Zoledronic acid: monoclinic and triclinic polymorphs from powder diffraction data
Chernyshev, Vladimir V.; Shkavrov, Sergey V.; Paseshnichenko, Ksenia A.; Puryaeva, Tamara P.; Velikodny, Yurii A.; Acta Crystallographica Section C 69 (2013) 263–266; doi:10.1107/S0108270113003089

data_2018811
_publ_section_title
;
 Zoledronic acid: monoclinic and triclinic polymorphs from powder
 diffraction data
;
_journal_coeditor_code           BI3053
_journal_issue                   3
_journal_name_full               'Acta Crystallographica Section C'
_journal_page_first              263
_journal_page_last               266
_journal_paper_doi               10.1107/S0108270113003089
_journal_volume                  69
_journal_year                    2013
_chemical_formula_iupac          'C5 H10 N2 O7 P2'
_chemical_formula_moiety         'C5 H10 N2 O7 P2'
_chemical_formula_sum            'C5 H10 N2 O7 P2'
_chemical_formula_weight         272.09
_chemical_melting_point          495
_chemical_name_common            'Zoledronic acid'
_chemical_name_systematic
;
1-(2-Hydroxy-2-phosphonato-2-phosphonoethyl)-1<i>H</i>-imidazol-3-ium
;
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_audit_creation_method           SHELXL97
_cell_angle_alpha                92.778(16)
_cell_angle_beta                 112.415(17)
_cell_angle_gamma                116.072(19)
_cell_formula_units_Z            2
_cell_length_a                   8.4217(13)
_cell_length_b                   8.6039(11)
_cell_length_c                   8.1818(12)
_cell_measurement_reflns_used    575
_cell_measurement_temperature    298(2)
_cell_measurement_theta_max      39.97
_cell_measurement_theta_min      5.92
_cell_volume                     475.33(18)
_computing_cell_refinement       'MRIA (Zlokazov & Chernyshev, 1992)'
_computing_data_collection
'<i>Software for G670 Imaging-Plate Guinier Camera</i> (Huber, 2002)'
_computing_data_reduction
'<i>Software for G670 Imaging-Plate Guinier Camera</i> (Huber, 2002)'
_computing_molecular_graphics
;
PLATON (Spek, 2009) and Mercury (Macrae <i>et al.</i>, 2008)
;
_computing_publication_material
;
MRIA (Zlokazov & Chernyshev, 1992) and SHELXL97 (Sheldrick,
2008)
;
_computing_structure_refinement  'MRIA (Zlokazov & Chernyshev, 1992)'
_computing_structure_solution
'simulated annealing (Zhukov <i>et al.</i>, 2001)'
_diffrn_ambient_temperature      298(2)
_diffrn_measurement_device       'Huber Guinier Camera G670'
_diffrn_radiation_monochromator  'Curved Germanium(111)'
_diffrn_radiation_source         'line-focus sealed tube'
_diffrn_radiation_type           CuK\a~1~
_diffrn_radiation_wavelength     1.5406
_exptl_absorpt_coefficient_mu    4.498
_exptl_absorpt_correction_type   none
_exptl_crystal_density_diffrn    1.901
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             280
_pd_block_diffractogram_id       T
_pd_char_colour                  white
_pd_char_particle_morphology     'no specific habit'
_pd_instr_location
;
Department of Chemistry, Moscow State University, 119991 Moscow, Russian
Federation
;
_pd_meas_2theta_range_inc        0.01
_pd_meas_2theta_range_max        80.00
_pd_meas_2theta_range_min        7.00
_pd_meas_number_of_points        7301
_pd_meas_scan_method             cont
_pd_prep_pressure                101
_pd_prep_temperature             298(2)
_pd_proc_2theta_range_inc        0.01
_pd_proc_2theta_range_max        80.00
_pd_proc_2theta_range_min        7.00
_pd_proc_info_excluded_regions   none
_pd_proc_ls_background_function  'Chebyshev polynomial up to the fifth order'
_pd_proc_ls_pref_orient_corr
'March--Dollase (Dollase, 1986) texture correction'
_pd_proc_ls_profile_function     'split-type pseudo-Voigt (Toraya, 1986)'
_pd_proc_ls_prof_R_factor        0.0261
_pd_proc_ls_prof_wR_expected     0.0153
_pd_proc_ls_prof_wR_factor       0.0333
_pd_proc_wavelength              1.5406
_pd_spec_mounting
;
thin layer in the specimen holder of the camera
;
_pd_spec_mount_mode              transmission
_pd_spec_shape                   flat_sheet
_pd_spec_size_axial              15
_pd_spec_size_equat              1
_pd_spec_size_thick              1
_refine_diff_density_max         0.37
_refine_diff_density_min         -0.42
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_all   2.133
_refine_ls_hydrogen_treatment    noref
_refine_ls_matrix_type           fullcycle
_refine_ls_number_constraints    0
_refine_ls_number_parameters     102
_refine_ls_number_restraints     43
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Inet
_refine_ls_weighting_scheme      sigma
_cod_data_source_file            bi3053.cif
_cod_data_source_block           IT
_cod_original_cell_volume        475.33(12)
_cod_database_code               2018811