Studies on the crystal structure and arrangement of water in sitagliptinl-tartrate hydrates
Tieger, Eszter; Kiss, Violetta; Pokol, György; Finta, Zoltán; Dušek, Michal; Rohlíček, Jan; Skořepová, Eliška; Brázda, Petr; CrystEngComm 18 (2016) 3819–; doi:10.1039/C6CE00322B

data_7225168
_publ_section_title
;
 Studies on the crystal structure and arrangement of water in
 sitagliptinl-tartrate hydrates
;
_journal_issue                   21
_journal_name_full               CrystEngComm
_journal_page_first              3819
_journal_paper_doi               10.1039/C6CE00322B
_journal_volume                  18
_journal_year                    2016
_chemical_formula_moiety         'C20H21F6N5O7 \\times 4 H2O'
_chemical_formula_sum            'C20 H20 F6 N5 O11.227'
_chemical_formula_weight         624
_chemical_name_common            tetrahydrate
_chemical_name_systematic        'Sitagliptin L-tartrate tetrahydrate'
_space_group_IT_number           5
_symmetry_cell_setting           monoclinic
_symmetry_Int_Tables_number      5
_symmetry_space_group_name_Hall  'C 2y'
_symmetry_space_group_name_H-M   'C 1 2 1'
_audit_update_record
;
2015-11-30 deposited with the CCDC.
2016-04-26 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 95.326(4)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   45.2368(4)
_cell_length_b                   8.2403(4)
_cell_length_c                   7.1817(18)
_cell_measurement_reflns_used    8241
_cell_measurement_temperature    119.98(10)
_cell_measurement_theta_max      62.1
_cell_measurement_theta_min      3.9
_cell_volume                     2665.5(7)
_computing_cell_refinement       'CrysAlisPro 1.171.38.41 (Rigaku OD, 2015)'
_computing_data_collection       'CrysAlisPro 1.171.38.41 (Rigaku OD, 2015)'
_computing_data_reduction        'CrysAlisPro 1.171.38.41 (Rigaku OD, 2015)'
_computing_molecular_graphics    Diamond
_computing_structure_refinement  Jana2006
_computing_structure_solution
;
Superflip, version February 2014
;
_diffrn_ambient_temperature      120
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 5.1873
_diffrn_measured_fraction_theta_full 0.99
_diffrn_measured_fraction_theta_max 0.99
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'Xcalibur, Atlas, Gemini ultra'
_diffrn_measurement_method       '\w scans'
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_source         'X-ray tube'
_diffrn_radiation_type           'Cu K\a'
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0633
_diffrn_reflns_av_unetI/netI     0.0324
_diffrn_reflns_limit_h_max       51
_diffrn_reflns_limit_h_min       -51
_diffrn_reflns_limit_k_max       9
_diffrn_reflns_limit_k_min       -9
_diffrn_reflns_limit_l_max       8
_diffrn_reflns_limit_l_min       -8
_diffrn_reflns_number            19028
_diffrn_reflns_theta_full        62.41
_diffrn_reflns_theta_max         62.41
_diffrn_reflns_theta_min         3.93
_diffrn_source                   'fine-focus sealed X-ray tube'
_exptl_absorpt_coefficient_mu    1.36
_exptl_absorpt_correction_T_max  0.942
_exptl_absorpt_correction_T_min  0.748
_exptl_absorpt_correction_type   analytical
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.38.41 (Rigaku Oxford Diffraction, 2015)
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            white
_exptl_crystal_density_diffrn    1.555
_exptl_crystal_description       platelet
_exptl_crystal_F_000             1275
_exptl_crystal_size_max          0.298
_exptl_crystal_size_mid          0.215
_exptl_crystal_size_min          0.044
_refine_diff_density_max         0.51
_refine_diff_density_min         -0.44
_refine_ls_abs_structure_details
'  1906 of Friedel pairs used in the refinement'
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_gt    2.51
_refine_ls_goodness_of_fit_ref   2.42
_refine_ls_hydrogen_treatment    mixed
_refine_ls_number_constraints    66
_refine_ls_number_parameters     430
_refine_ls_number_reflns         4175
_refine_ls_number_restraints     8
_refine_ls_R_factor_all          0.0716
_refine_ls_R_factor_gt           0.0669
_refine_ls_shift/su_max          0.0428
_refine_ls_shift/su_mean         0.0041
_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          0.1678
_refine_ls_wR_factor_ref         0.1707
_reflns_number_gt                3773
_reflns_number_total             4175
_reflns_threshold_expression     I>3\s(I)
_cod_data_source_file            c6ce00322b2.cif
_cod_data_source_block           I
_cod_depositor_comments
;
The following automatic conversions were performed:

'_diffrn_radiation_probe' value 'X-ray' changed to 'x-ray' according
to
/usr/data/users/saulius/crontab/automatic-downloads/rss-feeds/RSC/lib/dictionaries/cif_core.dic
dictionary named 'cif_core.dic' version 2.4.2 from 2011-04-26.

Automatic conversion script
Id: cif_fix_values 4268 2015-11-12 08:31:59Z antanas 

 Adding full bibliography for 7225166--7225168.cif.
;
_cod_original_formula_sum        'C20 H20 F6 N5 O4.227 O7'
_cod_database_code               7225168