A direct, efficient synthesis of unsymmetrically substituted bis(arylidene)alkanones
Rosamilia, Anthony E.; Giarrusso, Marilena A.; Scott, Janet L.; Strauss, Christopher R.; Green Chemistry 8 (2006) 1042–; doi:10.1039/b606042k

data_7203442
_publ_section_title
;
 A direct, efficient synthesis of unsymmetrically substituted
 bis(arylidene)alkanones
;
_journal_issue                   12
_journal_name_full               'Green Chemistry'
_journal_page_first              1042
_journal_paper_doi               10.1039/b606042k
_journal_volume                  8
_journal_year                    2006
_chemical_formula_moiety         'C26 H31 N3 O'
_chemical_formula_sum            'C26 H31 N3 O'
_chemical_formula_weight         401.54
_chemical_name_systematic
;
(E)-N,N-dimethyl-9-(pyridin-4-yl)-5-(pyridin-4-ylmethylene)
-2,3,4,4a,5,6,7,8,9,9a-decahydro-1H-xanthen-4a-amine
;
_space_group_IT_number           14
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 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                 103.9810(10)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   10.08960(10)
_cell_length_b                   13.2900(2)
_cell_length_c                   16.6649(3)
_cell_measurement_temperature    123(2)
_cell_volume                     2168.41(6)
_computing_cell_refinement       'Nonius collect'
_computing_data_collection       'Nonius collect'
_computing_data_reduction        'Nonius collect'
_computing_molecular_graphics    X-Seed
_computing_publication_material  ciftab
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      123(2)
_diffrn_measured_fraction_theta_full 0.990
_diffrn_measured_fraction_theta_max 0.990
_diffrn_measurement_device_type  'phi and omega 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  0.0503
_diffrn_reflns_av_sigmaI/netI    0.0436
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_number            30375
_diffrn_reflns_theta_full        28.19
_diffrn_reflns_theta_max         28.19
_diffrn_reflns_theta_min         3.71
_exptl_absorpt_coefficient_mu    0.076
_exptl_crystal_colour            block
_exptl_crystal_density_diffrn    1.230
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       colourless
_exptl_crystal_F_000             864
_exptl_crystal_size_max          .45
_exptl_crystal_size_mid          .3
_exptl_crystal_size_min          .3
_refine_diff_density_max         0.223
_refine_diff_density_min         -0.275
_refine_diff_density_rms         0.054
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.059
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     273
_refine_ls_number_reflns         5297
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.059
_refine_ls_R_factor_all          0.0836
_refine_ls_R_factor_gt           0.0498
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0425P)^2^+0.7951P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0985
_refine_ls_wR_factor_ref         0.1113
_reflns_number_gt                3772
_reflns_number_total             5297
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            b606042k.cif.txt
_cod_data_source_block           8b
_cod_database_code               7203442