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_1564383
_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_moiety
'C41 H49 N5 O3 Zn, 1.562(C H4 O), 0.657(H2 O)'
_chemical_formula_sum            'C42.56 H56.56 N5 O5.22 Zn'
_chemical_formula_weight         787.09
_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
_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                89.825(5)
_cell_angle_beta                 87.094(6)
_cell_angle_gamma                82.139(5)
_cell_formula_units_Z            2
_cell_length_a                   10.7675(10)
_cell_length_b                   11.1454(13)
_cell_length_c                   17.315(2)
_cell_measurement_reflns_used    7884
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      80.0136
_cell_measurement_theta_min      4.7373
_cell_volume                     2055.8(4)
_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 Rev1183 (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 0.980
_diffrn_measured_fraction_theta_max 0.911
_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  0.0497
_diffrn_reflns_av_unetI/netI     0.0574
_diffrn_reflns_Laue_measured_fraction_full 0.980
_diffrn_reflns_Laue_measured_fraction_max 0.911
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            19177
_diffrn_reflns_point_group_measured_fraction_full 0.980
_diffrn_reflns_point_group_measured_fraction_max 0.911
_diffrn_reflns_theta_full        67.679
_diffrn_reflns_theta_max         80.176
_diffrn_reflns_theta_min         4.743
_diffrn_source                   'I-mu-S microsource X-ray tube'
_diffrn_source_current           '1.0 mA'
_diffrn_source_voltage           '50 kV'
_exptl_absorpt_coefficient_mu    1.226
_exptl_absorpt_correction_T_max  0.7543
_exptl_absorpt_correction_T_min  0.6078
_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            black
_exptl_crystal_density_diffrn    1.272
_exptl_crystal_description       block
_exptl_crystal_F_000             837.4
_exptl_crystal_size_max          0.190
_exptl_crystal_size_mid          0.170
_exptl_crystal_size_min          0.110
_refine_diff_density_max         0.883
_refine_diff_density_min         -0.736
_refine_diff_density_rms         0.068
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.050
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     527
_refine_ls_number_reflns         8185
_refine_ls_number_restraints     60
_refine_ls_restrained_S_all      1.056
_refine_ls_R_factor_all          0.0674
_refine_ls_R_factor_gt           0.0532
_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^)+(0.0569P)^2^+2.3554P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1338
_refine_ls_wR_factor_ref         0.1428
_reflns_Friedel_coverage         0.000
_reflns_number_gt                6640
_reflns_number_total             8185
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d1sc03403k2.cif
_cod_data_source_block           8-O2-7-12Zn-pyridine
_cod_original_cell_volume        2055.7(4)
_cod_database_code               1564383
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_min   0.800
_shelx_estimated_absorpt_t_max   0.877
_shelx_res_checksum              21449
_shelx_hkl_checksum              39846