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_7126898
_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         'C22 H24 Cl F N4 O3'
_chemical_formula_sum            'C22 H24 Cl F N4 O3'
_chemical_formula_weight         446.90
_chemical_melting_point          468.5
_chemical_name_common            Gefitinib
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_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                93.6600(10)
_cell_angle_beta                 97.5860(10)
_cell_angle_gamma                101.8710(10)
_cell_formula_units_Z            2
_cell_length_a                   8.81100(10)
_cell_length_b                   9.6610(2)
_cell_length_c                   12.4893(2)
_cell_measurement_reflns_used    26680
_cell_measurement_temperature    100.00(10)
_cell_measurement_theta_max      76.9180
_cell_measurement_theta_min      3.5890
_cell_volume                     1026.74(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 1.000
_diffrn_measured_fraction_theta_max 0.975
_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    -94.00  -9.00   0.50    0.09    --  -46.62 123.00 -63.00  170
  2  \w   -119.00 -55.00   0.50    0.09    --  -46.62-149.00  52.00  128
  3  \w   -109.00 -23.00   0.50    0.09    --  -46.62 149.00  99.00  172
  4  \w   -119.00 -73.00   0.50    0.09    --  -46.62-123.00-143.00   92
  5  \w     14.00  94.00   0.50    0.09    --   46.62-123.00-143.00  160
  6  \w     28.00 110.00   0.50    0.09    --   46.62-149.00  52.00  164
  7  \w     59.00 120.00   0.50    0.09    --   46.62 149.00  99.00  122
  8  \w   -171.00 -55.00   0.50    0.37    -- -100.00-149.00  52.00  232
  9  \w   -115.00 -27.00   0.50    0.37    -- -100.00 123.00 -63.00  176
 10  \w   -173.00 -73.00   0.50    0.37    -- -100.00-123.00-143.00  200
 11  \w     34.00 115.00   0.50    0.37    --  107.00-123.00-143.00  162
 12  \w     59.00 172.00   0.50    0.37    --  107.00 149.00  99.00  226
 13  \w     34.00 133.00   0.50    0.37    --  107.00-149.00  52.00  198
 14  \w     77.00 178.00   0.50    0.37    --  107.00 123.00 -63.00  202
 15  \w    -22.00   4.00   0.50    0.09    --   16.00 106.00 165.43   52
 16  \w      9.00  43.00   0.50    0.09    --   40.00  92.00 -77.20   68
 17  \w     14.00  44.00   0.50    0.09    --   44.00  91.00  28.95   60
 18  \w     14.00  45.00   0.50    0.09    --   44.00  90.00 -16.87   62
 19  \w   -119.00 -30.00   0.50    0.09    --  -46.62 -57.00-180.00  178
 20  \w   -119.00 -23.00   0.50    0.09    --  -46.62 -77.00-120.00  192
 21  \w     32.00 120.00   0.50    0.09    --   46.62  38.00 -60.00  176
 22  \w     32.00 120.00   0.50    0.09    --   46.62  38.00  30.00  176
 23  \w     24.00 121.00   0.50    0.09    --   48.00  78.00-168.92  194
 24  \w     18.00  43.00   0.50    0.09    --   48.00  90.00  88.79   50
 25  \w     25.00  77.00   0.50    0.09    --   48.00  80.00-144.97  104
 26  \w     73.00  99.00   0.50    0.09    --   52.00  82.00-107.92   52
 27  \w     26.00  52.00   0.50    0.09    --   52.00  82.00-107.92   52
 28  \w     32.00  67.00   0.50    0.09    --   56.00  78.00  22.19   70
 29  \w     36.00  79.00   0.50    0.09    --   56.00  72.00 153.70   86
 30  \w    -71.00 -45.00   0.50    0.09    --  -60.00 -70.00-106.85   52
