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_1555270
_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         '3(C9 H6 O6), 2(C12 H10 O)'
_chemical_formula_sum            'C51 H38 O20'
_chemical_formula_weight         970.81
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_atom_sites_solution_hydrogens   mixed
_audit_creation_date             2018-05-21
_audit_creation_method
;
Olex2 1.2
(compiled 2018.04.26 svn.r3504 for OlexSys, GUI svn.r5492)
;
_audit_update_record
;
2019-05-10 deposited with the CCDC.	2019-08-20 downloaded from the CCDC.
;
_cell_angle_alpha                113.7260(4)
_cell_angle_beta                 98.4480(4)
_cell_angle_gamma                106.8020(4)
_cell_formula_units_Z            2
_cell_length_a                   10.50240(6)
_cell_length_b                   15.88590(7)
_cell_length_c                   16.60930(7)
_cell_measurement_reflns_used    21452
_cell_measurement_temperature    200
_cell_measurement_theta_max      35.6992161017
_cell_measurement_theta_min      1.35437565248
_cell_volume                     2316.46(2)
_computing_cell_refinement
'DIALS 2theta refinement, DIALS 1.9.3-gb491019a-release'
_computing_data_collection       'Diamond I19 GDA, (Diamond, RAL, Didcot, UK)'
_computing_data_reduction
;
aimless (Evans, P. R. and Murshudov, G. N., 2013)
ccp4 (Winn, M. D. et al., 2011)
DIALS 1.9.3-gb491019a-release (Winter, G. et al., 2018)
pointless (Evans, P., 2006)
XIA2 0.5.546-gdf2e0b53-dials-1.9 (Winter, G., 2010)
;
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'XL (Sheldrick, 2014)'
_computing_structure_solution    'XT (Sheldrick, 2014)'
_diffrn_ambient_temperature      200
_diffrn_detector                 'Photon counting pixel array'
_diffrn_detector_area_resol_mean PILATUS_2M_S_N_24_0107_Diamond
_diffrn_detector_type            PILATUS_2M_S_N_24_0107_Diamond
_diffrn_measured_fraction_theta_full 0.992
_diffrn_measured_fraction_theta_max 0.988
_diffrn_measurement_device       'Fixed \c 3-circle diffractometer'
_diffrn_measurement_device_type  'Fluid Film Devices'
_diffrn_measurement_method       'shutterless scans'
_diffrn_radiation_collimation    '0.3 x 1.5 Double Pinhole'
_diffrn_radiation_monochromator  'Silicon 111'
_diffrn_radiation_probe          x-ray
_diffrn_radiation_source         'Diamond Light Source Beamline I19-1'
_diffrn_radiation_wavelength     0.6889
_diffrn_reflns_av_R_equivalents  0.0281
_diffrn_reflns_av_unetI/netI     0.0317
_diffrn_reflns_Laue_measured_fraction_full 0.992
_diffrn_reflns_Laue_measured_fraction_max 0.988
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       21
_diffrn_reflns_limit_k_min       -21
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_number            36998
_diffrn_reflns_point_group_measured_fraction_full 0.992
_diffrn_reflns_point_group_measured_fraction_max 0.988
_diffrn_reflns_theta_full        24.415
_diffrn_reflns_theta_max         28.152
_diffrn_reflns_theta_min         1.361
_diffrn_source                   Synchrotron
_diffrn_source_type              'Undulator, I19, DLS, RAL'
_exptl_absorpt_coefficient_mu    0.100
_exptl_absorpt_correction_T_max  1.0
_exptl_absorpt_correction_T_min  0.995896160689
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_process_details
;
CCP4 7.0.052: AIMLESS, version 0.6.2 : 15/01/18
Scaling & analysis of unmerged intensities, absorption correction using spherical harmonics
;
_exptl_crystal_colour            colourless
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.392
_exptl_crystal_description       block
_exptl_crystal_F_000             1008
_exptl_crystal_size_max          0.078
_exptl_crystal_size_mid          0.028
_exptl_crystal_size_min          0.024
_refine_diff_density_max         0.306
_refine_diff_density_min         -0.380
_refine_diff_density_rms         0.110
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.100
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     700
_refine_ls_number_reflns         12320
_refine_ls_number_restraints     196
_refine_ls_restrained_S_all      1.113
_refine_ls_R_factor_all          0.0559
_refine_ls_R_factor_gt           0.0429
_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^)+(0.0900P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1345
_refine_ls_wR_factor_ref         0.1429
_reflns_Friedel_coverage         0.000
_reflns_number_gt                8999
_reflns_number_total             12320
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c9sc02832c2.cif
_cod_data_source_block           TMA_3-36_EtOH_Ph2O_publ
_cod_database_code               1555270
_shelx_shelxl_version_number     2014/7
_shelx_estimated_absorpt_t_max   0.998
_shelx_estimated_absorpt_t_min   0.992
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
2. Restrained distances
 O17-H17 = O14-H14 = O1-H1 = O16-H16 = O8-H8 = O9-H9 = O3-H3 = O12-H12 = O6-H6
 0.82 with sigma of 0.02
 C16-H8
 1.79 with sigma of 0.04
3. Rigid body (RIGU) restrains
 O20, C40, C46, C41, C45, C47, C51, C42, C44, C48, C50, C43, C49
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 O19, C28, C34, C29, C33, C35, C39, C30, C32, C36, C38, C31, C37
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
4.a Aromatic/amide H refined with riding coordinates:
 C29(H29), C30(H30), C31(H31), C32(H32), C33(H33), C35(H35), C36(H36),
 C37(H37), C38(H38), C39(H39), C45(H45), C44(H44), C43(H43), C42(H42), C41(H41),
  C47(H47), C48(H48), C49(H49), C50(H50), C51(H51)
4.b Fitted hexagon refined as free rotating group:
 C40(C45,C44,C43,C42,C41)
;
_shelx_res_checksum              8088
_olex2_submission_special_instructions 'No special instructions were received'