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_4122985
_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      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2ybc'
_space_group_name_H-M_alt        'P 1 21/c 1'
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/c 1'
_atom_sites_solution_hydrogens   mixed
_cell_angle_alpha                90
_cell_angle_beta                 90.158(3)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   12.9755(6)
_cell_length_b                   16.0657(7)
_cell_length_c                   17.3774(7)
_cell_measurement_reflns_used    9916
_cell_measurement_temperature    296.(2)
_cell_measurement_theta_max      26.4183
_cell_measurement_theta_min      2.3312
_cell_volume                     3622.5(3)
_computing_cell_refinement       'SAINT V8.34A (Bruker AXS Inc., 2013)'
_computing_data_collection       'APEX2 (Bruker AXS Inc., 2013)'
_computing_data_reduction        'SAINT V8.34A (Bruker AXS Inc., 2013)'
_computing_molecular_graphics    'XP (Bruker AXS Inc., 2013)'
_computing_publication_material  'APEX2 (Bruker AXS Inc., 2013)'
_computing_structure_refinement  'SHELXL-2013 (Sheldrick, 2013)'
_computing_structure_solution    'SHELXS-97 (Sheldrick 2008)'
_diffrn_ambient_temperature      296.(2)
_diffrn_detector_area_resol_mean 8.3333
_diffrn_measured_fraction_theta_full 0.977
_diffrn_measured_fraction_theta_max 0.977
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.1778
_diffrn_reflns_av_unetI/netI     0.1451
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            52945
_diffrn_reflns_theta_full        26.40
_diffrn_reflns_theta_max         26.40
_diffrn_reflns_theta_min         1.73
_diffrn_source                   'fine-focus sealed tube'
_exptl_absorpt_coefficient_mu    0.147
_exptl_absorpt_correction_T_max  0.98
_exptl_absorpt_correction_T_min  0.72
_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             1296
_exptl_crystal_size_max          0.400
_exptl_crystal_size_mid          0.200
_exptl_crystal_size_min          0.140
_refine_diff_density_max         0.270
_refine_diff_density_min         -0.391
_refine_ls_extinction_coef       0.0063(9)
_refine_ls_extinction_method     SHELXL
_refine_ls_goodness_of_fit_ref   1.020
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     394
_refine_ls_number_reflns         7257
_refine_ls_number_restraints     4
_refine_ls_restrained_S_all      1.020
_refine_ls_R_factor_all          0.2194
_refine_ls_R_factor_gt           0.0807
_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^)+(0.0877P)^2^+0.0584P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1498
_refine_ls_wR_factor_ref         0.2060
_reflns_number_gt                3025
_reflns_number_total             7257
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ja509963m_si_006.cif
_cod_data_source_block           I
_cod_database_code               4122985
_shelx_res_checksum              33846
_shelx_hkl_checksum              42894