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_4122982
_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 H60 B N2 P'
_chemical_formula_weight         562.64
_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                 113.7205(18)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   16.3011(11)
_cell_length_b                   12.2497(7)
_cell_length_c                   19.4830(9)
_cell_measurement_reflns_used    6557
_cell_measurement_temperature    103.(2)
_cell_measurement_theta_max      25.0407
_cell_measurement_theta_min      2.1625
_cell_volume                     3561.8(4)
_computing_cell_refinement       'SAINT V8.32B (Bruker AXS Inc., 2013)'
_computing_data_collection       'Bruker APEX2'
_computing_data_reduction        'SAINT V8.32B (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 0.992
_diffrn_measured_fraction_theta_max 0.992
_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  0.0711
_diffrn_reflns_limit_h_max       23
_diffrn_reflns_limit_h_min       -23
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       27
_diffrn_reflns_limit_l_min       -27
_diffrn_reflns_number            51768
_diffrn_reflns_theta_full        30.61
_diffrn_reflns_theta_max         30.61
_diffrn_reflns_theta_min         2.71
_exptl_absorpt_coefficient_mu    0.102
_exptl_absorpt_correction_T_max  0.98
_exptl_absorpt_correction_T_min  0.79
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS V2012/1 (Bruker AXS Inc.)'
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.049
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             1240
_exptl_crystal_size_max          0.410
_exptl_crystal_size_mid          0.260
_exptl_crystal_size_min          0.240
_refine_diff_density_max         0.744
_refine_diff_density_min         -0.466
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.038
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     489
_refine_ls_number_reflns         10878
_refine_ls_number_restraints     572
_refine_ls_restrained_S_all      1.034
_refine_ls_R_factor_all          0.1179
_refine_ls_R_factor_gt           0.0641
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0924P)^2^+0.7491P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1578
_refine_ls_wR_factor_ref         0.1920
_reflns_number_gt                6533
_reflns_number_total             10878
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ja509963m_si_003.cif
_cod_data_source_block           I
_cod_database_code               4122982
_shelx_res_checksum              89255
_shelx_hkl_checksum              23758