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_4122980
_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   mixed
_audit_creation_method           SHELXL-2013
_cell_angle_alpha                67.064(6)
_cell_angle_beta                 81.934(6)
_cell_angle_gamma                70.631(5)
_cell_formula_units_Z            2
_cell_length_a                   9.7159(7)
_cell_length_b                   12.9229(10)
_cell_length_c                   16.3051(16)
_cell_measurement_temperature    173(2)
_cell_volume                     1778.5(3)
_computing_structure_refinement  'SHELXL-2013 (Sheldrick, 2013)'
_diffrn_ambient_temperature      173(2)
_diffrn_measured_fraction_theta_full 0.973
_diffrn_measured_fraction_theta_max 0.935
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.1002
_diffrn_reflns_av_unetI/netI     0.1587
_diffrn_reflns_Laue_measured_fraction_full 0.973
_diffrn_reflns_Laue_measured_fraction_max 0.935
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            23044
_diffrn_reflns_point_group_measured_fraction_full 0.973
_diffrn_reflns_point_group_measured_fraction_max 0.935
_diffrn_reflns_theta_full        25.000
_diffrn_reflns_theta_max         28.005
_diffrn_reflns_theta_min         1.796
_exptl_absorpt_coefficient_mu    0.149
_exptl_crystal_density_diffrn    1.109
_exptl_crystal_F_000             648
_exptl_crystal_size_max          0.360
_exptl_crystal_size_mid          0.280
_exptl_crystal_size_min          0.220
_refine_diff_density_max         0.418
_refine_diff_density_min         -0.513
_refine_diff_density_rms         0.111
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.061
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     392
_refine_ls_number_reflns         8054
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.061
_refine_ls_R_factor_all          0.2111
_refine_ls_R_factor_gt           0.0979
_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^)+(0.1201P)^2^+2.2183P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2259
_refine_ls_wR_factor_ref         0.2986
_reflns_Friedel_coverage         0.000
_reflns_number_gt                3760
_reflns_number_total             8054
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ja509963m_si_008.cif
_cod_data_source_block           rei111r
_cod_database_code               4122980
_shelx_estimated_absorpt_t_min   0.948
_shelx_estimated_absorpt_t_max   0.968
_shelxl_version_number           2013-4
_shelx_res_checksum              86546
_shelx_hkl_checksum              67573