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_7126896
_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 H17 Cl O6'
_chemical_formula_sum            'C17 H17 Cl O6'
_chemical_formula_weight         352.76
_chemical_melting_point          488
_chemical_name_common            griseofulvin
_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             2019-04-17
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_audit_update_record
;
2019-05-24 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            8
_cell_length_a                   11.6345(2)
_cell_length_b                   12.0011(3)
_cell_length_c                   23.8695(5)
_cell_measurement_reflns_used    28350
_cell_measurement_temperature    100.00(10)
_cell_measurement_theta_max      77.0370
_cell_measurement_theta_min      3.7030
_cell_volume                     3332.82(12)
_computing_cell_refinement       'CrysAlisPro 1.171.39.46 (Rigaku OD, 2018)'
_computing_data_collection       'CrysAlisPro 1.171.39.46 (Rigaku OD, 2018)'
_computing_data_reduction        'CrysAlisPro 1.171.39.46 (Rigaku OD, 2018)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_computing_structure_solution    'ShelXT (Sheldrick, 2015)'
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      100.00(10)
_diffrn_detector                 'CCD plate'
_diffrn_detector_type            HyPix
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.988
_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    0.07    --   46.62 -35.00-105.00  176
  2  \w   -173.00 -81.00   0.50    0.42    -- -100.00 -93.00  62.00  184
  3  \w     85.00 178.00   0.50    0.42    --  107.00 108.00 -97.00  186
  4  \w     33.00 122.00   0.50    0.42    --  107.00 -35.00-105.00  178
  5  \w   -120.00 -32.00   0.50    0.07    --  -46.62 -38.00-180.00  176
  6  \w   -119.00 -71.00   0.50    0.07    --  -46.62-125.00 -30.00   96
  7  \w   -119.00 -71.00   0.50    0.07    --  -46.62-125.00-120.00   96
  8  \w   -119.00 -71.00   0.50    0.07    --  -46.62-125.00 -90.00   96
  9  \w     34.00 109.00   0.50    0.42    --  107.00 -94.00 -30.00  150
 10  \w     89.00 178.00   0.50    0.42    --  107.00  15.00 150.00  178
 11  \w     93.00 178.00   0.50    0.42    --  107.00  45.00  90.00  170
 12  \w     83.00 178.00   0.50    0.42    --  107.00  77.00-150.00  190
 13  \w     31.00 125.00   0.50    0.42    --  107.00 -15.00 120.00  188
 14  \w     34.00 125.00   0.50    0.42    --  107.00 -61.00  60.00  182
 15  \w     34.00 131.00   0.50    0.42    --  107.00 -77.00 150.00  194
 16  \w     34.00 125.00   0.50    0.42    --  107.00 -61.00 150.00  182
 17  \w   -119.00 -23.00   0.50    0.07    --  -46.62 -77.00   0.00  192
;
_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      0.0591749000
_diffrn_orient_matrix_UB_12      0.0507000000
_diffrn_orient_matrix_UB_13      0.0518285000
_diffrn_orient_matrix_UB_21      -0.1071653000
_diffrn_orient_matrix_UB_22      -0.0262328000
_diffrn_orient_matrix_UB_23      0.0355439000
_diffrn_orient_matrix_UB_31      0.0505420000
_diffrn_orient_matrix_UB_32      -0.1149746000
_diffrn_orient_matrix_UB_33      0.0146797000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0429
_diffrn_reflns_av_unetI/netI     0.0295
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.988
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       28
_diffrn_reflns_limit_l_min       -29
_diffrn_reflns_number            34215
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.981
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         77.197
_diffrn_reflns_theta_min         3.704
_diffrn_source                   'Rotating-anode X-ray tube'
_diffrn_source_type              'Rigaku (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    2.305
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.81011
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.39.46 (Rigaku Oxford Diffraction, 2018)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            'clear light colourless'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   light
_exptl_crystal_colour_primary    colourles
_exptl_crystal_density_diffrn    1.406
_exptl_crystal_description       block
_exptl_crystal_F_000             1472
_exptl_crystal_recrystallization_method 'From the Melt'
_exptl_crystal_size_max          0.2
_exptl_crystal_size_mid          0.15
_exptl_crystal_size_min          0.05
_refine_diff_density_max         0.176
_refine_diff_density_min         -0.258
_refine_diff_density_rms         0.045
_refine_ls_abs_structure_details
;
 Flack x determined using 2904 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   -0.009(4)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.044
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     441
_refine_ls_number_reflns         6937
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.044
_refine_ls_R_factor_all          0.0289
_refine_ls_R_factor_gt           0.0281
_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^)+(0.0404P)^2^+0.7341P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0720
_refine_ls_wR_factor_ref         0.0726
_reflns_Friedel_coverage         0.771
_reflns_Friedel_fraction_full    1.000
_reflns_Friedel_fraction_max     0.973
_reflns_number_gt                6785
_reflns_number_total             6937
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d0cc03157g2.cif
_cod_data_source_block           GSF-II-100K-XOu
_cod_depositor_comments
;
The following automatic conversions were performed:

data item '_chemical_melting_point' value '488k' was changed to '488'
-- 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               7126896
_shelx_shelxl_version_number     2016/6
_reflns_odcompleteness_completeness 99.97
_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
 At 1.5 times of:
  All C(H,H,H) groups
2.a Ternary CH refined with riding coordinates:
 C00W(H00W), C014(H014)
2.b Secondary CH2 refined with riding coordinates:
 C00Z(H00D,H00E), C019(H01P,H01Q)
2.c Aromatic/amide H refined with riding coordinates:
 C00G(H00G), C00H(H00H), C00Y(H00Y), C010(H010)
2.d Idealised Me refined as rotating group:
 C00R(H00A,H00B,H00C), C013(H01A,H01B,H01C), C015(H01J,H01K,H01L), C017(H01D,
 H01E,H01F), C018(H01M,H01N,H01O), C01A(H01R,H01S,H01T), C01B(H01G,H01H,H01I),
 C01C(H01U,H01V,H01W)
;
_shelx_res_checksum              66598
_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 1.341
_oxdiff_exptl_absorpt_empirical_full_min 0.738