Phosphorus peri-bridged acenaphthenes: efficient syntheses, characterisation and quaternization reactions
Wawrzyniak, Piotr; Slawin, Alexandra M. Z.; Fuller, Amy L.; Woollins, J. Derek; Kilian, Petr; Dalton Transactions  (2009) 7883–7884; doi:10.1039/b916166j

data_7030509
_publ_section_title
;
 Phosphorus peri-bridged acenaphthenes: efficient syntheses,
 characterisation and quaternization reactions
;
_journal_coden_ASTM              DTARAF
_journal_issue                   38
_journal_name_full               'Dalton Transactions'
_journal_page_first              7883
_journal_page_last               7884
_journal_paper_doi               10.1039/b916166j
_journal_year                    2009
_chemical_formula_moiety         'C31 H40 P, 3(C H Cl3), I '
_chemical_formula_sum            'C34 H43 Cl9 I P'
_chemical_formula_weight         928.67
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_symmetry_Int_Tables_number      2
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_cell_angle_alpha                74.273(20)
_cell_angle_beta                 80.28(2)
_cell_angle_gamma                63.267(14)
_cell_formula_units_Z            2
_cell_length_a                   11.2391(16)
_cell_length_b                   11.8953(12)
_cell_length_c                   18.116(3)
_cell_measurement_reflns_used    7671
_cell_measurement_temperature    125.1
_cell_measurement_theta_max      26.4
_cell_measurement_theta_min      2.0
_cell_volume                     2079.0(6)
_computing_cell_refinement       CrystalClear
_computing_data_collection       CrystalClear
_computing_data_reduction        CrystalStructure
_computing_publication_material  'CrystalStructure 3.8'
_computing_structure_refinement  SHELXL
_computing_structure_solution    SIR97
_diffrn_detector_area_resol_mean 14.63
_diffrn_measured_fraction_theta_full 0.986
_diffrn_measured_fraction_theta_max 0.986
_diffrn_measurement_device_type  'Rigaku Saturn'
_diffrn_measurement_method       \w
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71075
_diffrn_reflns_av_R_equivalents  0.077
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            23814
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         25.00
_exptl_absorpt_coefficient_mu    1.410
_exptl_absorpt_correction_T_max  0.881
_exptl_absorpt_correction_T_min  0.685
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'Jacobson, R. (1998) Private communication'
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.483
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             936.00
_exptl_crystal_size_max          0.21
_exptl_crystal_size_mid          0.15
_exptl_crystal_size_min          0.09
_refine_diff_density_max         0.89
_refine_diff_density_min         -1.00
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.193
_refine_ls_hydrogen_treatment    refall
_refine_ls_number_parameters     417
_refine_ls_number_reflns         7239
_refine_ls_R_factor_gt           0.0733
_refine_ls_shift/su_max          0.0030
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w = 1/[\s^2^(Fo^2^)+(0.1038P)^2^+4.1215P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_ref         0.2240
_reflns_number_gt                6455
_reflns_number_total             7239
_reflns_threshold_expression     F^2^>2.0\s(F^2^)
_cod_duplicate_entry             7002332
_cod_data_source_file            b916166j.txt
_cod_data_source_block           8
_cod_original_formula_sum        'C34 H43 Cl9 I P '
_cod_database_code               7030509