Template synthesis of benzannulated triphosphacyclononanes‒a new class of phosphacrowns via template assisted nucleophilic P-C bond formation.
Albers, Thomas; Edwards, Peter G; Chemical communications (Cambridge, England)  (2007) 858–860; doi:10.1039/b613672a

data_7101723
_publ_section_title
;
 Template synthesis of benzannulated triphosphacyclononanes--a new
 class of phosphacrowns via template assisted nucleophilic P-C bond
 formation.
;
_journal_issue                   8
_journal_name_full
'Chemical communications (Cambridge, England)'
_journal_page_first              858
_journal_page_last               860
_journal_paper_doi               10.1039/b613672a
_journal_year                    2007
_chemical_formula_sum            'C63 H53 B F2 Fe N P3'
_chemical_formula_weight         1021.63
_chemical_name_common
;
Cyclopentadienyl-1,4,7-triphospha-1,4-bis(2-fluorophenyl)-7-
phenyl (5,6),(8,9)dibenzocyclononane iron (ii) tetraphenylborate
acetonitrile solvate
;
_chemical_name_systematic
;
Cyclopentadienyl-1,4,7-triphospha-1,4-bis(2-fluorophenyl)-7-phenyl
[5,6],[8,9]dibenzocyclononane iron (ii) tetraphenylborate
acetonitrile solvate
;
_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                69.91(2)
_cell_angle_beta                 80.92(2)
_cell_angle_gamma                74.67(2)
_cell_formula_units_Z            2
_cell_length_a                   11.956(2)
_cell_length_b                   12.718(4)
_cell_length_c                   18.674(8)
_cell_measurement_temperature    150(2)
_cell_volume                     2564.8(14)
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      150(2)
_diffrn_measured_fraction_theta_full 0.815
_diffrn_measured_fraction_theta_max 0.815
_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  0.0395
_diffrn_reflns_av_sigmaI/netI    0.0424
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       0
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            6570
_diffrn_reflns_theta_full        23.69
_diffrn_reflns_theta_max         23.69
_diffrn_reflns_theta_min         2.39
_exptl_absorpt_coefficient_mu    0.437
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.323
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             1064
_exptl_crystal_size_max          .5
_exptl_crystal_size_mid          .5
_exptl_crystal_size_min          .3
_refine_diff_density_max         0.583
_refine_diff_density_min         -0.550
_refine_diff_density_rms         0.064
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.024
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     641
_refine_ls_number_reflns         6332
_refine_ls_number_restraints     15
_refine_ls_restrained_S_all      1.025
_refine_ls_R_factor_all          0.0649
_refine_ls_R_factor_gt           0.0404
_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^)+(0.0484P)^2^+4.1576P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0958
_refine_ls_wR_factor_ref         0.1121
_reflns_number_gt                5017
_reflns_number_total             6332
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            b613672a.txt
_cod_data_source_block           00pge004
_cod_original_sg_symbol_H-M      P-1
_cod_database_code               7101723