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_7126903
_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         'C17 H18 N2 O6'
_chemical_formula_sum            'C17 H18 N2 O6'
_chemical_formula_weight         346.33
_chemical_melting_point          445
_chemical_name_common            nifedipine
_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             2018-12-04
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_audit_update_record
;
2019-05-24 deposited with the CCDC.	2020-07-13 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 94.879(3)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   10.6219(4)
_cell_length_b                   10.4085(4)
_cell_length_c                   14.7800(5)
_cell_measurement_reflns_used    7919
_cell_measurement_temperature    100.00(10)
_cell_measurement_theta_max      75.8780
_cell_measurement_theta_min      3.0790
_cell_volume                     1628.13(10)
_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 0.993
_diffrn_measured_fraction_theta_max 0.934
_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   -118.00 -31.00   0.50    0.05    --  -46.37 -36.00  14.00  174
  2  \w     34.00  79.00   0.50    0.05    --   46.37  36.00 170.00   90
  3  \w     -1.00  57.00   0.50    0.05    --   46.37 -36.00  14.00  116
  4  \w   -169.00 -90.00   0.50    0.05    -- -100.00 -36.00  14.00  158
  5  \w   -115.00 -27.00   0.50    0.05    -- -100.00  36.00 170.00  176
  6  \w    138.00 163.00   0.50    0.05    --  107.00  36.00 170.00   50
  7  \w     94.00 119.00   0.50    0.05    --  107.00  36.00 170.00   50
  8  \w     47.00  72.00   0.50    0.05    --  107.00 -36.00  14.00   50
  9  \w    -41.00 -16.00   0.50    0.05    --  -46.37  36.00 170.00   50
 10  \w     16.00  95.00   0.50    0.05    --   46.37-125.00 -90.00  158
 11  \w    -61.00 -28.00   0.50    0.05    -- -100.00 125.00-180.00   66
 12  \w   -113.00 -25.00   0.50    0.05    -- -100.00  15.00   0.00  176
 13  \w   -117.00 -73.00   0.50    0.05    -- -100.00  61.00   0.00   88
 14  \w    -62.00 -27.00   0.50    0.05    -- -100.00  61.00   0.00   70
 15  \w   -113.00 -28.00   0.50    0.05    -- -100.00  45.00   0.00  170
 16  \w    103.00 166.00   0.50    0.05    --  107.00  45.00 -60.00  126
 17  \w     39.00  89.00   0.50    0.05    --  107.00 -95.00   0.00  100
;
_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      -0.1132664000
_diffrn_orient_matrix_UB_12      -0.0030968000
_diffrn_orient_matrix_UB_13      0.0585891000
_diffrn_orient_matrix_UB_21      -0.0826119000
_diffrn_orient_matrix_UB_22      0.0675998000
_diffrn_orient_matrix_UB_23      -0.0764535000
_diffrn_orient_matrix_UB_31      -0.0395898000
_diffrn_orient_matrix_UB_32      -0.1316604000
_diffrn_orient_matrix_UB_33      -0.0405501000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0447
_diffrn_reflns_av_unetI/netI     0.0302
_diffrn_reflns_Laue_measured_fraction_full 0.993
_diffrn_reflns_Laue_measured_fraction_max 0.934
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            10268
_diffrn_reflns_point_group_measured_fraction_full 0.993
_diffrn_reflns_point_group_measured_fraction_max 0.934
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         76.509
_diffrn_reflns_theta_min         5.204
_diffrn_source                   'Rotating-anode X-ray tube'
_diffrn_source_type              'Rigaku (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    0.911
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.26450
_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 yellowish yellow'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   yellowish
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    1.413
_exptl_crystal_description       block
_exptl_crystal_F_000             728
_exptl_crystal_recrystallization_method 'From the Melt'
_exptl_crystal_size_max          0.4
_exptl_crystal_size_mid          0.3
_exptl_crystal_size_min          0.3
_refine_diff_density_max         0.318
_refine_diff_density_min         -0.267
_refine_diff_density_rms         0.060
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.029
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     230
_refine_ls_number_reflns         3196
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.029
_refine_ls_R_factor_all          0.0519
_refine_ls_R_factor_gt           0.0471
_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^)+(0.0685P)^2^+0.9950P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1229
_refine_ls_wR_factor_ref         0.1269
_reflns_Friedel_coverage         0.000
_reflns_number_gt                2957
_reflns_number_total             3196
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d0cc03157g2.cif
_cod_data_source_block           Alpha-NIF-100K-XZLI
_cod_depositor_comments
;
The following automatic conversions were performed:

data item '_chemical_melting_point' value '445K' was changed to '445'
-- 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               7126903
_shelx_shelxl_version_number     2016/6
_shelx_estimated_absorpt_t_max   0.772
_shelx_estimated_absorpt_t_min   0.712
_reflns_odcompleteness_completeness 99.45
_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
2.a Ternary CH refined with riding coordinates:
 C00C(H00C)
2.b Aromatic/amide H refined with riding coordinates:
 N007(H007), C00A(H00A), C00J(H00J), C00K(H00K), C00L(H00L)
2.c Idealised Me refined as rotating group:
 C00M(H00B,H00D,H00E), C00N(H00F,H00G,H00H), C00O(H00I,H00M,H00N), C00P(H00O,
 H00P,H00Q)
;
_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 5.349
_oxdiff_exptl_absorpt_empirical_full_min 0.361