P-N Cooperative Borane Activation and Catalytic Hydroboration by a Distorted Phosphorous Triamide Platform.
Lin, Yi-Chun; Hatzakis, Emmanuel; McCarthy, Sean M.; Reichl, Kyle D.; Lai, Ting-Yi; Yennawar, Hemant P.; Radosevich, Alexander T.; Journal of the American Chemical Society 139 (2017) 6008–6016; doi:10.1021/jacs.7b02512

data_4126118
_publ_section_title
;
 P-N Cooperative Borane Activation and Catalytic Hydroboration by a
 Distorted Phosphorous Triamide Platform.
;
_journal_issue                   16
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              6008
_journal_page_last               6016
_journal_paper_doi               10.1021/jacs.7b02512
_journal_volume                  139
_journal_year                    2017
_chemical_formula_moiety         'C27 H34 B N4 O2 P'
_chemical_formula_sum            'C27 H34 B N4 O2 P'
_chemical_formula_weight         488.36
_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_date             2016-01-07
_audit_creation_method
;
Olex2 1.2
(compiled 2015.09.30 svn.r3233 for OlexSys, GUI svn.r5103)
;
_cell_angle_alpha                89.490(2)
_cell_angle_beta                 65.116(2)
_cell_angle_gamma                71.217(2)
_cell_formula_units_Z            2
_cell_length_a                   10.7971(12)
_cell_length_b                   11.4825(13)
_cell_length_c                   12.3601(14)
_cell_measurement_reflns_used    4458
_cell_measurement_temperature    213.5
_cell_measurement_theta_max      28.278
_cell_measurement_theta_min      2.436
_cell_volume                     1301.7(3)
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_computing_structure_solution    'olex2.solve (Bourhis et al., 2015)'
_diffrn_ambient_temperature      213.15
_diffrn_measured_fraction_theta_full 0.989
_diffrn_measured_fraction_theta_max 0.965
_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  0.0144
_diffrn_reflns_av_unetI/netI     0.0299
_diffrn_reflns_Laue_measured_fraction_full 0.989
_diffrn_reflns_Laue_measured_fraction_max 0.965
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       9
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_number            9853
_diffrn_reflns_point_group_measured_fraction_full 0.989
_diffrn_reflns_point_group_measured_fraction_max 0.965
_diffrn_reflns_theta_full        26.000
_diffrn_reflns_theta_max         28.323
_diffrn_reflns_theta_min         1.836
_exptl_absorpt_coefficient_mu    0.137
_exptl_absorpt_correction_T_max  0.9100
_exptl_absorpt_correction_T_min  0.855340
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
? was used for absorption correction.
R(int) was 0.0300 before and 0.0136 after correction.
The Ratio of minimum to maximum transmission is 0.8553.
The \l/2 correction factor is 0.0015.
;
_exptl_crystal_colour            'clear colourless'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.246
_exptl_crystal_description       block
_exptl_crystal_F_000             520
_exptl_crystal_preparation       edit
_exptl_crystal_recrystallization_method evaporation
_exptl_crystal_size_max          0.22
_exptl_crystal_size_mid          0.17
_exptl_crystal_size_min          0.1
_refine_diff_density_max         0.432
_refine_diff_density_min         -0.269
_refine_diff_density_rms         0.056
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.267
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     326
_refine_ls_number_reflns         6281
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.267
_refine_ls_R_factor_all          0.0659
_refine_ls_R_factor_gt           0.0589
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.1000P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1701
_refine_ls_wR_factor_ref         0.1746
_reflns_Friedel_coverage         0.000
_reflns_number_gt                5520
_reflns_number_total             6281
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ja7b02512_si_004.cif
_cod_data_source_block           yzl24s
_cod_database_code               4126118
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2.a Secondary CH2 refined with riding coordinates:
 C1(H1A,H1B)
2.b Aromatic/amide H refined with riding coordinates:
 C3(H3), C4(H4), C5(H5), C6(H6), C7(H7), C9(H9), C10(H10), C11(H11), C12(H12),
 C16(H16), C17(H17), C18(H18), C19(H19)
2.c Idealised Me refined as rotating group:
 C20(H20A,H20B,H20C), C21(H21A,H21B,H21C), C24(H24A,H24B,H24C), C25(H25A,H25B,
 H25C), C26(H26A,H26B,H26C), C27(H27A,H27B,H27C)
;
_shelx_res_checksum              63385
_shelx_hkl_checksum              95116
_shelx_shelxl_version_number     2014/7
_olex2_exptl_crystal_mounting_method 'paratone cryo-loop '
_olex2_submission_special_instructions 'No special instructions were received'