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_7126910
_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         'C17 H14 F3 N3 O2 S'
_chemical_formula_sum            'C17 H14 F3 N3 O2 S'
_chemical_formula_weight         381.37
_chemical_melting_point          436
_chemical_name_common            Celecoxib
_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   mixed
_atom_sites_solution_primary     dual
_audit_creation_date             2019-12-27
_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                89.8820(10)
_cell_angle_beta                 85.8650(10)
_cell_angle_gamma                80.5380(10)
_cell_formula_units_Z            2
_cell_length_a                   5.06400(10)
_cell_length_b                   10.01390(10)
_cell_length_c                   16.40730(10)
_cell_measurement_reflns_used    24344
_cell_measurement_temperature    100.01(10)
_cell_measurement_theta_max      75.9500
_cell_measurement_theta_min      2.7020
_cell_volume                     818.524(19)
_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 0.999
_diffrn_measured_fraction_theta_max 0.942
_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     31.00 122.00   0.50    0.05    --   46.37  19.00 -90.00  182
  2  \w     65.00  91.00   0.50    0.05    --   80.00  71.00   1.35   52
  3  \w     60.00  86.00   0.50    0.05    --   84.00  82.00 -50.78   52
  4  \w     64.00 118.00   0.50    0.05    --   46.37 143.00   9.00  108
  5  \w     64.00 175.00   0.50    0.05    --  105.44 143.00   9.00  222
  6  \w     74.00 178.00   0.50    0.05    --  105.44 127.00-159.00  208
  7  \w     81.00 107.00   0.50    0.05    --  105.44 -45.00  90.00   52
  8  \w     38.00  79.00   0.50    0.05    --  105.44 -45.00  90.00   82
  9  \w     16.00  96.00   0.50    0.05    --   46.37-127.00 124.00  160
 10  \w     33.00 118.00   0.50    0.05    --  105.44-127.00 124.00  170
 11  \w     25.00 106.00   0.50    0.05    --   46.37-143.00 -44.00  162
 12  \w     33.00 130.00   0.50    0.05    --  105.44-143.00 -44.00  194
 13  \w     33.00 106.00   0.50    0.05    --  105.44 -94.00 -30.00  146
 14  \w     32.00 120.00   0.50    0.05    --   46.37  38.00 120.00  176
 15  \w     39.00  65.00   0.50    0.05    --   64.00  79.00 172.52   52
 16  \w     24.00 121.00   0.50    0.05    --   48.00  78.00 129.92  194
 17  \w     30.00 118.00   0.50    0.05    --   46.37  57.00 -60.00  176
 18  \w     36.00 132.00   0.50    0.05    --   60.00  77.00 -23.59  192
 19  \w     39.00 132.00   0.50    0.05    --   60.00  71.00-111.06  186
 20  \w     32.00 120.00   0.50    0.05    --   46.37  38.00 -90.00  176
 21  \w     34.00 129.00   0.50    0.05    --   56.00  73.00-100.10  190
 22  \w     23.00 118.00   0.50    0.05    --   46.37  77.00   0.00  190
 23  \w     23.00 118.00   0.50    0.05    --   46.37  77.00  60.00  190
 24  \w     31.00 125.00   0.50    0.05    --   52.00  70.00 103.45  188
 25  \w     33.00 129.00   0.50    0.05    --   56.00  76.00 -72.86  192
 26  \w     23.00 118.00   0.50    0.05    --   46.37  77.00-180.00  190
 27  \w     -3.00  24.00   0.50    0.05    --   32.00 100.00 -50.70   54
 28  \w    -39.00 -13.00   0.50    0.05    --   12.00 129.00 -53.62   52
 29  \w    -96.00 -12.00   0.50    0.05    --  -46.37 127.00-159.00  168
 30  \w    -59.00 -31.00   0.50    0.05    -- -100.00  61.00  60.00   56
 31  \w   -100.00 -66.00   0.50    0.05    -- -100.00  61.00  60.00   68
 32  \w   -113.00 -27.00   0.50    0.05    -- -100.00  45.00  60.00  172
 33  \w   -105.00 -20.00   0.50    0.05    --  -46.37 143.00   9.00  170
 34  \w   -103.00 -78.00   0.50    0.05    -- -100.00 143.00   9.00   50
