The formation mechanism of hollow spherulites and molecular conformation of curcumin and solvate
Wan, Xuxing; Wu, Songgu; Wang, Yan; Gong, Junbo; CrystEngComm  (2020) –; doi:10.1039/D0CE01230K

data_7241450
_publ_section_title
;
 The formation mechanism of hollow spherulites and molecular conformation
 of curcumin and solvate
;
_journal_name_full               CrystEngComm
_journal_paper_doi               10.1039/D0CE01230K
_journal_year                    2020
_chemical_formula_moiety         'C21 H20 O6, C4 H8 O2'
_chemical_formula_sum            'C25 H28 O8'
_chemical_formula_weight         456.47
_space_group_crystal_system      monoclinic
_space_group_IT_number           15
_space_group_name_Hall           '-I 2ya'
_space_group_name_H-M_alt        'I 1 2/a 1'
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     dual
_audit_creation_date             2020-07-10
_audit_creation_method
;
Olex2 1.3-alpha
(compiled 2020.05.07 svn.rd67b107b for OlexSys, GUI svn.r6105)
;
_audit_update_record
;
2020-07-14 deposited with the CCDC.	2020-11-04 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 106.501(5)
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   24.3727(11)
_cell_length_b                   5.3458(2)
_cell_length_c                   36.3946(17)
_cell_measurement_reflns_used    2303
_cell_measurement_temperature    159.99(10)
_cell_measurement_theta_max      53.3220
_cell_measurement_theta_min      3.9190
_cell_volume                     4546.6(4)
_computing_cell_refinement       'CrysAlisPro 1.171.40.53 (Rigaku OD, 2019)'
_computing_data_collection       'CrysAlisPro 1.171.40.53 (Rigaku OD, 2019)'
_computing_data_reduction        'CrysAlisPro 1.171.40.53 (Rigaku OD, 2019)'
_computing_molecular_graphics    'Olex2 1.3-alpha (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.3-alpha (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      159.99(10)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 10.0000
_diffrn_detector_type            HyPix
_diffrn_measured_fraction_theta_full 0.993
_diffrn_measured_fraction_theta_max 0.993
_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    -41.00  36.00   0.50    1.00    --    0.82 -77.00 -60.00  154
  2  \w     -6.00  19.00   0.50    1.00    --    0.82-100.00 -78.00   50
  3  \w      4.00  29.00   0.50    1.00    --   -2.85-100.00 -78.00   50
  4  \w     39.00  89.00   0.50    1.00    --    0.82-179.00 -60.00  100
  5  \w     38.00 109.00   0.50    4.00    --   75.30-100.00 -78.00  142
  6  \w     17.00 116.00   0.50    4.00    --   75.30-125.00 -60.00  198
  7  \w     54.00  98.00   0.50    4.00    --   75.30-125.00  90.00   88
  8  \w     16.00  41.00   0.50    4.00    --   75.30-125.00  90.00   50
  9  \w     -4.00  76.00   0.50    1.00    --    0.82  57.00 120.00  160
 10  \w     97.00 122.00   0.50    4.00    --   75.30 100.00  26.00   50
 11  \w     88.00 155.00   0.50    4.00    --   75.30 125.00 -60.00  134
 12  \w     75.00 155.00   0.50    4.00    --   75.30 125.00 150.00  160
 13  \w    -28.00  61.00   0.50    1.00    --    0.82  57.00  90.00  178
 14  \w    -44.00 -19.00   0.50    1.00    --    0.82 100.00  26.00   50
 15  \w    -38.00   7.00   0.50    1.00    --   -2.85 100.00  26.00   90
 16  \w    -87.00 -62.00   0.50    4.00    --  -77.33 100.00  26.00   50
 17  \w    -81.00 -45.00   0.50    1.00    --   -2.85 179.00  30.00   72
 18  \w   -115.00   2.00   0.50    4.00    --  -77.33  77.00-150.00  234
 19  \w    -64.00 -38.00   0.50    4.00    --  -77.33 125.00-180.00   52
 20  \w   -153.00 -50.00   0.50    4.00    --  -77.33 -61.00  60.00  206
 21  \w   -125.00-100.00   0.50    4.00    --  -77.33-100.00 -78.00   50
 22  \w   -126.00 -45.00   0.50    4.00    --  -77.33 -61.00 -60.00  162
 23  \w   -138.00 -84.00   0.50    4.00    --  -77.33 -94.00 -30.00  108
 24  \w   -135.00 -81.00   0.50    4.00    --  -77.33-125.00-120.00  108
