Dibenzocycloheptanones construction through a removable P-centered radical: Synthesis of allocolchicine analogues
Zhang, Yan; Cai, Zhenzhi; Struwe, Julia; Ma, Chanchan; Zhu, Gangguo; Liao, Xinyi; Xu, Min; Ackermann, Lutz; Chemical Science  (2021) –; doi:10.1039/D1SC05404J

data_1565141
_publ_section_title
;
 Dibenzocycloheptanones construction through a removable P-centered
 radical: Synthesis of allocolchicine analogues
;
_journal_name_full               'Chemical Science'
_journal_paper_doi               10.1039/D1SC05404J
_journal_year                    2021
_chemical_formula_sum            'C29 H30 Cl O4 P'
_chemical_formula_weight         508.95
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2ybc'
_space_group_name_H-M_alt        'P 1 21/c 1'
_atom_sites_solution_hydrogens   geom
_audit_creation_method           SHELXL-2014/7
_audit_update_record
;
2021-08-18 deposited with the CCDC.	2021-11-09 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 110.584(2)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   12.1391(8)
_cell_length_b                   13.8283(9)
_cell_length_c                   17.2219(10)
_cell_measurement_reflns_used    9898
_cell_measurement_temperature    176(2)
_cell_measurement_theta_max      27.25
_cell_measurement_theta_min      2.32
_cell_volume                     2706.4(3)
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_diffrn_ambient_temperature      176(2)
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device_type  APEXII
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0774
_diffrn_reflns_av_unetI/netI     0.0282
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_number            73973
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.511
_diffrn_reflns_theta_min         2.320
_exptl_absorpt_coefficient_mu    0.232
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.249
_exptl_crystal_description       block
_exptl_crystal_F_000             1072
_exptl_crystal_size_max          .20
_exptl_crystal_size_mid          .20
_exptl_crystal_size_min          .16
_refine_diff_density_max         0.764
_refine_diff_density_min         -0.495
_refine_diff_density_rms         0.134
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.093
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     316
_refine_ls_number_reflns         6215
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.093
_refine_ls_R_factor_all          0.0785
_refine_ls_R_factor_gt           0.0562
_refine_ls_shift/su_max          0.043
_refine_ls_shift/su_mean         0.006
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.1381P)^2^+0.1784P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2014
_refine_ls_wR_factor_ref         0.2179
_reflns_Friedel_coverage         0.000
_reflns_number_gt                4293
_reflns_number_total             6215
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d1sc05404j2.cif
_cod_data_source_block           a
_cod_original_sg_symbol_H-M      'P 21/c'
_cod_database_code               1565141
_shelx_shelxl_version_number     2014/7
_shelx_res_checksum              22357
_shelx_hkl_checksum              32118