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_1564385
_publ_section_title
;
 \b-Trioxopyrrocorphins: Pyrrocorphins of graded aromaticity
;
_journal_name_full               'Chemical Science'
_journal_paper_doi               10.1039/D1SC03403K
_journal_year                    2021
_chemical_formula_sum            'C41 H49 N5 O3 Zn'
_chemical_formula_weight         725.22
_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
_atom_sites_solution_primary     dual
_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                67.041(2)
_cell_angle_beta                 88.923(2)
_cell_angle_gamma                78.976(2)
_cell_formula_units_Z            4
_cell_length_a                   12.0722(6)
_cell_length_b                   18.1055(9)
_cell_length_c                   19.2232(10)
_cell_measurement_reflns_used    9309
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      33.0431
_cell_measurement_theta_min      2.4937
_cell_volume                     3790.2(3)
_computing_cell_refinement       'SAINT V8.40B (Bruker, 2020)'
_computing_data_collection       'Apex3 v2019.11-0 (Bruker, 2020)'
_computing_data_reduction        'SAINT V8.40B (Bruker, 2020)'
_computing_structure_refinement
;  
SHELXL-2018/3 (Sheldrick, 2015, 2018), 
SHELXLE Rev1215 (H\"ubschle et al., 2011)
;
_computing_structure_solution    'SHELXT (Sheldrick, 2015)'
_diffrn_ambient_temperature      150(2)
_diffrn_detector_area_resol_mean 7.4074
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.996
_diffrn_measurement_device_type
;
Bruker AXS D8 Quest diffractometer with PhotonII charge-integrating pixel 
array detector (CPAD)
;
_diffrn_measurement_method       'omega and phi scans'
_diffrn_radiation_monochromator  'Triumph curved graphite crystal'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0445
_diffrn_reflns_av_unetI/netI     0.0238
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.996
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_h_min       -18
_diffrn_reflns_limit_k_max       27
_diffrn_reflns_limit_k_min       -27
_diffrn_reflns_limit_l_max       29
_diffrn_reflns_limit_l_min       -29
_diffrn_reflns_number            277906
_diffrn_reflns_point_group_measured_fraction_full 0.997
_diffrn_reflns_point_group_measured_fraction_max 0.996
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         33.232
_diffrn_reflns_theta_min         2.012
_diffrn_source                   'fine focus sealed tube X-ray source'
_diffrn_source_current           '30 mA'
_diffrn_source_voltage           '50 kV'
_exptl_absorpt_coefficient_mu    0.692
_exptl_absorpt_correction_T_max  0.7465
_exptl_absorpt_correction_T_min  0.6939
_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    1.271
_exptl_crystal_description       block
_exptl_crystal_F_000             1536
_exptl_crystal_size_max          0.410
_exptl_crystal_size_mid          0.230
_exptl_crystal_size_min          0.170
_refine_diff_density_max         1.330
_refine_diff_density_min         -1.396
_refine_diff_density_rms         0.077
_refine_ls_extinction_coef       0.0031(5)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     'SHELXL-2018/3 (Sheldrick 2018)'
_refine_ls_goodness_of_fit_ref   1.084
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1029
_refine_ls_number_reflns         29002
_refine_ls_number_restraints     284
_refine_ls_restrained_S_all      1.083
_refine_ls_R_factor_all          0.0752
_refine_ls_R_factor_gt           0.0583
_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^)+(0.0597P)^2^+4.6782P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1561
_refine_ls_wR_factor_ref         0.1677
_reflns_Friedel_coverage         0.000
_reflns_number_gt                22766
_reflns_number_total             29002
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d1sc03403k2.cif
_cod_data_source_block           8-O2-7-18Zn-pyridine
_cod_database_code               1564385
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_min   0.765
_shelx_estimated_absorpt_t_max   0.891
_shelx_res_checksum              6156
_shelx_hkl_checksum              32121