015)'
_refine_ls_goodness_of_fit_ref   1.050
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     101
_refine_ls_number_reflns         1128
_refine_ls_number_restraints     35
_refine_ls_restrained_S_all      1.035
_refine_ls_R_factor_all          0.0456
_refine_ls_R_factor_gt           0.0351
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0419P)^2^+0.4756P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0865
_refine_ls_wR_factor_ref         0.0949
_reflns_Friedel_coverage         0.000
_reflns_number_gt                901
_reflns_number_total             1128
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            yb5027sup1.cif
_cod_data_source_block           I_RTP
_cod_database_code               2108671
_shelx_shelxl_version_number     2014/7
_shelx_estimated_absorpt_t_min   0.838
_shelx_estimated_absorpt_t_max   0.950
_shelx_res_checksum              75603
_shelx_hkl_checksum              72095
_cod_database_fobs_code 2108671