 31  \w   -118.00 -92.00   0.50    0.09    --  -60.00 -70.00-106.85   52
 32  \w    -62.00 -36.00   0.50    0.09    --  -60.00 -79.00  65.89   52
 33  \w   -119.00 -93.00   0.50    0.09    --  -60.00 -79.00  65.89   52
 34  \w     37.00  65.00   0.50    0.09    --   60.00  75.00  58.58   56
 35  \w     40.00  73.00   0.50    0.09    --   64.00  78.00 111.23   66
 36  \w    -81.00 -46.00   0.50    0.09    --  -68.00 -73.00  12.68   70
 37  \w    -74.00 -43.00   0.50    0.09    --  -68.00 -83.00  61.40   62
 38  \w    -67.00 -42.00   0.50    0.09    --  -68.00 -81.00-167.34   50
 39  \w    -78.00 -45.00   0.50    0.09    --  -68.00 -75.00 -66.47   66
 40  \w    -73.00 -41.00   0.50    0.09    --  -68.00 -83.00-176.25   64
 41  \w    -86.00 -44.00   0.50    0.09    --  -68.00 -78.00 -28.19   84
 42  \w     42.00  68.00   0.50    0.09    --   68.00  83.00 151.63   52
 43  \w    -77.00 -47.00   0.50    0.09    --  -72.00 -80.00-108.11   60
 44  \w    -70.00 -45.00   0.50    0.09    --  -72.00 -83.00 111.37   50
 45  \w    -79.00 -51.00   0.50    0.09    --  -72.00 -69.00 -86.03   56
 46  \w     49.00  75.00   0.50    0.09    --   72.00  76.00  32.28   52
 47  \w    -80.00 -54.00   0.50    0.37    --  -80.00 -83.00-118.62   52
 48  \w    -83.00 -57.00   0.50    0.37    --  -80.00 -74.00  73.58   52
 49  \w    -79.00 -53.00   0.50    0.37    --  -80.00 -83.00  24.29   52
 50  \w    -85.00 -59.00   0.50    0.37    --  -80.00 -73.00  38.92   52
 51  \w    -90.00 -63.00   0.50    0.37    --  -84.00 -69.00-107.37   54
 52  \w    -96.00 -70.00   0.50    0.37    --  -88.00 -62.00-158.57   52
 53  \w    -97.00 -65.00   0.50    0.37    --  -88.00 -76.00 164.50   64
 54  \w    -90.00 -65.00   0.50    0.37    --  -88.00 -75.00 173.46   50
 55  \w    -91.00 -65.00   0.50    0.37    --  -88.00 -74.00 -55.23   52
 56  \w   -100.00 -72.00   0.50    0.37    --  -92.00 -68.00 -33.46   56
 57  \w    -99.00 -73.00   0.50    0.37    --  -92.00 -65.00 -53.65   52
 58  \w    -98.00 -72.00   0.50    0.37    --  -92.00 -74.00  23.23   52
 59  \w    -99.00 -73.00   0.50    0.37    --  -96.00 -76.00  -2.50   52
 60  \w   -104.00 -76.00   0.50    0.37    --  -96.00 -68.00 152.52   56
 61  \w   -143.00 -76.00   0.50    0.37    --  -96.00 -74.00  67.07  134
 62  \w   -158.00-132.00   0.50    0.37    --  -96.00 -76.00  -2.50   52
 63  \w   -139.00-114.00   0.50    0.37    --  -96.00 -68.00 152.52   50
 64  \w    -95.00 -70.00   0.50    0.37    --  -96.00 -81.00 -62.86   50
 65  \w   -160.00-134.00   0.50    0.37    --  -96.00 -81.00 -62.86   52
 66  \w    -99.00 -73.00   0.50    0.37    --  -96.00 -76.00-118.01   52
 67  \w   -137.00 -78.00   0.50    0.37    -- -100.00 -74.00-178.12  118
 68  \w   -173.00-142.00   0.50    0.37    -- -100.00 -74.00-178.12   62
 69  \w   -122.00 -76.00   0.50    0.37    -- -100.00 -77.00  60.00   92
 70  \w   -131.00 -79.00   0.50    0.37    -- -100.00 -70.00   7.54  104
 71  \w   -103.00 -74.00   0.50    0.37    -- -100.00 -83.00  58.28   58
 72  \w   -171.00 -82.00   0.50    0.37    -- -100.00 -61.00 120.00  178
 73  \w   -103.00 -76.00   0.50    0.37    -- -100.00 -78.00-151.07   54
 74  \w   -164.00-138.00   0.50    0.37    -- -100.00 -78.00-151.07   52
 75  \w   -162.00-126.00   0.50    0.37    -- -100.00 -83.00  58.28   72
