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_7126899
_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         'C21 H22 Cl2 F N5 O'
_chemical_formula_sum            'C21 H22 Cl2 F N5 O'
_chemical_formula_weight         450.33
_chemical_melting_point          478
_chemical_name_common            Crizotinib
_space_group_crystal_system      monoclinic
_space_group_IT_number           5
_space_group_name_Hall           'C 2y'
_space_group_name_H-M_alt        'C 1 2 1'
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     dual
_audit_creation_date             2019-08-01
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_audit_update_record
;
2019-08-06 deposited with the CCDC.	2020-07-13 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 100.491(3)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   15.2412(4)
_cell_length_b                   10.1051(3)
_cell_length_c                   14.0138(4)
_cell_measurement_reflns_used    5985
_cell_measurement_temperature    100.00(10)
_cell_measurement_theta_max      74.6810
_cell_measurement_theta_min      3.1950
_cell_volume                     2122.24(11)
_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 0.982
_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      2.00  86.00   0.50    0.55    --   46.12-108.00 -50.00  168
  2  \w     34.00 111.00   0.50    6.50    --  107.00-108.00 -50.00  154
  3  \w     34.00 109.00   0.50    6.50    --  107.00 -94.00-180.00  150
  4  \w     34.00 117.00   0.50    6.50    --  107.00-125.00-180.00  166
  5  \w     34.00 109.00   0.50    6.50    --  107.00 -94.00 -30.00  150
  6  \w     34.00 117.00   0.50    6.50    --  107.00-125.00 150.00  166
  7  \w     85.00 178.00   0.50    6.50    --  107.00 108.00  46.00  186
  8  \w     76.00 168.00   0.50    6.50    --  107.00 125.00  90.00  184
  9  \w     93.00 178.00   0.50    6.50    --  107.00  45.00-180.00  170
 10  \w    -85.00   2.00   0.50    0.55    --  -46.12 108.00  46.00  174
 11  \w   -110.00 -27.00   0.50    6.50    -- -100.00 108.00  46.00  166
 12  \w   -115.00 -25.00   0.50    6.50    -- -100.00  30.00  90.00  180
 13  \w   -114.00 -27.00   0.50    6.50    -- -100.00  45.00 -90.00  174
 14  \w   -118.00 -71.00   0.50    0.55    --  -46.12-125.00  60.00   94
 15  \w   -118.00 -71.00   0.50    0.55    --  -46.12-125.00 -30.00   94
 16  \w   -118.00 -71.00   0.50    0.55    --  -46.12-125.00   0.00   94
 17  \w   -118.00 -71.00   0.50    0.55    --  -46.12-125.00  90.00   94
 18  \w   -173.00 -80.00   0.50    6.50    -- -100.00-108.00 -50.00  186
 19  \w   -118.00 -71.00   0.50    0.55    --  -46.12-125.00-150.00   94
 20  \w   -172.00 -85.00   0.50    6.50    -- -100.00 -45.00 150.00  174
 21  \w     46.00 116.00   0.50    0.50    --   46.62  77.00  90.00  140
 22  \w     33.00  62.00   0.50    0.50    --   46.62 -57.00 -30.00   58
 23  \w     26.00  52.00   0.50    0.50    --   46.62-125.00-180.00   52
 24  \w    -24.00   5.00   0.50    0.50    --   46.62 -57.00 -30.00   58
 25  \w   -107.00 -79.00   0.50    0.05    -- -100.00  15.00  30.00   56
 26  \w    -56.00 -30.00   0.50    0.05    -- -100.00  15.00  30.00   52
 27  \w     90.00 117.00   0.50    0.05    --  107.00  15.00 120.00   54
 28  \w     45.00  71.00   0.50    0.05    --  107.00 -45.00  30.00   52
 29  \w     88.00 114.00   0.50    0.05    --  107.00 -77.00 150.00   52
 30  \w    139.00 165.00   0.50    0.05    --  107.00  77.00 -60.00   52
 31  \w     36.00  80.00   0.50    0.05    --  107.00 -77.00 150.00   88
 32  \w     85.00 114.00   0.50    0.05    --  107.00  77.00 -60.00   58
 33  \w     48.00  74.00   0.50    0.05    --  107.00 -94.00-120.00   52
 34  \w     85.00 111.00   0.50    0.05    --  107.00 -45.00  30.00   52
 35  \w     60.00  86.00   0.50    0.05    --  107.00 -94.00   0.00   52
 36  \w    129.00 178.00   0.50    0.05    --  107.00  15.00 120.00   98
 37  \w     57.00 110.00   0.50    0.05    --  107.00 -45.00 -60.00  106
