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_7126913
_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         'C8 H9 N O2'
_chemical_formula_sum            'C8 H9 N O2'
_chemical_formula_weight         151.16
_chemical_melting_point          444
_chemical_name_common            Paracetamol
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2yn'
_space_group_name_H-M_alt        'P 1 21/n 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                 97.8900(10)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   7.08950(10)
_cell_length_b                   9.21120(10)
_cell_length_c                   11.59660(10)
_cell_measurement_reflns_used    12179
_cell_measurement_temperature    100.01(10)
_cell_measurement_theta_max      75.6850
_cell_measurement_theta_min      3.8260
_cell_volume                     750.122(15)
_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 1.000
_diffrn_measured_fraction_theta_max 0.969
_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    -92.00  -7.00   0.50    0.05    --  -46.62 119.00-170.00  170
  2  \w     54.00 120.00   0.50    0.05    --   46.62 156.00 -14.00  132
  3  \w     79.00 178.00   0.50    0.05    --  105.44 119.00-170.00  198
  4  \w     90.00 178.00   0.50    0.05    --  105.44  30.00 120.00  176
  5  \w     31.00 114.00   0.50    0.05    --   46.62-156.00 -51.00  166
  6  \w     33.00 138.00   0.50    0.05    --  105.44-156.00 -51.00  210
  7  \w     33.00 113.00   0.50    0.05    --  105.44-119.00 104.00  160
  8  \w     33.00 129.00   0.50    0.05    --  105.44 -77.00  90.00  192
  9  \w     33.00 108.00   0.50    0.05    --  105.44 -94.00 -60.00  150
 10  \w     33.00 123.00   0.50    0.05    --  105.44 -61.00  60.00  180
 11  \w     33.00 108.00   0.50    0.05    --  105.44 -94.00 -30.00  150
 12  \w     11.00  92.00   0.50    0.05    --   46.62-119.00 104.00  162
 13  \w   -119.00 -50.00   0.50    0.05    --  -46.62-156.00 -51.00  138
 14  \w   -113.00 -27.00   0.50    0.05    -- -100.00 119.00-170.00  172
 15  \w   -115.00 -25.00   0.50    0.05    -- -100.00  30.00-120.00  180
 16  \w   -119.00 -23.00   0.50    0.05    --  -46.62 -77.00  30.00  192
 17  \w   -119.00 -23.00   0.50    0.05    --  -46.62 -77.00 120.00  192
 18  \w   -119.00 -71.00   0.50    0.05    --  -46.62-125.00  30.00   96
 19  \w   -119.00 -30.00   0.50    0.05    --  -46.62 -57.00 -60.00  178
 20  \w   -119.00 -71.00   0.50    0.05    --  -46.62-125.00-180.00   96
 21  \w   -119.00 -23.00   0.50    0.05    --  -46.62 -77.00-120.00  192
 22  \w   -117.00 -27.00   0.50    0.05    -- -100.00  61.00  30.00  180
 23  \w   -119.00 -74.00   0.50    0.05    --  -46.62 -57.00 150.00   90
 24  \w   -173.00 -75.00   0.50    0.05    -- -100.00-119.00 104.00  196
 25  \w   -166.00 -50.00   0.50    0.05    -- -100.00-156.00 -51.00  232
 26  \w   -173.00 -71.00   0.50    0.05    -- -100.00-125.00 150.00  204
 27  \w   -172.00 -85.00   0.50    0.05    -- -100.00 -45.00   0.00  174
 28  \w   -172.00 -85.00   0.50    0.05    -- -100.00 -45.00 -90.00  174
 29  \w   -173.00 -81.00   0.50    0.05    -- -100.00 -94.00-150.00  184
 30  \w   -137.00 -27.00   0.50    0.05    -- -100.00 156.00 -14.00  220
;
_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      -0.0294235000
_diffrn_orient_matrix_UB_12      -0.1395671000
_diffrn_orient_matrix_UB_13      0.0685580000
_diffrn_orient_matrix_UB_21      -0.0905237000
_diffrn_orient_matrix_UB_22      0.0899099000
_diffrn_orient_matrix_UB_23      0.0901268000
_diffrn_orient_matrix_UB_31      -0.1975441000
_diffrn_orient_matrix_UB_32      -0.0203639000
_diffrn_orient_matrix_UB_33      -0.0719463000
_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  0.0360
_diffrn_reflns_av_unetI/netI     0.0146
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.969
_diffrn_reflns_limit_h_max       8
_diffrn_reflns_limit_h_min       -8
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_l_max       14
_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_number            13453
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.969
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         76.038
_diffrn_reflns_theta_min         6.159
_diffrn_source                   'Rotating-anode X-ray tube'
_diffrn_source_type              'Rigaku (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    0.803
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.69621
_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    1.339
_exptl_crystal_description       block
_exptl_crystal_F_000             320
_exptl_crystal_recrystallization_method 'From the Melt'
_exptl_crystal_size_max          0.14
_exptl_crystal_size_mid          0.1
_exptl_crystal_size_min          0.05
_refine_diff_density_max         0.288
_refine_diff_density_min         -0.437
_refine_diff_density_rms         0.133
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.125
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     102
_refine_ls_number_reflns         1527
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.125
_refine_ls_R_factor_all          0.0433
_refine_ls_R_factor_gt           0.0424
_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^)+(0.0645P)^2^+0.2877P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1125
_refine_ls_wR_factor_ref         0.1137
_reflns_Friedel_coverage         0.000
_reflns_number_gt                1477
_reflns_number_total             1527
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d0cc03157g2.cif
_cod_data_source_block           Paracetamol-100k-XOu
_cod_depositor_comments
;
The following automatic conversions were performed:

data item '_chemical_melting_point' value '444K' was changed to '444'
-- 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               7126913
_shelx_shelxl_version_number     2016/6
_reflns_odcompleteness_completeness 100.00
_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) 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:
 N003(H003), C006(H006), C008(H008), C009(H009), C00A(H00A)
2.b Idealised Me refined as rotating group:
 C00B(H00B,H00C,H00D)
2.c Idealised tetrahedral OH refined as rotating group:
 O001(H001)
;
_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 1.469
_oxdiff_exptl_absorpt_empirical_full_min 0.590