 76  \w   -110.00 -74.00   0.50    0.37    -- -100.00 -81.00  87.95   72
 77  \w   -105.00 -76.00   0.50    0.37    -- -100.00 -79.00  13.55   58
 78  \w   -102.00 -76.00   0.50    0.37    -- -100.00 -76.00 125.30   52
 79  \w   -101.00 -76.00   0.50    0.37    -- -100.00 -77.00  30.00   50
 80  \w   -102.00 -76.00   0.50    0.37    -- -100.00 -77.00-120.00   52
 81  \w   -147.00-121.00   0.50    0.37    -- -100.00 -77.00-120.00   52
 82  \w   -115.00 -79.00   0.50    0.37    -- -100.00 -74.00 -11.82   72
 83  \w   -163.00-120.00   0.50    0.37    -- -100.00 -74.00 -11.82   86
 84  \w   -113.00 -79.00   0.50    0.37    -- -100.00 -72.00  93.48   68
 85  \w   -106.00 -80.00   0.50    0.37    -- -100.00 -67.00 -56.69   52
 86  \w   -101.00 -76.00   0.50    0.37    -- -100.00 -76.00 159.92   50
 87  \w   -170.00 -76.00   0.50    0.37    -- -100.00 -77.00  90.00  188
 88  \w   -102.00 -76.00   0.50    0.37    -- -100.00 -77.00 -90.00   52
 89  \w   -144.00-118.00   0.50    0.37    -- -100.00 -76.00 159.92   52
 90  \w   -172.00-106.00   0.50    0.37    -- -100.00 -94.00-120.00  132
 91  \w   -164.00-139.00   0.50    0.37    -- -100.00 -77.00 -90.00   50
 92  \w   -106.00 -80.00   0.50    0.37    -- -100.00 -73.00-164.61   52
 93  \w   -124.00 -98.00   0.50    0.37    -- -100.00 -62.00 -94.97   52
 94  \w   -173.00-109.00   0.50    0.37    -- -100.00 -73.00-164.61  128
 95  \w   -172.00 -79.00   0.50    0.37    -- -100.00 -70.00 142.79  186
 96  \w   -173.00-130.00   0.50    0.37    -- -100.00 -62.00 -94.97   86
 97  \w   -111.00 -81.00   0.50    0.37    -- -100.00 -65.00-115.70   60
 98  \w   -102.00 -77.00   0.50    0.37    -- -100.00 -75.00 -37.77   50
 99  \w   -167.00-106.00   0.50    0.37    -- -100.00 -75.00 -37.77  122
100  \w   -104.00 -79.00   0.50    0.37    -- -100.00 149.00  99.00   50
101  \w   -103.00 -77.00   0.50    0.37    -- -100.00 -78.00 115.15   52
102  \w     90.00 177.00   0.50    0.37    --  107.00  61.00-120.00  174
103  \w     34.00  82.00   0.50    0.37    --  107.00 -94.00  30.00   96
104  \w    114.00 145.00   0.50    0.37    --  107.00  30.00  90.00   62
105  \w     34.00  94.00   0.50    0.37    --  107.00 -61.00-150.00  120
106  \w     83.00 108.00   0.50    0.37    --  107.00 -94.00  90.00   50
107  \w     34.00  79.00   0.50    0.37    --  107.00 -94.00  90.00   90
108  \w     84.00 177.00   0.50    0.37    --  107.00  77.00 -30.00  186
109  \w     84.00 117.00   0.50    0.37    --  107.00-125.00 -30.00   66
110  \w     37.00  79.00   0.50    0.37    --  107.00-125.00 -30.00   84
111  \w    106.00 131.00   0.50    0.37    --  107.00 -77.00 120.00   50
112  \w     35.00  92.00   0.50    0.37    --  107.00 -77.00 120.00  114
113  \w    121.00 166.00   0.50    0.37    --  107.00  77.00-150.00   90
114  \w     83.00 112.00   0.50    0.37    --  107.00  77.00-150.00   58
115  \w     90.00 116.00   0.50    0.37    --  107.00-125.00 -60.00   52
116  \w     38.00  64.00   0.50    0.37    --  107.00-125.00 -60.00   52
117  \w     75.00 101.00   0.50    0.37    --  107.00 -94.00 120.00   52
118  \w     34.00  98.00   0.50    0.37    --  107.00 -61.00 -60.00  128
119  \w     38.00  69.00   0.50    0.37    --  107.00 -94.00 120.00   62
120  \w     85.00 162.00   0.50    0.37    --  107.00  77.00   0.00  154
