β-Trioxopyrrocorphins: Pyrrocorphins of graded aromaticity
Chaudhri, Nivedita; Guberman-Pfeffer, Matthew J.; Li, Ruoshi; Zeller, Matthias; Brückner, Christian; Chemical Science  (2021) –; doi:10.1039/D1SC03403K

data_1564384
_publ_section_title
;
 \b-Trioxopyrrocorphins: Pyrrocorphins of graded aromaticity
;
_journal_name_full               'Chemical Science'
_journal_paper_doi               10.1039/D1SC03403K
_journal_year                    2021
_chemical_absolute_configuration ukn
_chemical_formula_moiety         'C36 H46 N4 O3, 0.323(C H4 O)'
_chemical_formula_sum            'C36.32 H47.29 N4 O3.32'
_chemical_formula_weight         593.12
_space_group_crystal_system      monoclinic
_space_group_IT_number           7
_space_group_name_Hall           'P -2yc'
_space_group_name_H-M_alt        'P 1 c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-2018/3
_audit_update_record
;
2021-02-24 deposited with the CCDC.	2021-08-19 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90.0171(16)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   12.2252(4)
_cell_length_b                   12.1333(4)
_cell_length_c                   22.9886(8)
_cell_measurement_reflns_used    9928
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      78.9748
_cell_measurement_theta_min      3.6429
_cell_volume                     3409.9(2)
_computing_cell_refinement       'SAINT V8.40A (Bruker, 2019)'
_computing_data_collection       'Apex3 v2019.1-0 (Bruker, 2019)'
_computing_data_reduction        'SAINT V8.40A (Bruker, 2019)'
_computing_structure_refinement
;  
SHELXL-2018/3 (Sheldrick, 2015, 2018), 
SHELXLE Rev1117 (H\"ubschle et al., 2011)
;
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      150(2)
_diffrn_detector_area_resol_mean 7.4074
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.957
_diffrn_measurement_device_type
;
Bruker AXS D8 Quest diffractometer with PhotonIII_C14 charge-integrating and 
photon counting pixel array detector
;
_diffrn_measurement_method       'omega and phi scans'
_diffrn_radiation_monochromator  'laterally graded multilayer (Goebel) mirror'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54178
_diffrn_reflns_av_R_equivalents  0.0433
_diffrn_reflns_av_unetI/netI     0.0601
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.957
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       29
_diffrn_reflns_limit_l_min       -28
_diffrn_reflns_number            36871
_diffrn_reflns_point_group_measured_fraction_full 0.958
_diffrn_reflns_point_group_measured_fraction_max 0.885
_diffrn_reflns_theta_full        67.679
_diffrn_reflns_theta_max         79.933
_diffrn_reflns_theta_min         1.922
_diffrn_source                   'I-mu-S microsource X-ray tube'
_diffrn_source_current           '1.0 mA'
_diffrn_source_voltage           '50 kV'
_exptl_absorpt_coefficient_mu    0.586
_exptl_absorpt_correction_T_max  0.7542
_exptl_absorpt_correction_T_min  0.6826
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
 SADABS 2016/2: Krause, L., Herbst-Irmer, R., Sheldrick G.M. & Stalke D.,
 J. Appl. Cryst. 48 (2015) 3-10
;
_exptl_crystal_colour            green
_exptl_crystal_density_diffrn    1.155
_exptl_crystal_description       flake
_exptl_crystal_F_000             1279.3
_exptl_crystal_size_max          0.140
_exptl_crystal_size_mid          0.120
_exptl_crystal_size_min          0.030
_refine_diff_density_max         0.421
_refine_diff_density_min         -0.200
_refine_diff_density_rms         0.042
_refine_ls_abs_structure_details
;
 Flack x determined using 5161 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   0.46(10)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.061
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     851
_refine_ls_number_reflns         13171
_refine_ls_number_restraints     99
_refine_ls_restrained_S_all      1.072
_refine_ls_R_factor_all          0.0490
_refine_ls_R_factor_gt           0.0463
_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^)+(0.0686P)^2^+0.1612P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1172
_refine_ls_wR_factor_ref         0.1197
_reflns_Friedel_coverage         0.847
_reflns_Friedel_fraction_full    0.919
_reflns_Friedel_fraction_max     0.812
_reflns_number_gt                12382
_reflns_number_total             13171
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d1sc03403k2.cif
_cod_data_source_block           8-O2-7-18
_cod_original_sg_symbol_H-M      'P c'
_cod_database_code               1564384
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_min   0.922
_shelx_estimated_absorpt_t_max   0.983
_shelx_res_checksum              8638
_shelx_hkl_checksum              57114