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_7126911
_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_formula_moiety         'C9 H8 O4'
_chemical_formula_sum            'C9 H8 O4'
_chemical_formula_weight         180.15
_chemical_melting_point          415
_chemical_name_common            Aspirin
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2ybc'
_space_group_name_H-M_alt        'P 1 21/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_audit_creation_date             2019-12-24
_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                 95.949(2)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   11.2582(3)
_cell_length_b                   6.54710(10)
_cell_length_c                   11.2600(3)
_cell_measurement_reflns_used    8315
_cell_measurement_temperature    100.00(10)
_cell_measurement_theta_max      75.1610
_cell_measurement_theta_min      3.9230
_cell_volume                     825.49(3)
_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      100.00(10)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 10.0000
_diffrn_detector_type            HyPix
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.974
_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    -27.00  61.00   0.50    0.35    --   46.25 -38.00  60.00  176
  2  \w     -5.00  83.00   0.50    0.35    --   46.25-103.00  72.00  176
  3  \w     33.00 110.00   0.50    1.38    --  105.44-103.00  72.00  154
  4  \w     33.00 178.00   0.50    1.38    --  105.44   0.00 -90.00  290
  5  \w     90.00 178.00   0.50    1.38    --  105.44  30.00   0.00  176
  6  \w     86.00 178.00   0.50    1.38    --  105.44 103.00 174.00  184
  7  \w     33.00 108.00   0.50    1.38    --  105.44 -94.00  30.00  150
  8  \w     29.00 123.00   0.50    1.38    --  105.44 -15.00-120.00  188
  9  \w     33.00 108.00   0.50    1.38    --  105.44 -94.00 -90.00  150
 10  \w     33.00 120.00   0.50    1.38    --  105.44 -45.00  60.00  174
 11  \w     33.00 178.00   0.50    1.38    --  105.44   0.00 -90.00  290
 12  \w     33.00 108.00   0.50    1.38    --  105.44 -94.00-120.00  150
 13  \w     15.00  95.00   0.50    0.35    --   46.25-125.00 -90.00  160
 14  \w    -27.00  61.00   0.50    0.35    --   46.25 -38.00 120.00  176
 15  \w     30.00 118.00   0.50    0.35    --   46.25  57.00  90.00  176
 16  \w     30.00 118.00   0.50    0.35    --   46.25  57.00  30.00  176
 17  \w     30.00 118.00   0.50    0.35    --   46.25  57.00 150.00  176
 18  \w     23.00 118.00   0.50    0.35    --   46.25  77.00 -60.00  190
 19  \w     23.00 118.00   0.50    0.35    --   46.25  77.00-180.00  190
 20  \w     30.00 118.00   0.50    0.35    --   46.25  57.00 -90.00  176
 21  \w    -83.00   9.00   0.50    0.35    --  -46.25 103.00 174.00  184
 22  \w   -110.00 -27.00   0.50    1.38    -- -100.00 103.00 174.00  166
 23  \w   -115.00 -25.00   0.50    1.38    -- -100.00  30.00 150.00  180
 24  \w   -117.00 -27.00   0.50    1.38    -- -100.00 125.00 -30.00  180
 25  \w   -118.00 -24.00   0.50    1.38    -- -100.00  15.00-150.00  188
 26  \w   -118.00 -71.00   0.50    0.35    --  -46.25-125.00-150.00   94
 27  \w   -118.00 -71.00   0.50    0.35    --  -46.25-125.00-180.00   94
 28  \w   -118.00 -71.00   0.50    0.35    --  -46.25-125.00 -60.00   94
 29  \w   -173.00 -82.00   0.50    1.38    -- -100.00-103.00  72.00  182
 30  \w   -173.00 -82.00   0.50    1.38    -- -100.00 -61.00 120.00  182
 31  \w   -175.00 -84.00   0.50    1.38    -- -100.00 -30.00 -30.00  182
 32  \w   -173.00-138.00   0.50    1.38    -- -100.00 -61.00  90.00   70
;
_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      -0.0124908000
_diffrn_orient_matrix_UB_12      -0.1821279000
_diffrn_orient_matrix_UB_13      0.0844276000
_diffrn_orient_matrix_UB_21      0.1250412000
_diffrn_orient_matrix_UB_22      -0.0757692000
_diffrn_orient_matrix_UB_23      -0.0233908000
_diffrn_orient_matrix_UB_31      0.0560033000
_diffrn_orient_matrix_UB_32      0.1284291000
_diffrn_orient_matrix_UB_33      0.1059793000
_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  0.0980
_diffrn_reflns_av_unetI/netI     0.0393
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.974
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       8
_diffrn_reflns_limit_k_min       -8
_diffrn_reflns_limit_l_max       13
_diffrn_reflns_limit_l_min       -13
_diffrn_reflns_number            13802
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.974
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         75.931
_diffrn_reflns_theta_min         3.948
_diffrn_source                   'Rotating-anode X-ray tube'
_diffrn_source_type              'Rigaku (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    0.984
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.55063
_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    1.450
_exptl_crystal_description       block
_exptl_crystal_F_000             376
_exptl_crystal_recrystallization_method 'From the Melt'
_exptl_crystal_size_max          0.18
_exptl_crystal_size_mid          0.08
_exptl_crystal_size_min          0.05
_refine_diff_density_max         0.641
_refine_diff_density_min         -0.405
_refine_diff_density_rms         0.121
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.061
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     120
_refine_ls_number_reflns         1682
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.061
_refine_ls_R_factor_all          0.0701
_refine_ls_R_factor_gt           0.0680
_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^)+(0.1374P)^2^+0.2686P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1821
_refine_ls_wR_factor_ref         0.1847
_reflns_Friedel_coverage         0.000
_reflns_number_gt                1578
_reflns_number_total             1682
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d0cc03157g2.cif
_cod_data_source_block           Aspirin-100k-XOu
_cod_depositor_comments
;
The following automatic conversions were performed:

data item '_chemical_melting_point' value '415K' was changed to '415'
-- 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               7126911
_shelx_shelxl_version_number     2016/6
_reflns_odcompleteness_completeness 99.75
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     66.97
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
 At 1.5 times of:
  All C(H,H,H) groups, All O(H) groups
2.a Aromatic/amide H refined with riding coordinates:
 C009(H009), C00A(H00A), C00B(H00B), C00D(H00F)
2.b Idealised Me refined as rotating group:
 C00C(H00C,H00D,H00E)
2.c Idealised tetrahedral OH refined as rotating group:
 O002(H002)
;
_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 4.260
_oxdiff_exptl_absorpt_empirical_full_min 0.434