 35  \w   -115.00 -29.00   0.50    0.05    -- -100.00  61.00-120.00  172
 36  \w   -118.00 -27.00   0.50    0.05    -- -100.00 127.00-159.00  182
 37  \w    -87.00 -61.00   0.50    0.05    --  -76.00 -57.00 -20.88   52
 38  \w    -80.00 -54.00   0.50    0.05    --  -80.00 -82.00 -33.81   52
 39  \w    -67.00 -41.00   0.50    0.05    --  -64.00 -76.00 -75.65   52
 40  \w    -70.00 -44.00   0.50    0.05    --  -64.00 -68.00-116.04   52
 41  \w    -73.00 -47.00   0.50    0.05    --  -64.00 -65.00-141.10   52
 42  \w    -73.00 -47.00   0.50    0.05    --  -68.00 -79.00-159.48   52
 43  \w    -80.00 -54.00   0.50    0.05    --  -76.00 -72.00 -81.02   52
 44  \w    -83.00 -57.00   0.50    0.05    --  -80.00 -76.00-116.61   52
 45  \w    -95.00 -69.00   0.50    0.05    --  -84.00 -59.00-106.65   52
 46  \w   -101.00 -73.00   0.50    0.05    --  -88.00 -55.00 -29.51   56
 47  \w    -95.00 -50.00   0.50    0.05    --  -68.00 -62.00  26.21   90
 48  \w    -81.00 -55.00   0.50    0.05    --  -72.00 -61.00  41.68   52
 49  \w    -86.00 -60.00   0.50    0.05    --  -76.00 -60.00  55.48   52
 50  \w    -76.00 -50.00   0.50    0.05    --  -76.00 -81.00  48.70   52
 51  \w    -69.00 -39.00   0.50    0.05    --  -64.00 -81.00 128.81   60
 52  \w    -74.00 -48.00   0.50    0.05    --  -68.00 -68.00 155.08   52
 53  \w    -72.00 -46.00   0.50    0.05    --  -72.00 -83.00 162.30   52
 54  \w    -87.00 -53.00   0.50    0.05    --  -76.00 -76.00  95.11   68
 55  \w    -95.00 -56.00   0.50    0.05    --  -80.00 -78.00  29.13   78
 56  \w   -104.00 -74.00   0.50    0.05    --  -92.00 -63.00  71.54   60
 57  \w   -101.00 -76.00   0.50    0.05    -- -100.00 -77.00 120.00   50
 58  \w    -88.00 -62.00   0.50    0.05    --  -84.00 -72.00 146.09   52
 59  \w    -92.00 -66.00   0.50    0.05    --  -84.00 -65.00 147.74   52
 60  \w    -96.00 -70.00   0.50    0.05    --  -84.00 -61.00 168.18   52
 61  \w    -97.00 -71.00   0.50    0.05    --  -88.00 -59.00 177.88   52
 62  \w    -97.00 -71.00   0.50    0.05    --  -88.00 -62.00 158.43   52
 63  \w   -102.00 -73.00   0.50    0.05    --  -96.00 -76.00 146.49   58
 64  \w   -102.00 -76.00   0.50    0.05    -- -100.00 -77.00  90.00   52
 65  \w   -120.00 -78.00   0.50    0.05    -- -100.00 -74.00 172.02   84
 66  \w   -114.00 -84.00   0.50    0.05    -- -100.00 -64.00  89.70   60
 67  \w   -112.00 -76.00   0.50    0.05    -- -100.00 -77.00  30.00   72
 68  \w   -111.00 -72.00   0.50    0.05    --  -96.00 -77.00 -27.92   78
 69  \w   -109.00 -76.00   0.50    0.05    -- -100.00 -77.00 -60.00   66
 70  \w   -101.00 -76.00   0.50    0.05    -- -100.00 -77.00-120.00   50
 71  \w   -108.00 -81.00   0.50    0.05    -- -100.00 -72.00-178.91   54
 72  \w   -124.00 -75.00   0.50    0.05    --  -92.00 -59.00-161.93   98
 73  \w   -118.00 -23.00   0.50    0.05    --  -46.37 -77.00-150.00  190
 74  \w   -118.00 -59.00   0.50    0.05    --  -46.37-143.00 -44.00  118
 75  \w   -121.00 -77.00   0.50    0.05    --  -92.00 -57.00-112.04   88
 76  \w   -132.00 -35.00   0.50    0.05    --  -60.00 -80.00 -93.63  194
 77  \w   -124.00 -78.00   0.50    0.05    -- -100.00 -72.00  31.31   92
 78  \w   -118.00 -70.00   0.50    0.05    --  -46.37-127.00 124.00   96
 79  \w   -133.00 -84.00   0.50    0.05    -- -100.00 -59.00 115.49   98
 80  \w   -148.00-110.00   0.50    0.05    --  -88.00 -55.00 -29.51   76
 81  \w   -153.00 -75.00   0.50    0.05    -- -100.00 -79.00 -46.29  156
 82  \w   -132.00 -35.00   0.50    0.05    --  -60.00 -80.00-178.29  194
 83  \w   -164.00-115.00   0.50    0.05    --  -92.00 -63.00  71.54   98
 84  \w   -169.00-110.00   0.50    0.05    --  -96.00 -76.00 146.49  118
 85  \w   -173.00 -70.00   0.50    0.05    -- -100.00-127.00 124.00  206
