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_7126915
_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         'C18 H19 Cl2 N O4'
_chemical_formula_sum            'C18 H19 Cl2 N O4'
_chemical_formula_weight         384.24
_chemical_melting_point          418
_chemical_name_common            Felodipine
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2ybc'
_space_group_name_H-M_alt        'P 1 21/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_audit_creation_date             2019-12-23
_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                 116.167(2)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   12.0936(2)
_cell_length_b                   12.0624(2)
_cell_length_c                   13.4258(2)
_cell_measurement_reflns_used    22811
_cell_measurement_temperature    99.99(10)
_cell_measurement_theta_max      76.8090
_cell_measurement_theta_min      3.6620
_cell_volume                     1757.80(6)
_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      99.99(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 0.987
_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    -96.00 -12.00   0.50    0.05    --  -46.37 127.00   9.00  168
  2  \w   -105.00 -20.00   0.50    0.05    --  -46.37 143.00 179.00  170
  3  \w   -118.00 -70.00   0.50    0.05    --  -46.37-127.00 -65.00   96
  4  \w   -118.00 -59.00   0.50    0.05    --  -46.37-143.00 124.00  118
  5  \w     64.00 118.00   0.50    0.05    --   46.37 143.00 179.00  108
  6  \w     25.00 106.00   0.50    0.05    --   46.37-143.00 124.00  162
  7  \w     16.00  96.00   0.50    0.05    --   46.37-127.00 -65.00  160
  8  \w   -130.00 -27.00   0.50    0.05    -- -100.00 143.00 179.00  206
  9  \w   -118.00 -27.00   0.50    0.05    -- -100.00 127.00   9.00  182
 10  \w   -173.00 -70.00   0.50    0.05    -- -100.00-127.00 -65.00  206
 11  \w     74.00 178.00   0.50    0.05    --  107.00 127.00   9.00  208
 12  \w     34.00 130.00   0.50    0.05    --  107.00-143.00 124.00  192
 13  \w     34.00 118.00   0.50    0.05    --  107.00-127.00 -65.00  168
 14  \w     64.00 176.00   0.50    0.05    --  107.00 143.00 179.00  224
 15  \w   -118.00 -71.00   0.50    0.05    --  -46.37-125.00   0.00   94
 16  \w   -118.00 -71.00   0.50    0.05    --  -46.37-125.00 150.00   94
 17  \w     30.00 118.00   0.50    0.05    --   46.37  57.00  90.00  176
 18  \w     30.00 118.00   0.50    0.05    --   46.37  57.00-180.00  176
 19  \w     30.00 118.00   0.50    0.05    --   46.37  57.00 -60.00  176
 20  \w   -175.00 -82.00   0.50    0.05    -- -100.00 -15.00-180.00  186
 21  \w   -114.00 -27.00   0.50    0.05    -- -100.00  45.00  60.00  174
 22  \w   -142.00-111.00   0.50    0.05    -- -100.00 -59.00  20.52   62
 23  \w   -173.00-147.00   0.50    0.05    -- -100.00 -59.00  20.52   52
 24  \w   -140.00-115.00   0.50    0.05    -- -100.00-143.00 124.00   50
 25  \w     74.00 117.00   0.50    0.05    --  107.00-125.00-150.00   86
 26  \w    132.00 178.00   0.50    0.05    --  107.00 125.00-120.00   92
 27  \w     35.00 120.00   0.50    0.05    --  107.00 -45.00 150.00  170
 28  \w     92.00 177.00   0.50    0.05    --  107.00  30.00-120.00  170
 29  \w     97.00 123.00   0.50    0.05    --  107.00 -61.00  90.00   52
 30  \w     82.00 121.00   0.50    0.05    --  107.00 -45.00  60.00   78
 31  \w     37.00  63.00   0.50    0.05    --  107.00-125.00-120.00   52
 32  \w     58.00  88.00   0.50    0.05    --  107.00 -61.00  90.00   60
 33  \w     60.00  85.00   0.50    0.05    --  107.00-125.00 -30.00   50
 34  \w     80.00 117.00   0.50    0.05    --  107.00-125.00-120.00   74
 35  \w    146.00 178.00   0.50    0.05    --  107.00 125.00  60.00   64
 36  \w     34.00 117.00   0.50    0.05    --  107.00-125.00   0.00  166
