Metal-Assisted Ring-Closing/Opening Process of a Chiral Tetrahydroquinazoline
Ana M. García-Deibe; Jesús Sanmartín-Matalobos; Concepción González-Bello; Emilio Lence; Cristina Portela-García; Luis Martínez-Rodríguez; Matilde Fondo; Inorganic Chemistry 51 (2012) 1278–1293; doi:10.1021/ic2017038

data_4328136
_publ_section_title
;
 Metal-Assisted Ring-Closing/Opening Process of a Chiral
 Tetrahydroquinazoline
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              1278
_journal_page_last               1293
_journal_paper_doi               10.1021/ic2017038
_journal_volume                  51
_journal_year                    2012
_chemical_formula_moiety         'C24 H19  N3 O3 Pd S, C H2 Cl2'
_chemical_formula_sum            'C25 H21 Cl2 N3 O3 Pd S'
_chemical_formula_weight         620.81
_space_group_IT_number           61
_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_Hall  '-P 2ac 2ab'
_symmetry_space_group_name_H-M   'P b c a'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                90.00
_cell_formula_units_Z            8
_cell_length_a                   9.6380(4)
_cell_length_b                   19.9218(7)
_cell_length_c                   25.9126(9)
_cell_measurement_reflns_used    2731
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      17.796
_cell_measurement_theta_min      2.1905
_cell_volume                     4975.4(3)
_computing_cell_refinement       'BRUKER APEX2(Bruker, 2010)'
_computing_data_collection       'BRUKER APEX2(Bruker, 2010)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 1.000
_diffrn_measurement_device_type  'Bruker X8 Kappa APEXII'
_diffrn_measurement_method       'omega nad phi scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0815
_diffrn_reflns_av_sigmaI/netI    0.1043
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       0
_diffrn_reflns_limit_k_max       24
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       31
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_number            109274
_diffrn_reflns_theta_full        25.35
_diffrn_reflns_theta_max         25.35
_diffrn_reflns_theta_min         1.57
_exptl_absorpt_coefficient_mu    1.078
_exptl_absorpt_correction_T_max  1.0000
_exptl_absorpt_correction_T_min  0.8458
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS (Bruker 2008)'
_exptl_crystal_colour            brown
_exptl_crystal_density_diffrn    1.658
_exptl_crystal_description       needle
_exptl_crystal_F_000             2496
_exptl_crystal_size_max          0.34
_exptl_crystal_size_mid          0.08
_exptl_crystal_size_min          0.01
_refine_diff_density_max         0.708
_refine_diff_density_min         -0.960
_refine_diff_density_rms         0.148
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.018
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     317
_refine_ls_number_reflns         4556
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.018
_refine_ls_R_factor_all          0.1306
_refine_ls_R_factor_gt           0.0549
_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^)+(0.0441P)^2^+9.9668P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0952
_refine_ls_wR_factor_ref         0.1241
_reflns_number_gt                2586
_reflns_number_total             4556
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic2017038_si_001_4.cif
_cod_data_source_block           Pd(Li).CH2Cl2
_cod_original_cell_volume        4975.5
_cod_database_code               4328136