Reactivity of cyclooligophosphanes: synthesis and structural characterisation of cyclo-1,4-(BH3)2(P4Ph4CH2) and cyclo-1,2-(BH3)2(P5Ph5).
Wolf, Robert; Finger, Markus; Limburg, Carolin; Willis, Anthony C.; Wild, S. Bruce; Hey-Hawkins, Evamarie; Dalton transactions (Cambridge, England : 2003)  (2006) 831–837; doi:10.1039/b511833f

data_7006543
_publ_section_title
;
 Reactivity of cyclooligophosphanes: synthesis and structural
 characterisation of cyclo-1,4-(BH3)2(P4Ph4CH2) and
 cyclo-1,2-(BH3)2(P5Ph5).
;
_journal_issue                   6
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              831
_journal_page_last               837
_journal_paper_doi               10.1039/b511833f
_journal_year                    2006
_chemical_formula_sum            'C25 H28 B2 P4'
_chemical_formula_weight         473.97
_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                78.798(3)
_cell_angle_beta                 75.012(3)
_cell_angle_gamma                72.274(3)
_cell_formula_units_Z            2
_cell_length_a                   10.7171(16)
_cell_length_b                   10.7170(16)
_cell_length_c                   12.3396(18)
_cell_measurement_reflns_used    91
_cell_measurement_temperature    223(2)
_cell_measurement_theta_max      30.80
_cell_measurement_theta_min      1.72
_cell_volume                     1293.7(3)
_computing_cell_refinement       'Bruker SAINT'
_computing_data_collection       'Bruker SMART'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    'WINGX v.1.64.05 (Farrugia, 1999)'
_computing_publication_material  'WINGX v.1.64.05 (Farrugia, 1999)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1997)'
_diffrn_ambient_temperature      223(2)
_diffrn_measured_fraction_theta_full 0.931
_diffrn_measured_fraction_theta_max 0.931
_diffrn_measurement_device_type  'Bruker CCD'
_diffrn_measurement_method       '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  0.0188
_diffrn_reflns_av_sigmaI/netI    0.0520
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -12
_diffrn_reflns_number            10634
_diffrn_reflns_theta_full        30.80
_diffrn_reflns_theta_max         30.80
_diffrn_reflns_theta_min         1.72
_exptl_absorpt_coefficient_mu    0.303
_exptl_absorpt_correction_type   SADABS
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.217
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             496
_exptl_crystal_size_max          0.2
_exptl_crystal_size_mid          0.1
_exptl_crystal_size_min          0.1
_refine_diff_density_max         0.821
_refine_diff_density_min         -0.384
_refine_diff_density_rms         0.055
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.996
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     349
_refine_ls_number_reflns         7547
_refine_ls_number_restraints     30
_refine_ls_restrained_S_all      0.995
_refine_ls_R_factor_all          0.0905
_refine_ls_R_factor_gt           0.0502
_refine_ls_shift/su_max          0.009
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0563P)^2^+0.4205P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1094
_refine_ls_wR_factor_ref         0.1239
_reflns_number_gt                4895
_reflns_number_total             7547
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            b511833f.txt
_cod_data_source_block           3
_cod_original_sg_symbol_H-M      P-1
_cod_database_code               7006543