 25  \w   -138.00 -58.00   0.50    4.00    --  -77.33 -61.00 -30.00  160
 26  \w   -143.00 -52.00   0.50    4.00    --  -77.33 -61.00  90.00  182
 27  \w   -155.00 -81.00   0.50    4.00    --  -77.33-125.00  30.00  148
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'ROD, Synergy Custom system, HyPix'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      -0.0291307000
_diffrn_orient_matrix_UB_12      0.1056131000
_diffrn_orient_matrix_UB_13      0.0290832000
_diffrn_orient_matrix_UB_21      0.0587193000
_diffrn_orient_matrix_UB_22      0.0200886000
_diffrn_orient_matrix_UB_23      0.0302190000
_diffrn_orient_matrix_UB_31      0.0071284000
_diffrn_orient_matrix_UB_32      0.2673773000
_diffrn_orient_matrix_UB_33      -0.0137924000
_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  0.0547
_diffrn_reflns_av_unetI/netI     0.0457
_diffrn_reflns_Laue_measured_fraction_full 0.993
_diffrn_reflns_Laue_measured_fraction_max 0.993
_diffrn_reflns_limit_h_max       26
_diffrn_reflns_limit_h_min       -25
_diffrn_reflns_limit_k_max       5
_diffrn_reflns_limit_k_min       -5
_diffrn_reflns_limit_l_max       38
_diffrn_reflns_limit_l_min       -39
_diffrn_reflns_number            14127
_diffrn_reflns_point_group_measured_fraction_full 0.993
_diffrn_reflns_point_group_measured_fraction_max 0.993
_diffrn_reflns_theta_full        56.513
_diffrn_reflns_theta_max         56.513
_diffrn_reflns_theta_min         3.783
_diffrn_source                   'Rotating-anode X-ray tube'
_diffrn_source_type              'Rigaku (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    0.827
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.73396
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.40.53 (Rigaku Oxford Diffraction, 2019)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            colourless
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.334
_exptl_crystal_description       block
_exptl_crystal_F_000             1936
_exptl_crystal_size_max          0.1
_exptl_crystal_size_mid          0.08
_exptl_crystal_size_min          0.08
_refine_diff_density_max         0.233
_refine_diff_density_min         -0.188
_refine_diff_density_rms         0.053
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.035
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     312
_refine_ls_number_reflns         2991
_refine_ls_number_restraints     3
_refine_ls_restrained_S_all      1.036
_refine_ls_R_factor_all          0.0889
_refine_ls_R_factor_gt           0.0554
_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^)+(0.0827P)^2^+4.3883P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1366
_refine_ls_wR_factor_ref         0.1571
_reflns_Friedel_coverage         0.000
_reflns_number_gt                2064
_reflns_number_total             2991
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d0ce01230k3.cif
_cod_data_source_block           034592_wxx_160k_2_d
_cod_database_code               7241450
_shelx_shelxl_version_number     2018/3
_chemical_oxdiff_formula         'C25 H28 O8'
_shelx_estimated_absorpt_t_max   0.937
_shelx_estimated_absorpt_t_min   0.922
_reflns_odcompleteness_completeness 99.81
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     54.18
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Restrained distances
 H4-O4
 0.9 with sigma of 0.02
 H5-O5 = H1-O1
 0.9 with sigma of 0.02
3.a Secondary CH2 refined with riding coordinates:
 C25(H25A,H25B), C22(H22A,H22B), C24(H24A,H24B), C23(H23A,H23B)
3.b Aromatic/amide H refined with riding coordinates:
 C7(H7), C6(H6), C3(H3), C13(H13), C10(H10), C15(H15), C8(H8), C4(H4A),
 C12(H12), C19(H19), C18(H18)
3.c Idealised Me refined as rotating group:
 C20(H20A,H20B,H20C), C21(H21A,H21B,H21C)
;
_shelx_res_checksum              97259
_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 1.659
_oxdiff_exptl_absorpt_empirical_full_min 0.731