Electrooxidative tricyclic 6–7–6 fused-system domino assembly to allocolchicines by a removable radical strategy
Zhang, Yan; Ma, Chanchan; Cai, Zhenzhi; Struwe, Julia; Chen, Shengjie; Xu, Jinming; Li, Shiyin; Zeng, Wangyu; Ackermann, Lutz; Green Chemistry 24 (2022) 3697–3703; doi:10.1039/D2GC00684G

data_7244845
_publ_section_title
;
 Electrooxidative tricyclic 6--7--6 fused-system domino assembly to
 allocolchicines by a removable radical strategy
;
_journal_issue                   9
_journal_name_full               'Green Chemistry'
_journal_page_first              3697
_journal_page_last               3703
_journal_paper_doi               10.1039/D2GC00684G
_journal_volume                  24
_journal_year                    2022
_chemical_formula_sum            'C31 H26 O6 S'
_chemical_formula_weight         526.58
_space_group_crystal_system      monoclinic
_space_group_IT_number           15
_space_group_name_Hall           '-C 2yc'
_space_group_name_H-M_alt        'C 1 2/c 1'
_atom_sites_solution_hydrogens   geom
_audit_creation_method           SHELXL-2014/7
_audit_update_record
;
2021-11-28 deposited with the CCDC.	2022-03-10 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 100.316(2)
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   34.743(2)
_cell_length_b                   7.6413(3)
_cell_length_c                   19.9522(11)
_cell_measurement_reflns_used    6420
_cell_measurement_temperature    299(2)
_cell_measurement_theta_max      27.47
_cell_measurement_theta_min      2.57
_cell_volume                     5211.3(5)
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_diffrn_ambient_temperature      299(2)
_diffrn_measured_fraction_theta_full 0.993
_diffrn_measured_fraction_theta_max 0.990
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0757
_diffrn_reflns_av_unetI/netI     0.0513
_diffrn_reflns_Laue_measured_fraction_full 0.993
_diffrn_reflns_Laue_measured_fraction_max 0.990
_diffrn_reflns_limit_h_max       44
_diffrn_reflns_limit_h_min       -39
_diffrn_reflns_limit_k_max       9
_diffrn_reflns_limit_k_min       -9
_diffrn_reflns_limit_l_max       25
_diffrn_reflns_limit_l_min       -25
_diffrn_reflns_number            20203
_diffrn_reflns_point_group_measured_fraction_full 0.993
_diffrn_reflns_point_group_measured_fraction_max 0.990
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.490
_diffrn_reflns_theta_min         2.571
_exptl_absorpt_coefficient_mu    0.169
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.342
_exptl_crystal_description       block
_exptl_crystal_F_000             2208
_exptl_crystal_size_max          .26
_exptl_crystal_size_mid          .18
_exptl_crystal_size_min          .16
_refine_diff_density_max         0.327
_refine_diff_density_min         -0.367
_refine_diff_density_rms         0.048
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.035
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     343
_refine_ls_number_reflns         5908
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.035
_refine_ls_R_factor_all          0.0750
_refine_ls_R_factor_gt           0.0550
_refine_ls_shift/su_max          0.031
_refine_ls_shift/su_mean         0.004
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0725P)^2^+3.9726P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1407
_refine_ls_wR_factor_ref         0.1597
_reflns_Friedel_coverage         0.000
_reflns_number_gt                4474
_reflns_number_total             5908
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d2gc00684g2.cif
_cod_data_source_block           a_CCDC1
_cod_depositor_comments
'Adding full bibliography for 7244844--7244845.cif.'
_cod_original_sg_symbol_H-M      'C 2/c'
_cod_database_code               7244845
_shelx_shelxl_version_number     2014/7
_shelx_res_checksum              16348
_shelx_hkl_checksum              41182