 37  \w     91.00 177.00   0.50    0.05    --  107.00  61.00 -90.00  172
 38  \w     35.00 103.00   0.50    0.05    --  107.00-125.00  90.00  136
 39  \w     62.00 113.00   0.50    0.05    --  107.00 -61.00 -60.00  102
 40  \w     34.00  76.00   0.50    0.05    --  107.00 -77.00  90.00   84
 41  \w     78.00 128.00   0.50    0.05    --  107.00 125.00  60.00  100
 42  \w     87.00 113.00   0.50    0.05    --  107.00-125.00  30.00   52
 43  \w     37.00  63.00   0.50    0.05    --  107.00-125.00  30.00   52
 44  \w     33.00 122.00   0.50    0.05    --  107.00 -30.00-120.00  178
 45  \w     35.00  72.00   0.50    0.05    --  107.00 -45.00  60.00   74
;
_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      0.0642153000
_diffrn_orient_matrix_UB_12      0.1131037000
_diffrn_orient_matrix_UB_13      0.0126949000
_diffrn_orient_matrix_UB_21      0.1252284000
_diffrn_orient_matrix_UB_22      -0.0589806000
_diffrn_orient_matrix_UB_23      0.0393194000
_diffrn_orient_matrix_UB_31      -0.0187546000
_diffrn_orient_matrix_UB_32      -0.0073632000
_diffrn_orient_matrix_UB_33      -0.1209163000
_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  0.0537
_diffrn_reflns_av_unetI/netI     0.0208
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.987
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       12
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_number            33252
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.987
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         76.979
_diffrn_reflns_theta_min         4.073
_diffrn_source                   'Rotating-anode X-ray tube'
_diffrn_source_type              'Rigaku (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    3.527
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.14018
_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_density_diffrn    1.452
_exptl_crystal_description       block
_exptl_crystal_F_000             800
_exptl_crystal_recrystallization_method 'From the Melt'
_exptl_crystal_size_max          0.15
_exptl_crystal_size_mid          0.13
_exptl_crystal_size_min          0.1
_refine_diff_density_max         1.344
_refine_diff_density_min         -1.384
_refine_diff_density_rms         0.094
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.041
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     230
_refine_ls_number_reflns         3658
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.041
_refine_ls_R_factor_all          0.0798
_refine_ls_R_factor_gt           0.0782
_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^)+(0.0918P)^2^+4.4349P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1983
_refine_ls_wR_factor_ref         0.1997
_reflns_Friedel_coverage         0.000
_reflns_number_gt                3515
_reflns_number_total             3658
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d0cc03157g2.cif
_cod_data_source_block           Felodipine-100k-HWRong
_cod_depositor_comments
;
The following automatic conversions were performed:

data item '_chemical_melting_point' value '418K' was changed to '418'
-- 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               7126915
_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
 At 1.5 times of:
  All C(H,H,H) groups
2.a Ternary CH refined with riding coordinates:
 C00A(H00A)
2.b Secondary CH2 refined with riding coordinates:
 C00I(H00B,H00C)
2.c Aromatic/amide H refined with riding coordinates:
 N007(H007), C00D(H00D), C00K(H00K), C00O(H00O)
2.d Idealised Me refined as rotating group:
 C00J(H00E,H00F,H00G), C00L(H00H,H00I,H00J), C00N(H00L,H00M,H00N), C00P(H00P,
 H00Q,H00R)
;
_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 4.576
_oxdiff_exptl_absorpt_empirical_full_min 0.509