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_7225166
_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_sum            'C40 H44 F12 N10 O15'
_chemical_formula_weight         1132.8
_chemical_name_common            'Phase 1'
_chemical_name_systematic        'Sitagliptin L-tartrate Phase 1'
_space_group_IT_number           4
_symmetry_cell_setting           monoclinic
_symmetry_Int_Tables_number      4
_symmetry_space_group_name_Hall  'P 2yb'
_symmetry_space_group_name_H-M   'P 1 21 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                 106.181
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   7.2124
_cell_length_b                   29.0912
_cell_length_c                   11.686
_cell_measurement_reflns_used    7676
_cell_measurement_temperature    119.8(3)
_cell_measurement_theta_max      67
_cell_measurement_theta_min      4.22
_cell_volume                     2354.796
_computing_cell_refinement       'CrysAlisPro 1.171.38.24t (Agilent, 2015)'
_computing_data_collection       'CrysAlisPro 1.171.38.24t (Agilent, 2015)'
_computing_data_reduction        'CrysAlisPro 1.171.38.24t (Agilent, 2015)'
_computing_molecular_graphics    Diamond
_computing_structure_refinement  Jana2006
_computing_structure_solution
;
Superflip, version February 2014
;
_diffrn_ambient_temperature      119.8
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 10.3745
_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  0.036
_diffrn_reflns_av_unetI/netI     0.0512
_diffrn_reflns_limit_h_max       8
_diffrn_reflns_limit_h_min       -8
_diffrn_reflns_limit_k_max       33
_diffrn_reflns_limit_k_min       -34
_diffrn_reflns_limit_l_max       13
_diffrn_reflns_limit_l_min       -13
_diffrn_reflns_number            16059
_diffrn_reflns_theta_full        67.12
_diffrn_reflns_theta_max         67.12
_diffrn_reflns_theta_min         3.04
_diffrn_source                   'fine-focus sealed X-ray tube'
_exptl_absorpt_coefficient_mu    1.35
_exptl_absorpt_correction_T_max  0.8818
_exptl_absorpt_correction_T_min  0.6244
_exptl_absorpt_correction_type   gaussian
_exptl_absorpt_process_details   Jana2006
_exptl_crystal_colour            white
_exptl_crystal_density_diffrn    1.5977
_exptl_crystal_description       needle
_exptl_crystal_F_000             1164
_exptl_crystal_size_max          0.383
_exptl_crystal_size_mid          0.081
_exptl_crystal_size_min          0.058
_refine_diff_density_max         0.18
_refine_diff_density_min         -0.22
_refine_ls_abs_structure_details
'  3957 of Friedel pairs used in the refinement'
_refine_ls_abs_structure_Flack   0.00(14)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_gt    1.22
_refine_ls_goodness_of_fit_ref   1.22
_refine_ls_hydrogen_treatment    mixed
_refine_ls_number_constraints    125
_refine_ls_number_parameters     763
_refine_ls_number_reflns         8219
_refine_ls_number_restraints     18
_refine_ls_R_factor_all          0.0520
_refine_ls_R_factor_gt           0.0438
_refine_ls_shift/su_max          0.0819
_refine_ls_shift/su_mean         0.0014
_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          0.1042
_refine_ls_wR_factor_ref         0.1141
_reflns_number_gt                6914
_reflns_number_total             8219
_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.

'_exptl_absorpt_correction_type' value 'Gaussian' changed to
'gaussian' 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_database_code               7225166