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_7126907
_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 H26 N2 O7'
_chemical_formula_sum            'C21 H26 N2 O7'
_chemical_formula_weight         418.44
_chemical_melting_point          399
_chemical_name_common            Nimodipine
_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             2020-06-15
_audit_creation_method
;
Olex2 1.3
(compiled 2020.02.04 svn.rd84adfe8 for OlexSys, GUI svn.r6032)
;
_audit_update_record
;
2020-06-15 deposited with the CCDC.	2020-07-13 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 104.3000(10)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   13.76260(10)
_cell_length_b                   10.72760(10)
_cell_length_c                   14.78350(10)
_cell_measurement_reflns_used    30153
_cell_measurement_temperature    100.00(10)
_cell_measurement_theta_max      76.8510
_cell_measurement_theta_min      3.1010
_cell_volume                     2115.00(3)
_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      N~2~
_diffrn_ambient_temperature      100.00(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 0.990
_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    -74.00  27.00   0.50    0.05    --  -46.37  85.00  -5.00  202
  2  \w    -25.00  74.00   0.50    0.05    --   46.37 -85.00-124.00  198
  3  \w   -127.00 -27.00   0.50    0.05    -- -100.00  85.00  -5.00  200
  4  \w   -173.00 -77.00   0.50    0.05    -- -100.00 -85.00-124.00  192
  5  \w     34.00 135.00   0.50    0.05    --  107.00 -85.00-124.00  202
  6  \w   -118.00 -71.00   0.50    0.05    --  -46.37-125.00  60.00   94
  7  \w    -62.00  27.00   0.50    0.05    --  -46.37  57.00 -60.00  178
  8  \w   -118.00 -23.00   0.50    0.05    --  -46.37 -77.00-180.00  190
  9  \w   -118.00 -71.00   0.50    0.05    --  -46.37-125.00  30.00   94
 10  \w     31.00 122.00   0.50    0.05    --   46.37  19.00-120.00  182
 11  \w   -172.00 -85.00   0.50    0.05    -- -100.00 -45.00 -60.00  174
 12  \w   -175.00 -82.00   0.50    0.05    -- -100.00 -15.00 120.00  186
 13  \w   -173.00 -81.00   0.50    0.05    -- -100.00 -94.00 -60.00  184
 14  \w     32.00 123.00   0.50    0.05    --  107.00 -30.00  90.00  182
 15  \w     90.00 178.00   0.50    0.05    --  107.00  61.00 -60.00  176
 16  \w     34.00 117.00   0.50    0.05    --  107.00-125.00-120.00  166
 17  \w     34.00 117.00   0.50    0.05    --  107.00-125.00 -90.00  166
 18  \w     35.00 122.00   0.50    0.05    --  107.00 -45.00  90.00  174
 19  \w     31.00 125.00   0.50    0.05    --  107.00 -15.00-180.00  188
 20  \w     32.00 123.00   0.50    0.05    --  107.00 -30.00-150.00  182
 21  \w     93.00 178.00   0.50    0.05    --  107.00  45.00 120.00  170
 22  \w     34.00 117.00   0.50    0.05    --  107.00-125.00  90.00  166
 23  \w     93.00 178.00   0.50    0.05    --  107.00  45.00  60.00  170
 24  \w     35.00 122.00   0.50    0.05    --  107.00 -45.00-120.00  174
 25  \w     92.00 178.00   0.50    0.05    --  107.00  30.00 -30.00  172
 26  \w     34.00 109.00   0.50    0.05    --  107.00 -94.00 120.00  150
 27  \w     34.00 109.00   0.50    0.05    --  107.00 -94.00 -30.00  150
 28  \w     93.00 178.00   0.50    0.05    --  107.00  45.00 150.00  170
 29  \w     34.00 109.00   0.50    0.05    --  107.00 -94.00 -90.00  150
 30  \w     34.00 117.00   0.50    0.05    --  107.00-125.00  60.00  166
 31  \w     81.00 178.00   0.50    0.05    --  107.00  85.00  -5.00  194
 32  \w   -118.00 -23.00   0.50    0.05    --  -46.37 -77.00   0.00  190
;
_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      -0.0974466000
_diffrn_orient_matrix_UB_12      -0.0546445000
_diffrn_orient_matrix_UB_13      -0.0619603000
_diffrn_orient_matrix_UB_21      -0.0582981000
_diffrn_orient_matrix_UB_22      0.1151953000
_diffrn_orient_matrix_UB_23      0.0196937000
_diffrn_orient_matrix_UB_31      0.0212215000
_diffrn_orient_matrix_UB_32      0.0658411000
_diffrn_orient_matrix_UB_33      -0.0857604000
_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  0.0458
_diffrn_reflns_av_unetI/netI     0.0195
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.990
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            40061
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.990
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         76.841
_diffrn_reflns_theta_min         3.314
_diffrn_source                   'Rotating-anode X-ray tube'
_diffrn_source_type              'Rigaku (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    0.828
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.74365
_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    1.314
_exptl_crystal_description       block
_exptl_crystal_F_000             888
_exptl_crystal_recrystallization_method 'From the Melt'
_refine_diff_density_max         0.310
_refine_diff_density_min         -0.420
_refine_diff_density_rms         0.116
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.046
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     276
_refine_ls_number_reflns         4421
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.046
_refine_ls_R_factor_all          0.0456
_refine_ls_R_factor_gt           0.0447
_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^)+(0.0594P)^2^+1.0342P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1136
_refine_ls_wR_factor_ref         0.1143
_reflns_Friedel_coverage         0.000
_reflns_number_gt                4265
_reflns_number_total             4421
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d0cc03157g2.cif
_cod_data_source_block           Nimodipine-100k-HWRong
_cod_depositor_comments
;
The following automatic conversions were performed:

data item '_chemical_melting_point' value '399K' was changed to '399'
-- 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               7126907
_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) groups
 At 1.5 times of:
  All C(H,H,H) groups
2.a Ternary CH refined with riding coordinates:
 C00G(H00G), C00R(H00R)
2.b Secondary CH2 refined with riding coordinates:
 C00I(H00A,H00C), C00J(H00E,H00F)
2.c Aromatic/amide H refined with riding coordinates:
 N006(H006), C00B(H00B), C00D(H00D), C00O(H00O), C00P(H00P)
2.d Idealised Me refined as rotating group:
 C00M(H00H,H00I,H00J), C00Q(H00K,H00L,H00M), C00S(H00N,H00Q,H00S), C00T(H00T,
 H00U,H00V), C00U(H00W,H00X,H00Y)
;
_shelx_res_checksum              92074
_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 1.617
_oxdiff_exptl_absorpt_empirical_full_min 0.583