Mining predicted crystal structure landscapes with high throughput crystallisation: old molecules, new insights
Cui, Peng; McMahon, David P.; Spackman, Peter R.; Alston, Ben M.; Little, Marc A.; Day, Graeme M.; Cooper, Andrew I.; Chemical Science 10 (2019) 9988–; doi:10.1039/C9SC02832C

data_1555261
_publ_section_title
;
 Mining predicted crystal structure landscapes with high throughput
 crystallisation: old molecules, new insights
;
_journal_issue                   43
_journal_name_full               'Chemical Science'
_journal_page_first              9988
_journal_paper_doi               10.1039/C9SC02832C
_journal_volume                  10
_journal_year                    2019
_chemical_formula_moiety         '2(C14 H16 O8), 4(C8 H10 O2)'
_chemical_formula_sum            'C60 H72 O24'
_chemical_formula_weight         1177.17
_space_group_crystal_system      tetragonal
_space_group_IT_number           88
_space_group_name_Hall           '-I 4ad'
_space_group_name_H-M_alt        'I 41/a :2'
_atom_sites_solution_hydrogens   geom
_audit_creation_date             2018-12-05
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_audit_update_record
;
2019-05-10 deposited with the CCDC.	2019-08-20 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   16.2380(2)
_cell_length_b                   16.2380(2)
_cell_length_c                   22.3825(3)
_cell_measurement_reflns_used    8969
_cell_measurement_temperature    100.01(10)
_cell_measurement_theta_max      30.0790
_cell_measurement_theta_min      2.4890
_cell_volume                     5901.65(13)
_computing_cell_refinement
;
'CrysAlisPro 1.171.39.46e (Rigaku OD, 2018)'
;
_computing_data_collection
;
'CrysAlisPro 1.171.39.46e (Rigaku OD, 2018)'
;
_computing_data_reduction
;
'CrysAlisPro 1.171.39.46e (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)'
_diffrn_ambient_temperature      100.0
_diffrn_detector                 CCD
_diffrn_detector_area_resol_mean 28.5714
_diffrn_detector_type            'Rigaku Saturn724+'
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 1.000
_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   -109.00  16.00   1.00   10.00    --  -20.00 -68.00   0.00  125
  2  \w   -109.00  16.00   1.00   10.00    --  -20.00 -68.00 120.00  125
  3  \w   -109.00  16.00   1.00   10.00    --  -20.00 -68.00 240.00  125
  4  \w   -109.00  16.00   1.00   10.00    --  -20.00 -30.00  90.00  125
  5  \w    -90.00  90.00   1.00    1.00    --    0.00   0.00   0.00  180
;
_diffrn_measurement_device       'AFC12 (Right): Kappa 3 circle'
_diffrn_measurement_device_type  Rigaku_AFC12K_724P_007HF_Mo
_diffrn_measurement_method       'profile data from \w-scans'
_diffrn_measurement_specimen_support 'Mitegen 50um'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      -0.0227345000
_diffrn_orient_matrix_UB_12      -0.0050706000
_diffrn_orient_matrix_UB_13      -0.0267912000
_diffrn_orient_matrix_UB_21      -0.0353263000
_diffrn_orient_matrix_UB_22      -0.0107974000
_diffrn_orient_matrix_UB_23      0.0168476000
_diffrn_orient_matrix_UB_31      -0.0119427000
_diffrn_orient_matrix_UB_32      0.0419919000
_diffrn_orient_matrix_UB_33      0.0011003000
_diffrn_radiation_collimation    0.3
_diffrn_radiation_monochromator  Confocal
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0789
_diffrn_reflns_av_unetI/netI     0.0286
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 1.000
_diffrn_reflns_limit_h_max       20
_diffrn_reflns_limit_h_min       -20
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_l_max       27
_diffrn_reflns_limit_l_min       -27
_diffrn_reflns_number            45910
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 1.000
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         26.360
_diffrn_reflns_theta_min         2.509
_diffrn_source                   'Rotating Anode'
_diffrn_source_current           24.0
_diffrn_source_power             1.2
_diffrn_source_target            Mo
_diffrn_source_type              'Rotating Anode'
_diffrn_source_voltage           50.0
_exptl_absorpt_coefficient_mu    0.103
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.71430
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.39.46e (Rigaku Oxford Diffraction, 2018)
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    1.325
_exptl_crystal_description       block
_exptl_crystal_F_000             2496
_exptl_crystal_size_max          0.11
_exptl_crystal_size_mid          0.09
_exptl_crystal_size_min          0.07
_refine_diff_density_max         0.330
_refine_diff_density_min         -0.250
_refine_diff_density_rms         0.049
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.064
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     195
_refine_ls_number_reflns         3006
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.064
_refine_ls_R_factor_all          0.0639
_refine_ls_R_factor_gt           0.0511
_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^)+(0.0692P)^2^+4.1353P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1334
_refine_ls_wR_factor_ref         0.1421
_reflns_Friedel_coverage         0.000
_reflns_number_gt                2383
_reflns_number_total             3006
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c9sc02832c2.cif
_cod_data_source_block           ADTA_2-34_THF-1-2-dimethoxybenzene_publ
_cod_original_cell_volume        5901.65(17)
_cod_original_sg_symbol_H-M      'I 41/a'
_cod_database_code               1555261
_shelx_shelxl_version_number     2014/7
_shelx_estimated_absorpt_t_max   0.993
_shelx_estimated_absorpt_t_min   0.989
_oxdiff_exptl_absorpt_empirical_full_min 0.643
_oxdiff_exptl_absorpt_empirical_full_max 1.395
_oxdiff_exptl_absorpt_empirical_details
;
Empirical correction (ABSPACK) includes:
- Absorption correction using spherical harmonics
- Frame scaling
;
_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. Others
 Fixed Sof: H9A(0.5) H9B(0.5) H14A(0.5) H14B(0.5)
3.a Secondary CH2 refined with riding coordinates:
 C9(H9A,H9B), C14(H14A,H14B), C11(H11A,H11B), C16(H16A,H16B)
3.b Aromatic/amide H refined with riding coordinates:
 C6(H6), C5(H5), C3(H3), C4(H4)
3.c Idealised Me refined as rotating group:
 C8(H8A,H8B,H8C), C7(H7A,H7B,H7C)
3.d Idealised tetrahedral OH refined as rotating group:
 O4(H4A), O2(H2)
;
_shelx_res_checksum              16830
_olex2_submission_special_instructions 'No special instructions were received'