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_4328134
_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         'C48 H40 N6 Ni O6 S2, 2(C2 H4 O2)'
_chemical_formula_sum            'C52 H48 N6 Ni O10 S2'
_chemical_formula_weight         1039.79
_space_group_IT_number           15
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-C 2yc'
_symmetry_space_group_name_H-M   'C 1 2/c 1'
_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                 108.503(4)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   27.248(3)
_cell_length_b                   10.2025(11)
_cell_length_c                   17.7389(19)
_cell_measurement_reflns_used    1066
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      18.6505
_cell_measurement_theta_min      2.338
_cell_volume                     4676.5(9)
_computing_cell_refinement       'BRUKER APEX2'
_computing_data_collection       'BRUKER APEX2'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SIR-2004 (Burla, 2004)'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device_type  'Bruker X8 KappaAPEXII'
_diffrn_measurement_method       'omega and 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  0.0605
_diffrn_reflns_av_sigmaI/netI    0.1044
_diffrn_reflns_limit_h_max       28
_diffrn_reflns_limit_h_min       -30
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_number            27131
_diffrn_reflns_theta_full        23.25
_diffrn_reflns_theta_max         23.25
_diffrn_reflns_theta_min         2.15
_exptl_absorpt_coefficient_mu    0.573
_exptl_absorpt_correction_T_max  0.9830
_exptl_absorpt_correction_T_min  0.8543
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS-2008/1 (Bruker, 2008)'
_exptl_crystal_colour            Orange
_exptl_crystal_density_diffrn    1.477
_exptl_crystal_description       Plate
_exptl_crystal_F_000             2168
_exptl_crystal_size_max          0.13
_exptl_crystal_size_mid          0.11
_exptl_crystal_size_min          0.03
_refine_diff_density_max         0.403
_refine_diff_density_min         -0.688
_refine_diff_density_rms         0.088
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.016
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     327
_refine_ls_number_reflns         3360
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.016
_refine_ls_R_factor_all          0.1218
_refine_ls_R_factor_gt           0.0467
_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^)+(0.0417P)^2^+6.0625P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0857
_refine_ls_wR_factor_ref         0.1113
_reflns_number_gt                1994
_reflns_number_total             3360
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic2017038_si_001_2.cif
_cod_data_source_block           Ni(HLa)2.2AcOH
_cod_original_cell_volume        4676.4(8)
_cod_database_code               4328134