First domino radical cyclisation/Smiles rearrangement combination
Marc Pudlo; Ingrid Allart-Simon; Bernard Tinant; Stephane Gerard; Janos Sapi; Chem.Commun. 48 (2012) 2442–; doi:10.1039/c2cc15670a

data_7107400
_publ_section_title
;
 First domino radical cyclisation/Smiles rearrangement combination
;
_journal_name_full               Chem.Commun.
_journal_page_first              2442
_journal_paper_doi               10.1039/c2cc15670a
_journal_volume                  48
_journal_year                    2012
_chemical_formula_sum            'C18 H19 Cl N2 O2'
_chemical_formula_weight         330.80
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                88.77(2)
_cell_angle_beta                 72.15(2)
_cell_angle_gamma                77.04(2)
_cell_formula_units_Z            2
_cell_length_a                   9.071(3)
_cell_length_b                   9.395(3)
_cell_length_c                   10.422(3)
_cell_measurement_reflns_used    all
_cell_measurement_temperature    296(2)
_cell_measurement_theta_max      25.3
_cell_measurement_theta_min      3.1
_cell_volume                     822.8(5)
_computing_cell_refinement       MAR
_computing_data_collection       MAR
_computing_data_reduction        MAR
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      296(2)
_diffrn_detector_area_resol_mean 6.66
_diffrn_measured_fraction_theta_full 0.922
_diffrn_measured_fraction_theta_max 0.922
_diffrn_measurement_device_type  'MAR345 image plate'
_diffrn_measurement_method       '178 images, \D\F 3\%'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'RU200 rotating anode'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71069
_diffrn_reflns_av_R_equivalents  0.038
_diffrn_reflns_av_sigmaI/netI    0.0320
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       0
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_k_min       -10
_diffrn_reflns_limit_l_max       12
_diffrn_reflns_limit_l_min       -11
_diffrn_reflns_number            15453
_diffrn_reflns_theta_full        25.37
_diffrn_reflns_theta_max         25.37
_diffrn_reflns_theta_min         3.11
_exptl_absorpt_coefficient_mu    0.243
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.335
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       bloc
_exptl_crystal_F_000             348
_exptl_crystal_size_max          0.40
_exptl_crystal_size_mid          0.20
_exptl_crystal_size_min          0.20
_refine_diff_density_max         0.346
_refine_diff_density_min         -0.380
_refine_diff_density_rms         0.096
_refine_ls_extinction_coef       0.26(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   1.074
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     237
_refine_ls_number_reflns         2792
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.074
_refine_ls_R_factor_all          0.0733
_refine_ls_R_factor_gt           0.0675
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.1143P)^2^+0.3169P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1853
_refine_ls_wR_factor_ref         0.1944
_reflns_number_gt                2503
_reflns_number_total             2792
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c2cc15670a.txt
_cod_data_source_block           sg144
_cod_original_cell_volume        822.8(4)
_cod_original_sg_symbol_H-M      ' P -1 '
_cod_database_code               7107400