Solvent Controlled Racemic Resolution of C3-Symmetric Trihydroxytribenzotriquinacenes.
Wagner, Philippe; Rominger, Frank; Oeser, Thomas; Mastalerz, Michael; The Journal of organic chemistry  (2020) –; doi:10.1021/acs.joc.9b03410

data_4037901
_publ_section_title
;
 Solvent Controlled Racemic Resolution of C3-Symmetric
 Trihydroxytribenzotriquinacenes.
;
_journal_name_full               'The Journal of organic chemistry'
_journal_paper_doi               10.1021/acs.joc.9b03410
_journal_year                    2020
_chemical_formula_sum            'C32 H30 Br6 O3'
_chemical_formula_weight         942.02
_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   geom
_audit_creation_method           SHELXL-2018/3
_cell_angle_alpha                81.8372(15)
_cell_angle_beta                 83.7120(15)
_cell_angle_gamma                64.6173(13)
_cell_formula_units_Z            2
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_cell_length_b                   11.2035(10)
_cell_length_c                   15.5435(14)
_cell_measurement_reflns_used    9786
_cell_measurement_temperature    200(2)
_cell_measurement_theta_max      28.08
_cell_measurement_theta_min      2.24
_cell_volume                     1570.1(2)
_computing_cell_refinement       'Bruker SAINT'
_computing_data_collection       'Bruker APEX2'
_computing_data_reduction        'Bruker SAINT'
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_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-2018/3 (Sheldrick, 2018)'
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_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.921
_diffrn_measurement_device_type  'Bruker APEX-II Quazar area detector'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0388
_diffrn_reflns_av_unetI/netI     0.0418
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.921
_diffrn_reflns_limit_h_max       14
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_diffrn_reflns_limit_l_max       21
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_diffrn_reflns_number            31594
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.921
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         29.916
_diffrn_reflns_theta_min         1.325
_diffrn_source                   'ImuS microsource'
_exptl_absorpt_coefficient_mu    7.705
_exptl_absorpt_correction_T_max  0.8374
_exptl_absorpt_correction_T_min  0.6919
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
Sheldrick, G. M. (2008). <i>SADABS</i>. University of G\"ottingen, Germany.
;
_exptl_crystal_colour            brown
_exptl_crystal_density_diffrn    1.993
_exptl_crystal_description       plank
_exptl_crystal_F_000             912
_exptl_crystal_size_max          0.080
_exptl_crystal_size_mid          0.068
_exptl_crystal_size_min          0.028
_refine_diff_density_max         1.355
_refine_diff_density_min         -0.665
_refine_diff_density_rms         0.123
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.020
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     380
_refine_ls_number_reflns         8372
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.020
_refine_ls_R_factor_all          0.0642
_refine_ls_R_factor_gt           0.0377
_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^)+(0.0548P)^2^+0.5485P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0897
_refine_ls_wR_factor_ref         0.0999
_reflns_Friedel_coverage         0.000
_reflns_number_gt                6091
_reflns_number_total             8372
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            jo9b03410_si_002.cif
_cod_data_source_block           phw25
_cod_database_code               4037901
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_min   0.578
_shelx_estimated_absorpt_t_max   0.813
_shelx_res_checksum              65476
_shelx_hkl_checksum              76255