Sterically shielded pyramidal amino groups in two 4,4'-(arylmethylene)bis(6-allyl-3-chloro-2-methylaniline) derivatives
Blanco, Maria C.; Palma, Alirio; Bahsas, Ali; Hursthouse, Michael B.; Cobo, Justo; Glidewell, Christopher; Acta Crystallographica Section C 65 (2009) o479–o482; doi:10.1107/S0108270109031175

data_2017302
_publ_section_title
;
 Sterically shielded pyramidal amino groups in two
 4,4'-(arylmethylene)bis(6-allyl-3-chloro-2-methylaniline) derivatives
;
_journal_coeditor_code           GG3211
_journal_issue                   9
_journal_name_full               'Acta Crystallographica Section C'
_journal_page_first              o479
_journal_page_last               o482
_journal_paper_doi               10.1107/S0108270109031175
_journal_volume                  65
_journal_year                    2009
_chemical_formula_iupac          'C25 H26 Cl2 N2 S'
_chemical_formula_moiety         'C25 H26 Cl2 N2 S'
_chemical_formula_sum            'C25 H26 Cl2 N2 S'
_chemical_formula_weight         457.44
_chemical_name_systematic
;
4,4'-(2-thienylmethylene)bis(6-allyl-3-chloro-2-methylaniline)
;
_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
_cell_angle_alpha                77.1100(10)
_cell_angle_beta                 87.7930(10)
_cell_angle_gamma                82.367(2)
_cell_formula_units_Z            2
_cell_length_a                   8.7263(2)
_cell_length_b                   10.6766(2)
_cell_length_c                   12.2691(3)
_cell_measurement_reflns_used    5043
_cell_measurement_temperature    120(2)
_cell_measurement_theta_max      27.58
_cell_measurement_theta_min      2.92
_cell_volume                     1104.35(4)
_computing_cell_refinement
;
DENZO (Otwinowski & Minor, 1997) and COLLECT (Nonius, 1999)
;
_computing_data_collection       'COLLECT (Nonius, 1999)'
_computing_data_reduction
;
DENZO (Otwinowski & Minor, 1997) and COLLECT (Nonius, 1999)
;
_computing_molecular_graphics    'PLATON (Spek, 2009)'
_computing_publication_material
;
SHELXL97 (Sheldrick, 2008) and PLATON (Spek, 2009)
;
_computing_structure_refinement  'SHELXL97 (Sheldrick, 2008)'
_computing_structure_solution    'SIR2004 (Burla <i>et al.</i>,  2005)'
_diffrn_ambient_temperature      120(2)
_diffrn_detector_area_resol_mean '4096 x 4096 pixels/62 x 62mm'
_diffrn_measured_fraction_theta_full 0.992
_diffrn_measured_fraction_theta_max 0.987
_diffrn_measurement_device_type  'Bruker Nonius APEX II'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_monochromator  '10cm confocal mirrors'
_diffrn_radiation_source         'Bruker Nonius FR591 rotating anode'
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0299
_diffrn_reflns_av_sigmaI/netI    0.0362
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_limit_l_min       -13
_diffrn_reflns_number            16485
_diffrn_reflns_theta_full        27.50
_diffrn_reflns_theta_max         27.58
_diffrn_reflns_theta_min         2.92
_diffrn_standards_decay_%        0
_diffrn_standards_interval_count 0
_diffrn_standards_interval_time  0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.404
_exptl_absorpt_correction_T_max  0.980
_exptl_absorpt_correction_T_min  0.959
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   '(SADABS; Sheldrick, 2003)'
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.376
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             480
_exptl_crystal_size_max          0.08
_exptl_crystal_size_mid          0.06
_exptl_crystal_size_min          0.05
_refine_diff_density_max         0.304
_refine_diff_density_min         -0.248
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.098
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     298
_refine_ls_number_reflns         5043
_refine_ls_number_restraints     10
_refine_ls_restrained_S_all      1.097
_refine_ls_R_factor_all          0.0493
_refine_ls_R_factor_gt           0.0397
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w = 1/[\s^2^(Fo^2^)+(0.0118P)^2^+0.9169P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0804
_refine_ls_wR_factor_ref         0.0862
_reflns_number_gt                4375
_reflns_number_total             5043
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            gg3211.cif
_cod_data_source_block           II
_cod_database_code               2017302
_cod_database_fobs_code          2017302