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_7241451
_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         '3(C2 H4 O), C21 H20 O6'
_chemical_formula_sum            'C27 H32 O9'
_chemical_formula_weight         500.52
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2yn'
_space_group_name_H-M_alt        'P 1 21/n 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                 94.345(2)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   21.7077(6)
_cell_length_b                   5.14640(10)
_cell_length_c                   22.8388(4)
_cell_measurement_reflns_used    4864
_cell_measurement_temperature    160.00(10)
_cell_measurement_theta_max      72.9680
_cell_measurement_theta_min      2.7350
_cell_volume                     2544.14(10)
_computing_cell_refinement       'CrysAlisPro 1.171.39.45g (Rigaku OD, 2018)'
_computing_data_collection       'CrysAlisPro 1.171.39.45g (Rigaku OD, 2018)'
_computing_data_reduction        'CrysAlisPro 1.171.39.45g (Rigaku OD, 2018)'
_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 2014/5 (Sheldrick, 2014)'
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      160.00(10)
_diffrn_detector                 'CCD plate'
_diffrn_detector_type            HyPix
_diffrn_measured_fraction_theta_full 0.993
_diffrn_measured_fraction_theta_max 0.938
_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    -18.00  77.00   0.50    1.00    --   45.62 -96.00  72.00  190
  2  \w     42.00 109.00   0.50   10.00    --  101.75 -96.00  72.00  134
  3  \w     73.00 126.00   0.50   10.00    --  101.75 -77.00 -60.00  106
  4  \w     60.00 118.00   0.50    1.00    --   45.62  38.00   0.00  116
  5  \w    149.00 174.00   0.50   10.00    --  101.75  45.00 120.00   50
  6  \w     97.00 124.00   0.50   10.00    --  101.75  45.00 120.00   54
  7  \w     29.00  55.00   0.50   10.00    --  101.75 -77.00 -60.00   52
  8  \w     95.00 122.00   0.50   10.00    --  101.75  96.00-178.00   54
  9  \w    -69.00  26.00   0.50    1.00    --  -45.62  96.00-178.00  190
 10  \w    -60.00 -28.00   0.50   10.00    -- -100.00 125.00-150.00   64
 11  \w    -96.00 -61.00   0.50   10.00    -- -100.00  96.00-178.00   70
 12  \w   -117.00 -76.00   0.50   10.00    -- -100.00 125.00-150.00   82
 13  \w   -113.00 -27.00   0.50   10.00    -- -100.00  45.00-180.00  172
 14  \w   -113.00 -74.00   0.50    1.00    --  -45.62-125.00-150.00   78
 15  \w   -167.00 -95.00   0.50   10.00    -- -100.00 -45.00   0.00  144
 16  \w   -172.00 -79.00   0.50   10.00    -- -100.00 -96.00  72.00  186
 17  \w   -118.00 -91.00   0.50    1.00    --  -45.62-125.00 150.00   54
 18  \w   -171.00-118.00   0.50   10.00    -- -100.00 -45.00 -30.00  106
;
_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      -0.0131689000
_diffrn_orient_matrix_UB_12      -0.1668015000
_diffrn_orient_matrix_UB_13      -0.0555530000
_diffrn_orient_matrix_UB_21      0.0209708000
_diffrn_orient_matrix_UB_22      0.2257895000
_diffrn_orient_matrix_UB_23      -0.0380318000
_diffrn_orient_matrix_UB_31      0.0667603000
_diffrn_orient_matrix_UB_32      -0.1037561000
_diffrn_orient_matrix_UB_33      0.0064830000
_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  0.0489
_diffrn_reflns_av_unetI/netI     0.0525
_diffrn_reflns_Laue_measured_fraction_full 0.993
_diffrn_reflns_Laue_measured_fraction_max 0.938
_diffrn_reflns_limit_h_max       26
_diffrn_reflns_limit_h_min       -22
_diffrn_reflns_limit_k_max       6
_diffrn_reflns_limit_k_min       -6
_diffrn_reflns_limit_l_max       28
_diffrn_reflns_limit_l_min       -27
_diffrn_reflns_number            16343
_diffrn_reflns_point_group_measured_fraction_full 0.993
_diffrn_reflns_point_group_measured_fraction_max 0.938
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         74.474
_diffrn_reflns_theta_min         2.708
_diffrn_source                   'Rotating-anode X-ray tube'
_diffrn_source_type              'Rigaku (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    0.815
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.61214
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.39.45g (Rigaku Oxford Diffraction, 2018)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            yellow
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    1.307
_exptl_crystal_description       needle
_exptl_crystal_F_000             1064
_exptl_crystal_size_max          0.1
_exptl_crystal_size_mid          0.03
_exptl_crystal_size_min          0.03
_refine_diff_density_max         0.172
_refine_diff_density_min         -0.262
_refine_diff_density_rms         0.053
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.032
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     333
_refine_ls_number_reflns         4893
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.032
_refine_ls_R_factor_all          0.0700
_refine_ls_R_factor_gt           0.0509
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0835P)^2^+0.3829P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1345
_refine_ls_wR_factor_ref         0.1496
_reflns_Friedel_coverage         0.000
_reflns_number_gt                3618
_reflns_number_total             4893
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d0ce01230k3.cif
_cod_data_source_block           034236_wxx_160k_a
_cod_database_code               7241451
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   0.976
_shelx_estimated_absorpt_t_min   0.923
_reflns_odcompleteness_completeness 99.32
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     66.49
_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, All O(H) groups
2. Restrained distances
 O4-H4
 0.9 with sigma of 0.02
3.a Secondary CH2 refined with riding coordinates:
 C27(H27A,H27B), C26(H26A,H26B), C23(H23A,H23B), C22(H22A,H22B), C24(H24A,
 H24B), C25(H25A,H25B)
3.b Aromatic/amide H refined with riding coordinates:
 C15(H15), C10(H10), C12(H12), C13(H13), C6(H6), C19(H19), C18(H18), C4(H4A),
 C8(H8), C7(H7), C3(H3)
3.c Idealised Me refined as rotating group:
 C21(H21A,H21B,H21C), C20(H20A,H20B,H20C)
3.d Idealised tetrahedral OH refined as rotating group:
 O5(H5), O1(H1)
;
_shelx_res_checksum              22690
_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 1.608
_oxdiff_exptl_absorpt_empirical_full_min 0.674