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_7126897
_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         'C21 H19 F N6 O2'
_chemical_formula_sum            'C21 H19 F N6 O2'
_chemical_formula_weight         406.42
_chemical_name_common            Lorlatinib
_space_group_crystal_system      orthorhombic
_space_group_IT_number           61
_space_group_name_Hall           '-P 2ac 2ab'
_space_group_name_H-M_alt        'P b c a'
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     dual
_audit_creation_date             2020-06-27
_audit_creation_method
;
Olex2 1.3
(compiled 2020.02.04 svn.rd84adfe8 for OlexSys, GUI svn.r6032)
;
_audit_update_record
;
2020-06-27 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                   13.16690(10)
_cell_length_b                   15.49550(10)
_cell_length_c                   18.85980(10)
_cell_measurement_reflns_used    17053
_cell_measurement_temperature    297.99(15)
_cell_measurement_theta_max      76.7220
_cell_measurement_theta_min      4.6850
_cell_volume                     3847.92(4)
_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 2018/3 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT 2018/2 (Sheldrick, 2018)'
_diffrn_ambient_environment      air
_diffrn_ambient_temperature      297.99(15)
_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 0.991
_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    3.94    --   46.62 -38.00 120.00  176
  2  \w     89.00 178.00   0.50   15.76    --  107.00  15.00  20.00  178
  3  \w     89.00 178.00   0.50   15.76    --  107.00  15.00  90.00  178
  4  \w     83.00 178.00   0.50   15.76    --  107.00  77.00-120.00  190
  5  \w     62.00 120.00   0.50    3.94    --   46.62 145.00-109.00  116
  6  \w     34.00 112.00   0.50   15.76    --  107.00-112.00  88.00  156
  7  \w     34.00 131.00   0.50   15.76    --  107.00 -77.00 120.00  194
  8  \w     34.00 125.00   0.50   15.76    --  107.00 -61.00 -90.00  182
  9  \w     34.00 109.00   0.50   15.76    --  107.00 -94.00  90.00  150
 10  \w     34.00 117.00   0.50   15.76    --  107.00-125.00  90.00  166
 11  \w     34.00 131.00   0.50   15.76    --  107.00 -77.00 150.00  194
 12  \w    -28.00  64.00   0.50    3.94    --   46.62 -15.00-149.00  184
 13  \w     32.00 123.00   0.50   15.76    --  107.00 -30.00-150.00  182
 14  \w     23.00 120.00   0.50    3.94    --   46.62  77.00-150.00  194
 15  \w   -119.00 -71.00   0.50    3.94    --  -46.62-125.00 120.00   96
 16  \w   -119.00 -71.00   0.50    3.94    --  -46.62-125.00-150.00   96
 17  \w   -130.00 -27.00   0.50   15.76    -- -100.00 145.00-109.00  206
;
_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      -0.0842203000
_diffrn_orient_matrix_UB_12      0.0685322000
_diffrn_orient_matrix_UB_13      -0.0068296000
_diffrn_orient_matrix_UB_21      -0.0808305000
_diffrn_orient_matrix_UB_22      -0.0695423000
_diffrn_orient_matrix_UB_23      0.0150619000
_diffrn_orient_matrix_UB_31      0.0079794000
_diffrn_orient_matrix_UB_32      0.0188981000
_diffrn_orient_matrix_UB_33      0.0799679000
_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  0.0275
_diffrn_reflns_av_unetI/netI     0.0164
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.991
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            36896
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.991
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         76.997
_diffrn_reflns_theta_min         4.689
_diffrn_source                   'Rotating-anode X-ray tube'
_diffrn_source_type              'Rigaku (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    0.841
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.70242
_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_colour_lustre     clear
_exptl_crystal_density_diffrn    1.403
_exptl_crystal_description       block
_exptl_crystal_F_000             1696
_exptl_crystal_size_max          0.17
_exptl_crystal_size_mid          0.1
_exptl_crystal_size_min          0.05
_refine_diff_density_max         0.306
_refine_diff_density_min         -0.346
_refine_diff_density_rms         0.035
_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     275
_refine_ls_number_reflns         4036
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.061
_refine_ls_R_factor_all          0.0500
_refine_ls_R_factor_gt           0.0422
_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^)+(0.0668P)^2^+0.9995P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1231
_refine_ls_wR_factor_ref         0.1302
_reflns_Friedel_coverage         0.000
_reflns_number_gt                3345
_reflns_number_total             4036
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d0cc03157g2.cif
_cod_data_source_block           '_Lorlatinib-298k-XOu'
_cod_depositor_comments
'Adding full bibliography for 7126896--7126915.cif.'
_cod_database_code               7126897
_shelx_shelxl_version_number     2018/3
_reflns_odcompleteness_completeness 100.00
_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,H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2.a Rotating group:
 N007(H00A,H00B)
2.b Ternary CH refined with riding coordinates:
 C00J(H00J)
2.c Secondary CH2 refined with riding coordinates:
 C00K(H00D,H00E)
2.d Aromatic/amide H refined with riding coordinates:
 C00C(H00C), C00M(H00M), C00O(H00O), C00Q(H00Q), C00R(H00R)
2.e Idealised Me refined as rotating group:
 C00S(H00F,H00G,H00H), C00T(H00I,H00K,H00L), C00U(H00N,H00P,H00S)
;
_shelx_res_checksum              19638
_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 1.354
_oxdiff_exptl_absorpt_empirical_full_min 0.787