Pd-Catalyzed Regioselective Rollover Dual C-H Annulation Cascade: Facile Approach to phenanthrene derivatives
Naveen Kumar, Muniganti; Suresh, Vavilapalli; Nagi Reddy, Attunuri; Nanubolu, Jagadesh Babu; Maddi, Sridhar Reddy; Chemical Communications  (2023) –; doi:10.1039/D3CC02523C

data_7131807
_publ_section_title
;
 Pd-Catalyzed Regioselective Rollover Dual C-H Annulation Cascade: Facile
 Approach to phenanthrene derivatives
;
_journal_name_full               'Chemical Communications'
_journal_paper_doi               10.1039/D3CC02523C
_journal_year                    2023
_chemical_formula_moiety         '4(C18 H14 O3), C3 H6 O'
_chemical_formula_sum            'C75 H62 O13'
_chemical_formula_weight         1171.24
_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
_audit_creation_method           SHELXL-2018/3
_audit_update_record
;
2023-04-07 deposited with the CCDC.	2023-06-30 downloaded from the CCDC.
;
_cell_angle_alpha                86.075(6)
_cell_angle_beta                 79.905(4)
_cell_angle_gamma                71.038(4)
_cell_formula_units_Z            1
_cell_length_a                   10.0982(19)
_cell_length_b                   11.617(3)
_cell_length_c                   13.448(3)
_cell_measurement_reflns_used    9854
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      30.492
_cell_measurement_theta_min      2.442
_cell_volume                     1468.8(6)
_computing_cell_refinement       '<i>SAINT</i> (Bruker, 2016)'
_computing_data_collection       '<i>APEX3</i> (Bruker, 2016)'
_computing_data_reduction        'Bruker SAINT'
_computing_structure_refinement  'SHELXL-2018/3 (Sheldrick, 2018)'
_computing_structure_solution    'SHELXT 2018/2 (Sheldrick, 2018)'
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 0.976
_diffrn_measured_fraction_theta_max 0.981
_diffrn_measurement_device_type  'Bruker D8 QUEST PHOTON III C7 HPAD'
_diffrn_measurement_method       '\w and \f'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0362
_diffrn_reflns_av_unetI/netI     0.0284
_diffrn_reflns_Laue_measured_fraction_full 0.976
_diffrn_reflns_Laue_measured_fraction_max 0.981
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            36590
_diffrn_reflns_point_group_measured_fraction_full 0.976
_diffrn_reflns_point_group_measured_fraction_max 0.981
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.500
_diffrn_reflns_theta_min         2.357
_diffrn_source                   microfocus
_exptl_absorpt_coefficient_mu    0.090
_exptl_absorpt_correction_T_max  0.7461
_exptl_absorpt_correction_T_min  0.6892
_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            COLORLESS
_exptl_crystal_density_diffrn    1.324
_exptl_crystal_description       PLATE
_exptl_crystal_F_000             616
_exptl_crystal_recrystallization_method
'Re-crystallisation from solvent: Acetone'
_exptl_crystal_size_max          0.280
_exptl_crystal_size_mid          0.240
_exptl_crystal_size_min          0.150
_refine_diff_density_max         0.375
_refine_diff_density_min         -0.189
_refine_diff_density_rms         0.036
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.030
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     425
_refine_ls_number_reflns         6612
_refine_ls_number_restraints     28
_refine_ls_restrained_S_all      1.050
_refine_ls_R_factor_all          0.0694
_refine_ls_R_factor_gt           0.0525
_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^)+(0.0651P)^2^+0.5621P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1296
_refine_ls_wR_factor_ref         0.1447
_reflns_Friedel_coverage         0.000
_reflns_number_gt                5106
_reflns_number_total             6612
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d3cc02523c2.cif
_cod_data_source_block           KB693_0m
_cod_original_cell_volume        1468.8(5)
_cod_database_code               7131807
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_min   0.975
_shelx_estimated_absorpt_t_max   0.987
_shelx_res_checksum              7144
_shelx_hkl_checksum              64529