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_7108326
_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            'C6 H21 B10 P'
_chemical_formula_weight         232.3
_chemical_name_systematic
;
?
;
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/c 1'
_atom_sites_solution_hydrogens   difmap
_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             2012-03-27T12:11:37-00:00
_audit_creation_method           'WinGX routine CIF_UPDATE'
_cell_angle_alpha                90
_cell_angle_beta                 112.994(5)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   10.6520(4)
_cell_length_b                   10.6114(3)
_cell_length_c                   13.2551(6)
_cell_measurement_reflns_used    2948
_cell_measurement_temperature    130(2)
_cell_measurement_theta_max      32.5148
_cell_measurement_theta_min      2.8363
_cell_volume                     1379.22(10)
_computing_cell_refinement
;
CrysAlisPro, Agilent Technologies,
Version 1.171.35.15 (release 03-08-2011 CrysAlis171 .NET)
(compiled Aug 3 2011,13:03:54)
;
_computing_data_collection
;
CrysAlisPro, Agilent Technologies,
Version 1.171.35.15 (release 03-08-2011 CrysAlis171 .NET)
(compiled Aug 3 2011,13:03:54)
;
_computing_data_reduction
;
CrysAlisPro, Agilent Technologies,
Version 1.171.35.15 (release 03-08-2011 CrysAlis171 .NET)
(compiled Aug 3 2011,13:03:54)
;
_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 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device_type  'Xcalibur, Sapphire3, Gemini'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_UB_11      -0.026828
_diffrn_orient_matrix_UB_12      0.0508555
_diffrn_orient_matrix_UB_13      -0.0369078
_diffrn_orient_matrix_UB_21      -0.0213347
_diffrn_orient_matrix_UB_22      -0.0427656
_diffrn_orient_matrix_UB_23      -0.0446441
_diffrn_orient_matrix_UB_31      -0.0637179
_diffrn_orient_matrix_UB_32      -0.0070912
_diffrn_orient_matrix_UB_33      0.0047433
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0649
_diffrn_reflns_av_unetI/netI     0.0678
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -12
_diffrn_reflns_number            15173
_diffrn_reflns_theta_full        30.51
_diffrn_reflns_theta_max         30.51
_diffrn_reflns_theta_min         2.84
_exptl_absorpt_coefficient_mu    0.162
_exptl_absorpt_correction_T_max  1
_exptl_absorpt_correction_T_min  0.99677
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro, Agilent Technologies,
Version 1.171.35.15 (release 03-08-2011 CrysAlis171 .NET)
(compiled Aug 3 2011,13:03:54)
Empirical absorption correction using spherical harmonics,
implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.119
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             488
_exptl_crystal_size_max          0.2
_exptl_crystal_size_mid          0.1
_exptl_crystal_size_min          0.1
_refine_diff_density_max         0.288
_refine_diff_density_min         -0.266
_refine_diff_density_rms         0.054
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.042
_refine_ls_hydrogen_treatment    refall
_refine_ls_matrix_type           full
_refine_ls_number_parameters     243
_refine_ls_number_reflns         4206
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.042
_refine_ls_R_factor_all          0.087
_refine_ls_R_factor_gt           0.0541
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0466P)^2^+0.2938P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1091
_refine_ls_wR_factor_ref         0.1218
_reflns_number_gt                2993
_reflns_number_total             4206
_reflns_threshold_expression     >2\s(I)
_cod_data_source_file            c2cc34860h.txt
_cod_data_source_block           x1433fin
_cod_original_cell_volume        1379.22(9)
_cod_original_sg_symbol_H-M      P2(1)/c
_cod_database_code               7108326