Phosphine and carbene azido-cations: [(L)N3]+and [(L)2N3]+
Winkelhaus, Daniel; Holthausen, Michael H.; Dobrovetsky, Roman; Stephan, Douglas W.; Chem. Sci. 6 (2015) 6367–; doi:10.1039/C5SC02336J

data_1529254
_publ_section_title
;
 Phosphine and carbene azido-cations: [(L)N3]+and [(L)2N3]+
;
_journal_issue                   11
_journal_name_full               'Chem. Sci.'
_journal_page_first              6367
_journal_paper_doi               10.1039/C5SC02336J
_journal_volume                  6
_journal_year                    2015
_chemical_formula_sum            'C42 H50 B Cl0 F2 N7'
_chemical_formula_weight         701.70
_chemical_name_systematic
;
 ?
;
_space_group_IT_number           2
_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
_audit_update_record
;
2015-05-28 deposited with the CCDC.
2015-07-21 downloaded from the CCDC.
;
_cell_angle_alpha                86.770(2)
_cell_angle_beta                 76.082(2)
_cell_angle_gamma                83.169(2)
_cell_formula_units_Z            2
_cell_length_a                   11.7044(5)
_cell_length_b                   16.5009(7)
_cell_length_c                   18.3335(7)
_cell_measurement_temperature    149(2)
_cell_volume                     3411.0(2)
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_diffrn_ambient_temperature      149(2)
_diffrn_measured_fraction_theta_full 0.995
_diffrn_measured_fraction_theta_max 0.995
_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  0.0335
_diffrn_reflns_av_sigmaI/netI    0.0296
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -15
_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            72578
_diffrn_reflns_theta_full        27.52
_diffrn_reflns_theta_max         27.52
_diffrn_reflns_theta_min         1.67
_exptl_absorpt_coefficient_mu    0.045
_exptl_crystal_density_diffrn    0.683
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             748
_refine_diff_density_max         9.369
_refine_diff_density_min         -0.800
_refine_diff_density_rms         0.348
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   2.992
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     847
_refine_ls_number_reflns         15624
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      2.992
_refine_ls_R_factor_all          0.2521
_refine_ls_R_factor_gt           0.2240
_refine_ls_shift/su_max          0.009
_refine_ls_shift/su_mean         0.002
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.2000P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.5913
_refine_ls_wR_factor_ref         0.6199
_reflns_number_gt                11527
_reflns_number_total             15624
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c5sc02336j2.cif
_cod_data_source_block           mh047_0m
_cod_depositor_comments
'Adding full bibliography for 1529251--1529255.cif.'
_cod_database_code               1529254