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_7126900
_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 H20 N2 O6'
_chemical_formula_sum            'C18 H20 N2 O6'
_chemical_formula_weight         360.36
_chemical_melting_point          434
_chemical_name_common            Nitrendipine
_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             2020-01-08
_audit_creation_method
;
Olex2 1.3
(compiled Nov 21 2019 18:26:39 for OlexSys, GUI svn.r6003)
;
_audit_update_record
;
2020-06-27 deposited with the CCDC.	2020-07-13 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 93.7770(10)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   8.82590(10)
_cell_length_b                   15.2013(2)
_cell_length_c                   12.94740(10)
_cell_measurement_reflns_used    16420
_cell_measurement_temperature    99.99(10)
_cell_measurement_theta_max      76.8790
_cell_measurement_theta_min      4.4520
_cell_volume                     1733.32(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 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 0.986
_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    -62.00  29.00   0.50    0.52    --  -46.37  19.00 -60.00  182
  2  \w     69.00 118.00   0.50    0.52    --   46.37 135.00  46.00   98
  3  \w     69.00 178.00   0.50    2.10    --  107.00 135.00  46.00  218
  4  \w    128.00 178.00   0.50    2.10    --  107.00  15.00-120.00  100
  5  \w    103.00 129.00   0.50    2.10    --  107.00 125.00-180.00   52
  6  \w    147.00 177.00   0.50    2.10    --  107.00 125.00-180.00   60
  7  \w     90.00 123.00   0.50    2.10    --  107.00  15.00-120.00   66
  8  \w     63.00 122.00   0.50    2.10    --  107.00 -45.00 -60.00  118
  9  \w     86.00 113.00   0.50    2.10    --  107.00-125.00 -60.00   54
 10  \w     57.00  82.00   0.50    2.10    --  107.00-125.00 -60.00   50
 11  \w     34.00 124.00   0.50    2.10    --  107.00-135.00 -19.00  180
 12  \w     65.00 125.00   0.50    2.10    --  107.00 -61.00 120.00  120
 13  \w     90.00 178.00   0.50    2.10    --  107.00  15.00  60.00  176
 14  \w     70.00 178.00   0.50    2.10    --  107.00 134.00-132.00  216
 15  \w     70.00 118.00   0.50    0.52    --   46.37 134.00-132.00   96
 16  \w     32.00 124.00   0.50    2.10    --  107.00 -15.00-180.00  184
 17  \w     35.00 115.00   0.50    2.10    --  107.00 -61.00-120.00  160
 18  \w     36.00 107.00   0.50    2.10    --  107.00 -94.00   0.00  142
 19  \w     37.00 130.00   0.50    2.10    --  107.00 -77.00 120.00  186
 20  \w     35.00 108.00   0.50    2.10    --  107.00 -94.00 -30.00  146
 21  \w     34.00 117.00   0.50    2.10    --  107.00-125.00-150.00  166
 22  \w     21.00 101.00   0.50    0.52    --   46.37-135.00 -19.00  160
 23  \w     35.00  90.00   0.50    2.10    --  107.00 -45.00  60.00  110
 24  \w     35.00 122.00   0.50    2.10    --  107.00 -30.00  90.00  174
 25  \w     34.00 124.00   0.50    2.10    --  107.00-134.00 160.00  180
 26  \w     20.00 100.00   0.50    0.52    --   46.37-134.00 160.00  160
 27  \w    -25.00  63.00   0.50    0.52    --   46.37 -57.00-150.00  176
 28  \w    -62.00  29.00   0.50    0.52    --  -46.37  19.00 120.00  182
 29  \w   -100.00 -16.00   0.50    0.52    --  -46.37 134.00-132.00  168
 30  \w   -100.00 -16.00   0.50    0.52    --  -46.37 135.00  46.00  168
 31  \w   -102.00 -26.00   0.50    2.10    -- -100.00  30.00  90.00  152
 32  \w   -115.00 -25.00   0.50    2.10    -- -100.00  30.00 -90.00  180
 33  \w   -114.00 -28.00   0.50    2.10    -- -100.00  61.00  90.00  172
 34  \w   -124.00 -27.00   0.50    2.10    -- -100.00 135.00  46.00  194
 35  \w   -124.00 -27.00   0.50    2.10    -- -100.00 134.00-132.00  194
 36  \w   -173.00 -82.00   0.50    2.10    -- -100.00 -61.00-120.00  182
 37  \w   -118.00 -65.00   0.50    0.52    --  -46.37-135.00 -19.00  106
 38  \w   -118.00 -71.00   0.50    0.52    --  -46.37-125.00  30.00   94
 39  \w   -118.00 -66.00   0.50    0.52    --  -46.37-134.00 160.00  104
 40  \w   -118.00 -71.00   0.50    0.52    --  -46.37-125.00-150.00   94
;
_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      0.0343610000
_diffrn_orient_matrix_UB_12      -0.0984087000
_diffrn_orient_matrix_UB_13      0.0179248000
_diffrn_orient_matrix_UB_21      -0.1389318000
_diffrn_orient_matrix_UB_22      -0.0243183000
_diffrn_orient_matrix_UB_23      -0.0727558000
_diffrn_orient_matrix_UB_31      0.1006713000
_diffrn_orient_matrix_UB_32      -0.0000826000
_diffrn_orient_matrix_UB_33      -0.0926919000
_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  0.0674
_diffrn_reflns_av_unetI/netI     0.0311
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.986
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_number            34313
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.986
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         76.897
_diffrn_reflns_theta_min         4.492
_diffrn_source                   'Rotating-anode X-ray tube'
_diffrn_source_type              'Rigaku (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    0.877
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.85700
_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    1.381
_exptl_crystal_description       Strip
_exptl_crystal_F_000             760
_exptl_crystal_recrystallization_method 'From the Melt'
_exptl_crystal_size_max          0.12
_exptl_crystal_size_mid          0.06
_exptl_crystal_size_min          0.04
_refine_diff_density_max         0.707
_refine_diff_density_min         -0.516
_refine_diff_density_rms         0.073
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.054
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     239
_refine_ls_number_reflns         3602
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.054
_refine_ls_R_factor_all          0.0819
_refine_ls_R_factor_gt           0.0766
_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^)+(0.1027P)^2^+2.2389P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2034
_refine_ls_wR_factor_ref         0.2078
_reflns_Friedel_coverage         0.000
_reflns_number_gt                3257
_reflns_number_total             3602
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d0cc03157g2.cif
_cod_data_source_block           Nitrendipine-100k-HWRong
_cod_depositor_comments
;
The following automatic conversions were performed:

data item '_chemical_melting_point' value '434K' was changed to '434'
-- 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               7126900
_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:
 C00E(H00E)
2.b Secondary CH2 refined with riding coordinates:
 C00O(H00L,H00M)
2.c Aromatic/amide H refined with riding coordinates:
 N006(H006), C00F(H00F), C00G(H00G), C00I(H00I), C00J(H00J)
2.d Idealised Me refined as rotating group:
 C00K(H00A,H00B,H00C), C00N(H00D,H00H,H00K), C00P(H00N,H00O,H00P), C00Q(H00Q,
 H00R,H00S)
;
_shelx_res_checksum              87951
_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 2.086
_oxdiff_exptl_absorpt_empirical_full_min 0.438