Metallacyclophanes of 1,6-Bis(diphenylphosphino)pyrene: Excimeric Emission and Effect of Oxygen on Stability of the Rings
Jian Hu; Minh-Hai Nguyen; John H. K. Yip; Inorganic Chemistry 50 (2011) 7429–7439; doi:10.1021/ic102441b

data_4325847
_publ_section_title
;
 Metallacyclophanes of 1,6-Bis(diphenylphosphino)pyrene: Excimeric
 Emission and Effect of Oxygen on Stability of the Rings
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              7429
_journal_page_last               7439
_journal_paper_doi               10.1021/ic102441b
_journal_volume                  50
_journal_year                    2011
_chemical_formula_sum            'C40 H28 O2 P2'
_chemical_formula_weight         602.56
_chemical_name_common            6
_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                67.7060(10)
_cell_angle_beta                 71.7350(10)
_cell_angle_gamma                77.6660(10)
_cell_formula_units_Z            1
_cell_length_a                   9.1022(5)
_cell_length_b                   9.5051(5)
_cell_length_c                   9.9259(6)
_cell_measurement_reflns_used    4565
_cell_measurement_temperature    223(2)
_cell_measurement_theta_max      27.45
_cell_measurement_theta_min      2.29
_cell_volume                     750.14(7)
_computing_cell_refinement       'Bruker SMART'
_computing_data_collection       'Bruker SMART'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      223(2)
_diffrn_measured_fraction_theta_full 0.996
_diffrn_measured_fraction_theta_max 0.996
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       '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  0.0211
_diffrn_reflns_av_sigmaI/netI    0.0235
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       12
_diffrn_reflns_limit_l_min       -12
_diffrn_reflns_number            9892
_diffrn_reflns_theta_full        27.50
_diffrn_reflns_theta_max         27.50
_diffrn_reflns_theta_min         2.29
_exptl_absorpt_coefficient_mu    0.182
_exptl_absorpt_correction_T_max  0.9543
_exptl_absorpt_correction_T_min  0.8988
_exptl_absorpt_correction_type   'Sadabs, (Sheldrick 2001)'
_exptl_crystal_colour            'PALE YELLOW'
_exptl_crystal_density_diffrn    1.334
_exptl_crystal_density_meas      0
_exptl_crystal_description       BLOCK
_exptl_crystal_F_000             314
_exptl_crystal_size_max          0.60
_exptl_crystal_size_mid          0.32
_exptl_crystal_size_min          0.26
_refine_diff_density_max         0.529
_refine_diff_density_min         -0.215
_refine_diff_density_rms         0.065
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.051
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     199
_refine_ls_number_reflns         3427
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.051
_refine_ls_R_factor_all          0.0518
_refine_ls_R_factor_gt           0.0479
_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^)+(0.0735P)^2^+0.3407P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1267
_refine_ls_wR_factor_ref         0.1298
_reflns_number_gt                3111
_reflns_number_total             3427
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic102441b_si_002_6.cif
_cod_data_source_block           7169
_cod_database_code               4325847