Orchestrated catalytic double rollover annulation: Rapid access to N-enriched cationic and neutral PAHs
Karak, Pirudhan; Dutta, Champak; Dutta, Tanoy; Koner, Apurba Lal; Choudhury, Joyanta; Chemical Communications  (2019) –; doi:10.1039/C9CC02710F

data_7123498
_publ_section_title
;
 Orchestrated catalytic double rollover annulation: Rapid access to
 N-enriched cationic and neutral PAHs
;
_journal_name_full               'Chemical Communications'
_journal_paper_doi               10.1039/C9CC02710F
_journal_year                    2019
_chemical_formula_sum            'C40 H28 Cl3 F3 N2 O3 S'
_chemical_formula_weight         780.05
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2yn'
_space_group_name_H-M_alt        'P 1 21/n 1'
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 1'
_atom_sites_solution_hydrogens   geom
_audit_block_doi                 10.5517/cc141prm
_audit_creation_method           SHELXL-2014
_audit_update_record
;
2015-09-18 deposited with the CCDC.    2019-05-20 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 103.677(9)
_cell_angle_gamma                90
_cell_formula_units_Z            4
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_cell_length_b                   9.628(4)
_cell_length_c                   24.030(10)
_cell_measurement_reflns_used    6323
_cell_measurement_temperature    273(2)
_cell_measurement_theta_max      25.000
_cell_measurement_theta_min      1.394
_cell_volume                     3588(3)
_computing_cell_refinement       'Bruker XSCANS'
_computing_data_collection       'Bruker XSCANS'
_computing_data_reduction        'Bruker SHELXTL'
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_computing_structure_refinement  'SHELXL-2014 (Sheldrick, 2014)'
_computing_structure_solution    SIR-92
_diffrn_ambient_temperature      273(2)
_diffrn_measured_fraction_theta_full 0.974
_diffrn_measured_fraction_theta_max 1.000
_diffrn_measurement_device_type  'Bruker P4'
_diffrn_measurement_method       '\w scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.3718
_diffrn_reflns_av_unetI/netI     0.2263
_diffrn_reflns_Laue_measured_fraction_full 0.974
_diffrn_reflns_Laue_measured_fraction_max 1.000
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_h_min       -18
_diffrn_reflns_limit_k_max       11
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_diffrn_reflns_limit_l_max       28
_diffrn_reflns_limit_l_min       -28
_diffrn_reflns_number            82361
_diffrn_reflns_point_group_measured_fraction_full 0.974
_diffrn_reflns_point_group_measured_fraction_max 1.000
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         25.000
_diffrn_reflns_theta_min         1.394
_diffrn_source                   'sealed tube'
_exptl_absorpt_coefficient_mu    0.372
_exptl_absorpt_correction_T_max  0.967
_exptl_absorpt_correction_T_min  0.936
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   SADABS
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.444
_exptl_crystal_description       prism
_exptl_crystal_F_000             1600
_exptl_crystal_size_max          0.180
_exptl_crystal_size_mid          0.130
_exptl_crystal_size_min          0.090
_refine_diff_density_max         0.719
_refine_diff_density_min         -0.607
_refine_diff_density_rms         0.167
_refine_ls_extinction_coef       0.021(4)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     SHELXL
_refine_ls_goodness_of_fit_ref   1.090
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     470
_refine_ls_number_reflns         6323
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.090
_refine_ls_R_factor_all          0.3457
_refine_ls_R_factor_gt           0.1452
_refine_ls_shift/su_max          0.175
_refine_ls_shift/su_mean         0.016
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.2000P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.3339
_refine_ls_wR_factor_ref         0.4242
_reflns_Friedel_coverage         0.000
_reflns_number_gt                2103
_reflns_number_total             6323
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c9cc02710f2.cif
_cod_data_source_block           shelx
_cod_database_code               7123498
_shelx_estimated_absorpt_t_min   0.936
_shelx_estimated_absorpt_t_max   0.967
_shelxl_version_number           2014-3
_shelx_res_checksum              26515
_shelx_hkl_checksum              11282