121  \w     71.00 108.00   0.50    0.37    --  107.00 -94.00  60.00   74
122  \w    140.00 170.00   0.50    0.37    --  107.00  77.00 -90.00   60
123  \w     84.00 125.00   0.50    0.37    --  107.00  77.00 -90.00   82
124  \w     37.00  65.00   0.50    0.37    --  107.00 -94.00  60.00   56
;
_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      0.1674044000
_diffrn_orient_matrix_UB_12      0.0915689000
_diffrn_orient_matrix_UB_13      0.0299380000
_diffrn_orient_matrix_UB_21      -0.0198104000
_diffrn_orient_matrix_UB_22      0.0059289000
_diffrn_orient_matrix_UB_23      0.1208206000
_diffrn_orient_matrix_UB_31      0.0650083000
_diffrn_orient_matrix_UB_32      -0.1355260000
_diffrn_orient_matrix_UB_33      0.0113544000
_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  0.0559
_diffrn_reflns_av_unetI/netI     0.0237
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.975
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_number            40850
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.975
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         77.110
_diffrn_reflns_theta_min         3.586
_diffrn_source                   'Rotating-anode X-ray tube'
_diffrn_source_type              'Rigaku (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    2.013
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.42500
_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    1.446
_exptl_crystal_description       block
_exptl_crystal_F_000             468
_exptl_crystal_recrystallization_method 'From the Melt'
_exptl_crystal_size_max          0.2
_exptl_crystal_size_mid          0.15
_exptl_crystal_size_min          0.1
_refine_diff_density_max         0.271
_refine_diff_density_min         -0.348
_refine_diff_density_rms         0.051
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.089
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     281
_refine_ls_number_reflns         4234
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.089
_refine_ls_R_factor_all          0.0362
_refine_ls_R_factor_gt           0.0340
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0484P)^2^+0.3245P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0908
_refine_ls_wR_factor_ref         0.0925
_reflns_Friedel_coverage         0.000
_reflns_number_gt                3892
_reflns_number_total             4234
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d0cc03157g2.cif
_cod_data_source_block           Gefitinib-100k-XOu
_cod_depositor_comments
'Adding full bibliography for 7126896--7126915.cif.'
_cod_database_code               7126898
_shelx_shelxl_version_number     2016/6
_reflns_odcompleteness_completeness 99.98
_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
2.a Secondary CH2 refined with riding coordinates:
 C00G(H00A,H00B), C00N(H00C,H00D), C00O(H00E,H00G), C00Q(H00I,H00J), C00S(H00Q,
 H00R), C00T(H00S,H00T), C00V(H00V,H00W)
2.b Aromatic/amide H refined with riding coordinates:
 N008(H008), C00F(H00F), C00H(H00H), C00K(H00K), C00M(H00M), C00P(H00P),
 C00U(H00U)
2.c Idealised Me refined as rotating group:
 C00R(H00L,H00N,H00O)
;
_shelx_res_checksum              88353
_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 3.155
_oxdiff_exptl_absorpt_empirical_full_min 0.536