A Modular Approach to Carbene-Stabilized Diphosphorus Species
Doddi, Adinarayana; Bockfeld, Dirk; Zaretzke, Marc-Kevin; Kleeberg, Christian; Bannenberg, Thomas; Tamm, Matthias; Dalton Transactions  (2017) –; doi:10.1039/C7DT03436A

data_7044626
_publ_section_title
;
 A Modular Approach to Carbene-Stabilized Diphosphorus Species
;
_journal_name_full               'Dalton Transactions'
_journal_paper_doi               10.1039/C7DT03436A
_journal_year                    2017
_chemical_formula_moiety         'C48 H60 N4 P2 2+, 2(C32 H12 B F24 1-)'
_chemical_formula_sum            'C112 H84 B2 F48 N4 P2'
_chemical_formula_weight         2481.39
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     iterative
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-2014/7
_audit_update_record
;
2017-09-05 deposited with the CCDC.
2017-11-01 downloaded from the CCDC.
;
_cell_angle_alpha                80.996(4)
_cell_angle_beta                 76.569(4)
_cell_angle_gamma                69.481(4)
_cell_formula_units_Z            2
_cell_length_a                   16.1731(7)
_cell_length_b                   19.4127(10)
_cell_length_c                   20.26550(10)
_cell_measurement_reflns_used    43942
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      75.80
_cell_measurement_theta_min      3.33
_cell_volume                     5776.3(4)
_computing_cell_refinement
;
 CrysAlisPro, Agilent Technologies,
 Version 1.171.37.35 (release 13-08-2014 CrysAlis171 .NET)
 (compiled Aug 13 2014,18:06:01)
;
_computing_data_collection
;
 CrysAlisPro, Agilent Technologies,
 Version 1.171.37.35 (release 13-08-2014 CrysAlis171 .NET)
 (compiled Aug 13 2014,18:06:01)
;
_computing_data_reduction
;
 CrysAlisPro, Agilent Technologies,
 Version 1.171.37.35 (release 13-08-2014 CrysAlis171 .NET)
 (compiled Aug 13 2014,18:06:01)
;
_computing_molecular_graphics
;
 K. Brandenburg, 1999, Diamond 3.2i, Crystal Impact GbR, Bonn, Germany.
;
_computing_publication_material
;
 WinGX v2014.1 (L. J. Farrugia, J. Appl. Cryst., 2012, 45, 849-854.)
;
_computing_structure_refinement
;
 SHELXL-2014/7 (G. M. Sheldrick, Acta Cryst. (2008), A64, 112-122)'
;
_computing_structure_solution
;
 SHELXT (Ver. 2014/4) (G. M. Sheldrick, Acta Cryst., 2015, A71, 3--8)
;
_diffrn_ambient_temperature      100(2)
_diffrn_detector_area_resol_mean 10.3543
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device_type  'Oxford Diffraction, Xcalibur, Atlas, Nova'
_diffrn_measurement_method       \w-scan
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0786
_diffrn_reflns_av_unetI/netI     0.0289
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_limit_h_max       19
_diffrn_reflns_limit_h_min       -19
_diffrn_reflns_limit_k_max       23
_diffrn_reflns_limit_k_min       -23
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_limit_l_min       -24
_diffrn_reflns_number            274849
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_theta_full        65.996
_diffrn_reflns_theta_max         65.996
_diffrn_reflns_theta_min         3.367
_diffrn_source                   'Nova (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    1.474
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.830
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
 CrysAlisPro, Agilent Technologies,
 Version 1.171.37.35 (release 13-08-2014 CrysAlis171 .NET)
 (compiled Aug 13 2014,18:06:01)
 Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            'clear orange'
_exptl_crystal_density_diffrn    1.427
_exptl_crystal_description       'fragment of plate'
_exptl_crystal_F_000             2512
_exptl_crystal_recrystallization_method
;
 ADF-631 from a solution in DCM/n-hexane.
;
_exptl_crystal_size_max          0.21
_exptl_crystal_size_mid          0.18
_exptl_crystal_size_min          0.04
_refine_diff_density_max         0.851
_refine_diff_density_min         -0.596
_refine_diff_density_rms         0.062
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.061
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1697
_refine_ls_number_reflns         20102
_refine_ls_number_restraints     228
_refine_ls_restrained_S_all      1.093
_refine_ls_R_factor_all          0.0810
_refine_ls_R_factor_gt           0.0685
_refine_ls_shift/su_max          0.007
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.1102P)^2^+4.6446P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1888
_refine_ls_wR_factor_ref         0.1997
_reflns_number_gt                16591
_reflns_number_total             20102
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c7dt03436a2.cif
_cod_data_source_block           ad2ck
_cod_database_code               7044626
_shelx_shelxl_version_number     2014/7
_shelx_res_checksum              54602
_shelx_fab_checksum              19496