A general method for cultivating single crystals from melt microdroplets.
Ou, Xiao; Li, Xizhen; Rong, Haowei; Yu, Lian; Lu, Ming; Chemical communications (Cambridge, England) 56 (2020) 9950–9953; doi:10.1039/d0cc03157g

data_7126908
_publ_section_title
;
 A general method for cultivating single crystals from melt microdroplets.
;
_journal_issue                   69
_journal_name_full
'Chemical communications (Cambridge, England)'
_journal_page_first              9950
_journal_page_last               9953
_journal_paper_doi               10.1039/d0cc03157g
_journal_volume                  56
_journal_year                    2020
_chemical_absolute_configuration ad
_chemical_formula_moiety         'C17 H25 N3 O2'
_chemical_formula_sum            'C17 H26 N3 O2'
_chemical_formula_weight         304.41
_chemical_melting_point          428
_chemical_name_common            Vildagliptin
_space_group_crystal_system      orthorhombic
_space_group_IT_number           19
_space_group_name_Hall           'P 2ac 2ab'
_space_group_name_H-M_alt        'P 21 21 21'
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     dual
_audit_creation_date             2020-01-02
_audit_creation_method
;
Olex2 1.3
(compiled Nov 21 2019 18:26:39 for OlexSys, GUI svn.r6003)
;
_audit_update_record
;
2020-03-01 deposited with the CCDC.	2020-07-13 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   10.14270(10)
_cell_length_b                   10.60440(10)
_cell_length_c                   14.51410(10)
_cell_measurement_reflns_used    11987
_cell_measurement_temperature    100.01(10)
_cell_measurement_theta_max      75.7290
_cell_measurement_theta_min      5.1370
_cell_volume                     1561.10(2)
_computing_cell_refinement       'CrysAlisPro 1.171.40.54a (Rigaku OD, 2019)'
_computing_data_collection       'CrysAlisPro 1.171.40.54a (Rigaku OD, 2019)'
_computing_data_reduction        'CrysAlisPro 1.171.40.54a (Rigaku OD, 2019)'
_computing_molecular_graphics    'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2016/6 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT 2014/5 (Sheldrick, 2014)'
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      100.01(10)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 10.0000
_diffrn_detector_type            HyPix
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.967
_diffrn_measurement_details
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  t~exp~   \w     \q     \k     \f   Frames
  1  \w    -63.00  26.00   0.50    0.05    --  -46.62  57.00   0.00  178
  2  \w     74.00 120.00   0.50    0.05    --   46.62 127.00  58.00   92
  3  \w     87.00 178.00   0.50    0.11    --  105.44  13.00  -4.00  182
  4  \w     33.00 117.00   0.50    0.11    --  105.44-125.00  60.00  168
  5  \w     15.00  95.00   0.50    0.05    --   46.62-125.00-150.00  160
  6  \w   -112.00 -27.00   0.50    0.11    -- -100.00 116.00 155.00  170
  7  \w   -117.00 -27.00   0.50    0.11    -- -100.00  61.00 -30.00  180
  8  \w   -119.00 -30.00   0.50    0.05    --  -46.62 -57.00  60.00  178
  9  \w   -119.00 -23.00   0.50    0.05    --  -46.62 -77.00  30.00  192
 10  \w   -123.00 -28.00   0.50    0.05    --  -46.62 -13.00-176.00  190
 11  \w   -119.00 -23.00   0.50    0.05    --  -46.62 -77.00-180.00  192
 12  \w   -119.00 -23.00   0.50    0.05    --  -46.62 -77.00 -30.00  192
 13  \w   -124.00 -27.00   0.50    0.11    -- -100.00  77.00 -30.00  194
 14  \w   -173.00 -70.00   0.50    0.11    -- -100.00-127.00 -17.00  206
 15  \w   -173.00 -82.00   0.50    0.11    -- -100.00 -61.00-180.00  182
 16  \w   -172.00-135.00   0.50    0.11    -- -100.00 -45.00  90.00   74
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'XtaLAB Synergy R, DW system, HyPix'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      0.0002758000
_diffrn_orient_matrix_UB_12      -0.0507122000
_diffrn_orient_matrix_UB_13      -0.0994573000
_diffrn_orient_matrix_UB_21      0.0256063000
_diffrn_orient_matrix_UB_22      0.1342618000
_diffrn_orient_matrix_UB_23      -0.0365362000
_diffrn_orient_matrix_UB_31      0.1496417000
_diffrn_orient_matrix_UB_32      -0.0228911000
_diffrn_orient_matrix_UB_33      0.0064125000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Cu K\a'
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0522
_diffrn_reflns_av_unetI/netI     0.0311
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.967
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            14740
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.947
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         76.016
_diffrn_reflns_theta_min         5.166
_diffrn_source                   'Rotating-anode X-ray tube'
_diffrn_source_type              'Rigaku (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    0.685
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.66427
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.40.54a (Rigaku Oxford Diffraction, 2019)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            'clear light colourless'
_exptl_crystal_density_diffrn    1.295
_exptl_crystal_description       block
_exptl_crystal_F_000             660
_exptl_crystal_recrystallization_method 'From the Melt'
_exptl_crystal_size_max          0.14
_exptl_crystal_size_mid          0.09
_exptl_crystal_size_min          0.05
_refine_diff_density_max         0.273
_refine_diff_density_min         -0.249
_refine_diff_density_rms         0.069
_refine_ls_abs_structure_details
;
 Flack x determined using 1184 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   -0.06(11)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.086
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     203
_refine_ls_number_reflns         3087
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.086
_refine_ls_R_factor_all          0.0410
_refine_ls_R_factor_gt           0.0384
_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^)+(0.0648P)^2^+0.2077P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0994
_refine_ls_wR_factor_ref         0.1027
_reflns_Friedel_coverage         0.702
_reflns_Friedel_fraction_full    0.997
_reflns_Friedel_fraction_max     0.918
_reflns_number_gt                2938
_reflns_number_total             3087
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d0cc03157g2.cif
_cod_data_source_block           Vildagliptin-100k-HWRong
_cod_depositor_comments
;
The following automatic conversions were performed:

data item '_chemical_melting_point' value '428K' was changed to '428'
-- the value should be numeric and without a unit designator.

Automatic conversion script
Id: cif_fix_values 7556 2019-12-06 15:28:31Z antanas 

 Adding full bibliography for 7126896--7126915.cif.
;
_cod_database_code               7126908
_shelx_shelxl_version_number     2016/6
_reflns_odcompleteness_completeness 100.00
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     66.97
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups, All N(H) groups
 At 1.5 times of:
  All O(H) groups
2.a Ternary CH refined with riding coordinates:
 C008(H008), C00C(H00G), C00G(H00L)
2.b Secondary CH2 refined with riding coordinates:
 C007(H00A,H00B), C00A(H00C,H00D), C00B(H00E,H00F), C00D(H00H,H00I), C00E(H00J,
 H00K), C00H(H00M,H00N), C00I(H00O,H00P), C00J(H00Q,H00R), C00K(H00S,H00T),
 C00M(H00U,H00V)
2.c Idealised tetrahedral OH refined as rotating group:
 O002(H002)
;
_shelx_res_checksum              63106
_olex2_submission_special_instructions 'No special instructions were received'
_oxdiff_exptl_absorpt_empirical_details
;
Empirical correction (ABSPACK) includes:
- Absorption correction using spherical harmonics
- Frame scaling
;
_oxdiff_exptl_absorpt_empirical_full_max 1.293
_oxdiff_exptl_absorpt_empirical_full_min 0.734