 38  \w     90.00 116.00   0.50    0.05    --  107.00-125.00  90.00   52
 39  \w    142.00 175.00   0.50    0.05    --  107.00  30.00 -60.00   66
 40  \w     20.00  45.00   0.50    0.50    --   46.62-108.00 -51.00   50
 41  \w     20.00  45.00   0.50    0.50    --   46.62-108.00 -51.00   50
 42  \w     20.00  45.00   0.50    0.50    --   46.62-108.00 -51.00   50
 43  \w    -66.00 -41.00   0.50    0.50    --  -46.62 108.00  46.00   50
;
_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      0.0242325000
_diffrn_orient_matrix_UB_12      -0.1479053000
_diffrn_orient_matrix_UB_13      0.0094450000
_diffrn_orient_matrix_UB_21      0.0341983000
_diffrn_orient_matrix_UB_22      0.0062600000
_diffrn_orient_matrix_UB_23      -0.0968361000
_diffrn_orient_matrix_UB_31      0.0938659000
_diffrn_orient_matrix_UB_32      0.0362446000
_diffrn_orient_matrix_UB_33      0.0551322000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0645
_diffrn_reflns_av_unetI/netI     0.0401
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.982
_diffrn_reflns_limit_h_max       19
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            15504
_diffrn_reflns_point_group_measured_fraction_full 0.983
_diffrn_reflns_point_group_measured_fraction_max 0.948
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         77.036
_diffrn_reflns_theta_min         3.207
_diffrn_source                   'Rotating-anode X-ray tube'
_diffrn_source_type              'Rigaku (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    3.025
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.69338
_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_density_diffrn    1.409
_exptl_crystal_description       block
_exptl_crystal_F_000             936
_exptl_crystal_recrystallization_method 'From the Melt'
_exptl_crystal_size_max          0.19
_exptl_crystal_size_mid          0.1
_exptl_crystal_size_min          0.05
_refine_diff_density_max         0.668
_refine_diff_density_min         -0.383
_refine_diff_density_rms         0.071
_refine_ls_abs_structure_details
;
 Flack x determined using 1501 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   0.017(11)
_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     273
_refine_ls_number_reflns         4263
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.061
_refine_ls_R_factor_all          0.0696
_refine_ls_R_factor_gt           0.0617
_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^)+(0.1050P)^2^+2.4487P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1681
_refine_ls_wR_factor_ref         0.1754
_reflns_Friedel_coverage         0.824
_reflns_Friedel_fraction_full    0.963
_reflns_Friedel_fraction_max     0.910
_reflns_number_gt                3816
_reflns_number_total             4263
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d0cc03157g2.cif
_cod_data_source_block           Crizotinib-100k-XOu
_cod_depositor_comments
;
The following automatic conversions were performed:

data item '_chemical_melting_point' value '478k' was changed to '478'
-- 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               7126899
_shelx_shelxl_version_number     2016/6
_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) groups, All N(H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2.a Riding coordinates:
 N008(H008)
2.b Rotating group:
 N006(H00A,H00B)
2.c Ternary CH refined with riding coordinates:
 C00D(H00D), C00I(H00I)
2.d Secondary CH2 refined with riding coordinates:
 C00M(H00E,H00F), C00O(H00H,H00J), C00Q(H00P,H00Q), C00S(H00R,H00S)
2.e Aromatic/amide H refined with riding coordinates:
 C00B(H00C), C00G(H00G), C00K(H00K), C00N(H00N), C00T(H00T), C00U(H00U)
2.f Idealised Me refined as rotating group:
 C00P(H00L,H00M,H00O)
;
_shelx_res_checksum              56878
_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 1.889
_oxdiff_exptl_absorpt_empirical_full_min 0.294