Endocyclic P-P bond cleavage in carbaborane-substituted 1,2-diphosphetane ‒ A new route to secondary phosphinocarbaboranes
Evamarie Hey-Hawkins; Peter Lonnecke; Anika Kreienbrink; Matthias Findeisen; Chem.Commun. 48 (2012) 9385–; doi:10.1039/c2cc34860h

data_7108327
_publ_section_title
;
 Endocyclic P-P bond cleavage in carbaborane-substituted 1,2-diphosphetane
 -- A new route to secondary phosphinocarbaboranes
;
_journal_name_full               Chem.Commun.
_journal_page_first              9385
_journal_paper_doi               10.1039/c2cc34860h
_journal_volume                  48
_journal_year                    2012
_chemical_formula_sum            'C18 H37 B10 N P2'
_chemical_formula_weight         437.53
_space_group_IT_number           61
_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_Hall  '-P 2ac 2ab'
_symmetry_space_group_name_H-M   'P b c a'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_conform_dict_location     ftp://ftp.iucr.org/pub/cif_core.dic
_audit_conform_dict_name         cif_core.dic
_audit_conform_dict_version      2.4
_audit_creation_date             2012-07-05T11:32:17-00:00
_audit_creation_method           'WinGX routine CIF_UPDATE'
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   11.8524(8)
_cell_length_b                   19.2981(11)
_cell_length_c                   21.5647(16)
_cell_measurement_reflns_used    1025
_cell_measurement_temperature    130(2)
_cell_measurement_theta_max      26.5823
_cell_measurement_theta_min      2.8272
_cell_volume                     4932.5(6)
_computing_cell_refinement
;
CrysAlisPro, Agilent Technologies,
Version 1.171.35.21 (release 20-01-2012 CrysAlis171 .NET)
(compiled Jan 23 2012,18:06:46)
;
_computing_data_collection
;
CrysAlisPro, Agilent Technologies,
Version 1.171.35.21 (release 20-01-2012 CrysAlis171 .NET)
(compiled Jan 23 2012,18:06:46)
;
_computing_data_reduction
;
CrysAlisPro, Agilent Technologies,
Version 1.171.35.21 (release 20-01-2012 CrysAlis171 .NET)
(compiled Jan 23 2012,18:06:46)
;
_computing_molecular_graphics
;
ORTEP3 for Windows
L. J. Farrugia, J. Appl. Crystallogr. 1997, 30, 565.
;
_computing_publication_material
;
WINGX
L.J. Farrugia,
J. Appl. Cryst., 1999, 32, 837-838.
;
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_computing_structure_solution
;
SIR92
A. Altomare, G. Cascarano, C. Giacovazzo and A. Guagliardi,
J. Appl. Crystallogr. 1993, 26, 343-350.
;
_diffrn_ambient_temperature      130(2)
_diffrn_detector_area_resol_mean 16.356
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device_type  'Xcalibur, Sapphire3, Gemini'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_UB_11      0.020173
_diffrn_orient_matrix_UB_12      -0.0335503
_diffrn_orient_matrix_UB_13      -0.0075519
_diffrn_orient_matrix_UB_21      0.0489114
_diffrn_orient_matrix_UB_22      0.0148842
_diffrn_orient_matrix_UB_23      -0.0134921
_diffrn_orient_matrix_UB_31      0.027977
_diffrn_orient_matrix_UB_32      -0.0018068
_diffrn_orient_matrix_UB_33      0.0290346
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.272
_diffrn_reflns_av_unetI/netI     0.1633
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       21
_diffrn_reflns_limit_k_min       -21
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_number            28712
_diffrn_reflns_theta_full        23.26
_diffrn_reflns_theta_max         23.26
_diffrn_reflns_theta_min         2.83
_exptl_absorpt_coefficient_mu    0.184
_exptl_absorpt_correction_T_max  1
_exptl_absorpt_correction_T_min  0.9701
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro, Agilent Technologies,
Version 1.171.35.21 (release 20-01-2012 CrysAlis171 .NET)
(compiled Jan 23 2012,18:06:46)
Empirical absorption correction using spherical harmonics,
implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.178
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       'small needles'
_exptl_crystal_F_000             1856
_exptl_crystal_size_max          0.2
_exptl_crystal_size_mid          0.07
_exptl_crystal_size_min          0.01
_refine_diff_density_max         0.701
_refine_diff_density_min         -0.291
_refine_diff_density_rms         0.072
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.007
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     286
_refine_ls_number_reflns         3533
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.007
_refine_ls_R_factor_all          0.1788
_refine_ls_R_factor_gt           0.0759
_refine_ls_shift/su_max          0
_refine_ls_shift/su_mean         0
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0753P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1504
_refine_ls_wR_factor_ref         0.1942
_reflns_number_gt                1734
_reflns_number_total             3533
_reflns_threshold_expression     >2\s(I)
_cod_data_source_file            c2cc34860h.txt
_cod_data_source_block           x1598fin
_cod_original_sg_symbol_H-M      Pbca
_cod_database_code               7108327