 86  \w   -173.00 -59.00   0.50    0.05    -- -100.00-143.00 -44.00  228
 87  \w   -163.00-131.00   0.50    0.05    --  -92.00 -59.00-161.93   64
 88  \w   -157.00 -82.00   0.50    0.05    -- -100.00 -61.00-180.00  150
 89  \w   -164.00 -76.00   0.50    0.05    --  -92.00 -56.00-134.11  176
 90  \w   -168.00 -78.00   0.50    0.05    --  -96.00 -66.00  52.63  180
 91  \w   -168.00-126.00   0.50    0.05    --  -96.00 -77.00 -27.92   84
 92  \w   -172.00 -78.00   0.50    0.05    -- -100.00 -77.00   0.00  188
 93  \w   -172.00-122.00   0.50    0.05    -- -100.00 -77.00 120.00  100
;
_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      -0.0008649000
_diffrn_orient_matrix_UB_12      0.0448571000
_diffrn_orient_matrix_UB_13      0.0897908000
_diffrn_orient_matrix_UB_21      0.0141808000
_diffrn_orient_matrix_UB_22      0.1458530000
_diffrn_orient_matrix_UB_23      -0.0277923000
_diffrn_orient_matrix_UB_31      -0.3089066000
_diffrn_orient_matrix_UB_32      0.0322829000
_diffrn_orient_matrix_UB_33      0.0053300000
_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  0.0374
_diffrn_reflns_av_unetI/netI     0.0164
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.942
_diffrn_reflns_limit_h_max       5
_diffrn_reflns_limit_h_min       -6
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            28889
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.942
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         76.107
_diffrn_reflns_theta_min         2.700
_diffrn_source                   'Rotating-anode X-ray tube'
_diffrn_source_type              'Rigaku (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    2.230
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.40314
_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    1.547
_exptl_crystal_description       block
_exptl_crystal_F_000             392
_exptl_crystal_recrystallization_method 'From the Melt'
_exptl_crystal_size_max          0.85
_exptl_crystal_size_mid          0.06
_exptl_crystal_size_min          0.05
_refine_diff_density_max         0.391
_refine_diff_density_min         -0.468
_refine_diff_density_rms         0.067
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.067
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     242
_refine_ls_number_reflns         3225
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.067
_refine_ls_R_factor_all          0.0374
_refine_ls_R_factor_gt           0.0351
_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^)+(0.0438P)^2^+0.6454P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0885
_refine_ls_wR_factor_ref         0.0899
_reflns_Friedel_coverage         0.000
_reflns_number_gt                3162
_reflns_number_total             3225
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d0cc03157g2.cif
_cod_data_source_block           Celecoxib-100k-XOu
_cod_depositor_comments
;
The following automatic conversions were performed:

data item '_chemical_melting_point' value '436K' was changed to '436'
-- 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               7126910
_shelx_shelxl_version_number     2016/6
_reflns_odcompleteness_completeness 99.97
_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 N(H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2.a Aromatic/amide H refined with riding coordinates:
 C00C(H00C), C00D(H00D), C00E(H00E), C00F(H00F), C00G(H00G), C00J(H00J),
 C00K(H00K), C00N(H00N), C00P(H00P)
2.b Idealised Me refined as rotating group:
 C00M(H00H,H00I,H00L)
;
_shelx_res_checksum              81812
_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 2.285
_oxdiff_exptl_absorpt_empirical_full_min 0.540