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_7126906
_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         'C27 H36 N2 O4'
_chemical_formula_sum            'C27 H36 N2 O4'
_chemical_formula_weight         452.58
_chemical_melting_point          409
_chemical_name_common            Repaglinide
_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   geom
_atom_sites_solution_primary     dual
_audit_creation_date             2019-12-25
_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                   8.32210(10)
_cell_length_b                   13.3053(2)
_cell_length_c                   22.7527(3)
_cell_measurement_reflns_used    13390
_cell_measurement_temperature    99.99(10)
_cell_measurement_theta_max      76.6040
_cell_measurement_theta_min      5.1250
_cell_volume                     2519.36(6)
_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      99.99(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 0.993
_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    -61.00  27.00   0.50    0.64    --  -46.62  38.00  60.00  176
  2  \w     14.00  94.00   0.50    0.64    --   46.62-123.00 -77.00  160
  3  \w   -120.00 -32.00   0.50    0.64    --  -46.62 -38.00  90.00  176
  4  \w   -119.00 -73.00   0.50    0.64    --  -46.62-123.00 -77.00   92
  5  \w   -119.00 -71.00   0.50    0.64    --  -46.62-125.00 -30.00   96
  6  \w   -119.00 -30.00   0.50    0.64    --  -46.62 -57.00 -90.00  178
  7  \w   -119.00 -23.00   0.50    0.64    --  -46.62 -77.00-150.00  192
  8  \w   -119.00 -30.00   0.50    0.64    --  -46.62 -57.00   0.00  178
  9  \w     34.00 115.00   0.50    2.55    --  107.00-123.00-168.00  162
 10  \w     34.00 115.00   0.50    2.55    --  107.00-123.00 -77.00  162
 11  \w     34.00 109.00   0.50    2.55    --  107.00 -94.00   0.00  150
 12  \w     31.00 125.00   0.50    2.55    --  107.00 -15.00 -60.00  188
 13  \w     85.00 178.00   0.50    2.55    --  107.00  10.00-176.00  186
 14  \w     34.00 109.00   0.50    2.55    --  107.00 -94.00-120.00  150
 15  \w     32.00 123.00   0.50    2.55    --  107.00 -30.00-180.00  182
 16  \w     34.00 131.00   0.50    2.55    --  107.00 -77.00-150.00  194
 17  \w     34.00 109.00   0.50    2.55    --  107.00 -94.00-180.00  150
 18  \w     35.00 122.00   0.50    2.55    --  107.00 -45.00-180.00  174
;
_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      -0.0030190000
_diffrn_orient_matrix_UB_12      0.0919930000
_diffrn_orient_matrix_UB_13      -0.0410167000
_diffrn_orient_matrix_UB_21      0.0248655000
_diffrn_orient_matrix_UB_22      -0.0693909000
_diffrn_orient_matrix_UB_23      -0.0534841000
_diffrn_orient_matrix_UB_31      -0.1834467000
_diffrn_orient_matrix_UB_32      -0.0109028000
_diffrn_orient_matrix_UB_33      -0.0065769000
_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  0.0452
_diffrn_reflns_av_unetI/netI     0.0295
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.993
_diffrn_reflns_limit_h_max       7
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       28
_diffrn_reflns_limit_l_min       -28
_diffrn_reflns_number            25212
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.980
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         76.883
_diffrn_reflns_theta_min         3.849
_diffrn_source                   'Rotating-anode X-ray tube'
_diffrn_source_type              'Rigaku (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    0.637
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.63520
_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            colourless
_exptl_crystal_density_diffrn    1.193
_exptl_crystal_description       block
_exptl_crystal_F_000             976
_exptl_crystal_recrystallization_method 'From the Melt'
_exptl_crystal_size_max          0.3
_exptl_crystal_size_mid          0.05
_exptl_crystal_size_min          0.03
_refine_diff_density_max         0.193
_refine_diff_density_min         -0.210
_refine_diff_density_rms         0.037
_refine_ls_abs_structure_details
;
 Flack x determined using 1927 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   -0.01(9)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.049
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     302
_refine_ls_number_reflns         5214
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.049
_refine_ls_R_factor_all          0.0404
_refine_ls_R_factor_gt           0.0370
_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^)+(0.0537P)^2^+0.3297P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0921
_refine_ls_wR_factor_ref         0.0938
_reflns_Friedel_coverage         0.737
_reflns_Friedel_fraction_full    1.000
_reflns_Friedel_fraction_max     0.963
_reflns_number_gt                4875
_reflns_number_total             5214
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d0cc03157g2.cif
_cod_data_source_block           Repaglinide-100k-XOu
_cod_depositor_comments
;
The following automatic conversions were performed:

data item '_chemical_melting_point' value '409K' was changed to '409'
-- 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               7126906
_shelx_shelxl_version_number     2016/6
_reflns_odcompleteness_completeness 100.00
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     71.98
_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 C(H,H,H) groups, All O(H) groups
2.a Ternary CH refined with riding coordinates:
 C00I(H00I), C00L(H00L)
2.b Secondary CH2 refined with riding coordinates:
 C00G(H00A,H00B), C00J(H00D,H00F), C00O(H00G,H00J), C00P(H00O,H00P), C00S(H00U,
 H00V), C00U(H00Z,H), C00V(H00,HA), C00X(H2,HD)
2.c Aromatic/amide H refined with riding coordinates:
 N005(H005), C00C(H00C), C00E(H00E), C00H(H00H), C00K(H00K), C00M(H00M),
 C00N(H00N), C00Q(H00Q)
2.d Idealised Me refined as rotating group:
 C00R(H00R,H00S,H00T), C00T(H00W,H00X,H00Y), C00W(H1,HB,HC)
2.e Idealised tetrahedral OH refined as rotating group:
 O004(H004)
;
_shelx_res_checksum              18839
_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 2.100
_oxdiff_exptl_absorpt_empirical_full_min 0.581