Metal-Bis(helicene) Assemblies Incorporating π-Conjugated Phosphole-Azahelicene Ligands: Impacting Chiroptical Properties by Metal Variation
Sébastien Graule; Mark Rudolph; Nicolas Vanthuyne; Jochen Autschbach; Christian Roussel; Jeanne Crassous; Régis Réau; Journal of the American Chemical Society 131 (2009) 3183–3185; doi:10.1021/ja809396f

data_4104293
_publ_section_title
;
 Metal-Bis(helicene) Assemblies Incorporating \p-Conjugated
 Phosphole-Azahelicene Ligands: Impacting Chiroptical Properties by Metal
 Variation
;
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              3183
_journal_page_last               3185
_journal_paper_doi               10.1021/ja809396f
_journal_volume                  131
_journal_year                    2009
_chemical_formula_moiety         'C45 H32 N P'
_chemical_formula_sum            'C45 H32 N P'
_chemical_formula_weight         617.69
_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                78.216(10)
_cell_angle_beta                 87.051(11)
_cell_angle_gamma                83.926(12)
_cell_formula_units_Z            2
_cell_length_a                   9.701(2)
_cell_length_b                   11.374(2)
_cell_length_c                   14.341(2)
_cell_measurement_reflns_used    0
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      27.56
_cell_measurement_theta_min      1.45
_cell_volume                     1539.6(5)
_computing_molecular_graphics    'Ortep-3 for Windows (Farrugia, 1997)'
_computing_publication_material  'WinGX publication routines (Farrugia, 1999)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-86 (Sheldrick, 1986)'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 0.969
_diffrn_measured_fraction_theta_max 0.969
_diffrn_measurement_device_type  CCD
_diffrn_measurement_method       none
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71069
_diffrn_reflns_av_R_equivalents  0.0786
_diffrn_reflns_av_sigmaI/netI    0.1768
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -12
_diffrn_reflns_number            11764
_diffrn_reflns_theta_full        27.56
_diffrn_reflns_theta_max         27.56
_diffrn_reflns_theta_min         1.45
_diffrn_standards_decay_%        none
_exptl_absorpt_coefficient_mu    0.126
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.332
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             648
_exptl_crystal_size_max          0.08
_exptl_crystal_size_mid          0.04
_exptl_crystal_size_min          0.02
_refine_diff_density_max         0.451
_refine_diff_density_min         -0.388
_refine_diff_density_rms         0.073
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.022
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     424
_refine_ls_number_reflns         6896
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.022
_refine_ls_R_factor_all          0.1713
_refine_ls_R_factor_gt           0.0791
_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^)+(0.0641P)^2^+0.4630P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1615
_refine_ls_wR_factor_ref         0.1921
_reflns_number_gt                3479
_reflns_number_total             6896
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja809396f_si_001.cif
_cod_data_source_block           sg280_0m
_cod_original_cell_volume        1539.6(4)
_cod_original_sg_symbol_H-M      P-1
_cod_database_code               4104293