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_1555259
_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         'C14 H20 O8, 8.75(O)'
_chemical_formula_sum            'C14 H20 O16.75'
_chemical_formula_weight         456.30
_space_group_crystal_system      cubic
_space_group_IT_number           201
_space_group_name_Hall           '-P 2ab 2bc 3'
_space_group_name_H-M_alt        'P n -3 :2'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_audit_creation_date             2019-05-07
_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            2
_cell_length_a                   11.4074(5)
_cell_length_b                   11.4074(5)
_cell_length_c                   11.4074(5)
_cell_measurement_reflns_used    6150
_cell_measurement_temperature    200
_cell_measurement_theta_max      29.768
_cell_measurement_theta_min      2.525
_cell_volume                     1484.43(11)
_computing_cell_refinement       'SAINT v8.34A (Bruker, 2013)'
_computing_data_collection
'CrystalClear-SM Expert 2.0 r7 (Rigaku, 2011)'
_computing_data_reduction        'SAINT v8.34A (Bruker, 2013)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'XL (Sheldrick, 2008)'
_computing_structure_solution    'ShelXT (Sheldrick, 2015)'
_diffrn_ambient_temperature      200
_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_device       'AFC12 (Right): Kappa 3 circle'
_diffrn_measurement_device_type  'Rigaku Saturn724+ (2x2 bin mode)'
_diffrn_measurement_method       'profile data from \w-scans'
_diffrn_measurement_specimen_support 'Mitegen 50um'
_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  0.0579
_diffrn_reflns_av_unetI/netI     0.0236
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 1.000
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       14
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_number            15739
_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         30.472
_diffrn_reflns_theta_min         1.785
_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
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.097
_exptl_absorpt_correction_T_max  0.7461
_exptl_absorpt_correction_T_min  0.4751
_exptl_absorpt_correction_type   multi-scan
_exptl_crystal_colour            colourless
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.021
_exptl_crystal_description       prism
_exptl_crystal_F_000             476
_exptl_crystal_size_max          0.397
_exptl_crystal_size_mid          0.385
_exptl_crystal_size_min          0.379
_refine_diff_density_max         0.338
_refine_diff_density_min         -0.420
_refine_diff_density_rms         0.110
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.196
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     76
_refine_ls_number_reflns         761
_refine_ls_number_restraints     36
_refine_ls_restrained_S_all      1.271
_refine_ls_R_factor_all          0.0928
_refine_ls_R_factor_gt           0.0859
_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^)+(0.1422P)^2^+0.1067P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2151
_refine_ls_wR_factor_ref         0.2255
_reflns_Friedel_coverage         0.000
_reflns_number_gt                656
_reflns_number_total             761
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c9sc02832c2.cif
_cod_data_source_block           ADTA_2-27_THF_oX_100K_2-fold_publ
_cod_original_cell_volume        1484.4(2)
_cod_original_sg_symbol_H-M      'P n -3'
_cod_database_code               1555259
_shelx_shelxl_version_number     2014/7
_shelx_estimated_absorpt_t_max   0.964
_shelx_estimated_absorpt_t_min   0.963
_olex2_refinement_description
;
1. Twinned data refinement
 Scales: 0.506(13)
 0.494(13)
2. Fixed Uiso
 At 1.2 times of:
  All C(H,H) groups
 At 1.5 times of:
  All O(H) groups
3. Restrained distances
 H1-H2_$1
 2.1 with sigma of 0.04
 H2-H1_$2
 2.1 with sigma of 0.04
4. Restrained planarity
 H2_$1, O2_$1, C3, O1, H1
 with sigma of 0.001
 H2, O2, C3, O1_$2, H1_$2
 with sigma of 0.001
5. Uiso/Uaniso restraints and constraints
Uanis(O5S) \\sim Ueq, Uanis(O4S) \\sim Ueq, Uanis(O2S) \\sim Ueq, Uanis(O3S)
\\sim Ueq, Uanis(O1S) \\sim Ueq: with sigma of 0.01 and sigma for terminal
atoms of 0.02
6. Others
 Fixed Sof: O1(0.33333) H1(0.33333) O2(0.33333) H2(0.33333) H1A(0.5) H1B(0.5)
 O1S(0.125) O2S(0.125) O3S(0.125) O4S(0.25) O5S(0.04167) O6S(0.0625)
7.a Secondary CH2 refined with riding coordinates:
 C1(H1A,H1B)
7.b Idealised tetrahedral OH refined as rotating group:
 O1(H1), O2(H2)
;
_shelx_res_checksum              59100
_olex2_submission_special_instructions 'No special instructions were received'