Metal-Free σ-Bond Metathesis in Ammonia Activation by a Diazadiphosphapentalene.
Cui, Jingjing; Li, Yongxin; Ganguly, Rakesh; Inthirarajah, Anusiya; Hirao, Hajime; Kinjo, Rei; Journal of the American Chemical Society  (2014) 141119074650008–; doi:10.1021/ja509963m

data_4122984
_publ_section_title
;
 Metal-Free \s-Bond Metathesis in Ammonia Activation by a
 Diazadiphosphapentalene.
;
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              141119074650008
_journal_paper_doi               10.1021/ja509963m
_journal_year                    2014
_chemical_formula_sum            'C36 H57 N3 P2'
_chemical_formula_weight         593.78
_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
_cell_angle_alpha                114.231(8)
_cell_angle_beta                 90.678(8)
_cell_angle_gamma                95.787(8)
_cell_formula_units_Z            2
_cell_length_a                   9.5581(18)
_cell_length_b                   13.979(3)
_cell_length_c                   14.962(3)
_cell_measurement_reflns_used    1442
_cell_measurement_temperature    103.(2)
_cell_measurement_theta_max      18.5532
_cell_measurement_theta_min      2.5280
_cell_volume                     1810.6(6)
_computing_cell_refinement       'SAINT V8.34A (Bruker AXS Inc., 2013)'
_computing_data_collection       'Bruker APEX2'
_computing_data_reduction        'SAINT V8.34A (Bruker AXS Inc., 2013)'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-2013 (Sheldrick, 2013)'
_computing_structure_solution    'SHELXS-97 (Sheldrick 2008)'
_diffrn_ambient_temperature      103.(2)
_diffrn_detector_area_resol_mean 8.3333
_diffrn_measured_fraction_theta_full 0.981
_diffrn_measured_fraction_theta_max 0.981
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.1671
_diffrn_reflns_av_sigmaI/netI    0.2407
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            41401
_diffrn_reflns_theta_full        26.34
_diffrn_reflns_theta_max         26.34
_diffrn_reflns_theta_min         2.15
_exptl_absorpt_coefficient_mu    0.147
_exptl_absorpt_correction_T_max  0.99
_exptl_absorpt_correction_T_min  0.84
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS V2012/1 (Bruker AXS Inc.)'
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.089
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             648
_exptl_crystal_size_max          0.400
_exptl_crystal_size_mid          0.120
_exptl_crystal_size_min          0.060
_refine_diff_density_max         0.263
_refine_diff_density_min         -0.284
_refine_ls_extinction_coef       0.030(2)
_refine_ls_extinction_method     SHELXL
_refine_ls_goodness_of_fit_ref   0.970
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     769
_refine_ls_number_reflns         7231
_refine_ls_number_restraints     2503
_refine_ls_restrained_S_all      0.842
_refine_ls_R_factor_all          0.2294
_refine_ls_R_factor_gt           0.0722
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0776P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1453
_refine_ls_wR_factor_ref         0.1991
_reflns_number_gt                2774
_reflns_number_total             7231
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ja509963m_si_007.cif
_cod_data_source_block           I
_cod_database_code               4122984
_shelx_res_checksum              28238
_shelx_hkl_checksum              81815