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_4125930
_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_absolute_configuration ad
_chemical_formula_moiety         'C34 H40 B N4 O4 P S'
_chemical_formula_sum            'C34 H40 B N4 O4 P S'
_chemical_formula_weight         642.54
_chemical_name_systematic
;
 ? 
;
_space_group_crystal_system      triclinic
_space_group_IT_number           1
_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
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_date             2016-07-01
_audit_creation_method
;
Olex2 1.2
(compiled 2016.02.19 svn.r3266 for OlexSys, GUI svn.r5155)
;
_cell_angle_alpha                108.388(5)
_cell_angle_beta                 92.418(3)
_cell_angle_gamma                90.015(4)
_cell_formula_units_Z            2
_cell_length_a                   10.580(2)
_cell_length_b                   10.675(2)
_cell_length_c                   15.627(4)
_cell_measurement_reflns_used    2764
_cell_measurement_temperature    298(2)
_cell_measurement_theta_max      2.316
_cell_measurement_theta_min      26.603
_cell_volume                     1673.2(6)
_computing_cell_refinement       'SAINT v6.36a (Bruker, 2001)'
_computing_data_collection       'SMART v5.625 (Bruker, 2001)'
_computing_data_reduction        'SAINT v6.36a (Bruker, 2001)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'XL (Sheldrick, 2008)'
_computing_structure_solution    'XS (Sheldrick, 2008)'
_diffrn_ambient_temperature      298(2)
_diffrn_measured_fraction_theta_full 0.923
_diffrn_measured_fraction_theta_max 0.871
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_radiation_monochromator  Parallel,graphite
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0252
_diffrn_reflns_av_unetI/netI     0.0823
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            12176
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         28.41
_diffrn_reflns_theta_min         1.93
_diffrn_source                   'fine-focus sealed tube'
_diffrn_source_current           32.0
_diffrn_source_power             1.6
_diffrn_source_voltage           50.0
_exptl_absorpt_coefficient_mu    0.188
_exptl_absorpt_correction_T_max  0.9
_exptl_absorpt_correction_T_min  0.125722
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS was used for absorption correction.
R(int) was 0.0590 before and 0.0330 after correction.
The Ratio of minimum to maximum transmission is 0.1257.
The \l/2 correction factor is 0.0015.
;
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.275
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             680
_exptl_crystal_size_max          0.15
_exptl_crystal_size_mid          0.14
_exptl_crystal_size_min          0.11
_refine_diff_density_max         0.655
_refine_diff_density_min         -0.686
_refine_diff_density_rms         0.066
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   0.42(14)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.111
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     664
_refine_ls_number_reflns         11236
_refine_ls_number_restraints     567
_refine_ls_restrained_S_all      1.087
_refine_ls_R_factor_all          0.1176
_refine_ls_R_factor_gt           0.0879
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.1000P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1906
_refine_ls_wR_factor_ref         0.2168
_reflns_number_gt                7899
_reflns_number_total             11236
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja7b02512_si_003.cif
_cod_data_source_block           yzl26t
_cod_depositor_comments          'Adding full bibliography for 4125930.cif.'
_cod_original_cell_volume        1673.3(7)
_cod_database_code               4125930
_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. Uiso/Uaniso restraints and constraints
All non-hydrogen atoms have similar U: within 2A with sigma of 0.04 and sigma
for terminal atoms of 0.08
3.a Free rotating group:
 C21(C22,C23,C24,C25,C26,C27,C28), C29(C34,C33,C32,C31,C30,B1,S2,P2,O6,O5,O7,
 O8,N5,N6,N7,N8,C35,C36,C37,C38,C39,C40,C41,C42,C43,C44,C45,C46,C47,C48,C49,C50,
 C51,C52,C53,C54), C55(C56,C57,C58,C59,C60,C61,C62), C63(C64,C65,C66,C67,C68,B2)
3.b Secondary CH2 refined with riding coordinates:
 C28(H28A,H28B), C62(H62A,H62B)
3.c Aromatic/amide H refined with riding coordinates:
 C3(H3), C4(H4), C5(H5), C6(H6), C9(H9), C10(H10), C11(H11), C12(H12),
 C22(H22), C23(H23), C25(H25), C26(H26), C34(H34), C33(H33), C32(H32), C31(H31),
  C30(H30), C38(H38), C39(H39), C40(H40), C41(H41), C44(H44), C45(H45),
 C46(H46), C47(H47), C56(H56), C57(H57), C59(H59), C60(H60), C64(H64), C65(H65),
  C66(H66), C67(H67), C68(H68)
3.d Idealised Me refined as rotating group:
 C1(H1A,H1B,H1C), C14(H14A,H14B,H14C), C16(H16A,H16B,H16C), C17(H17A,H17B,
 H17C), C19(H19A,H19B,H19C), C20(H20A,H20B,H20C), C27(H27A,H27B,H27C), C35(H35A,
 H35B,H35C), C48(H48A,H48B,H48C), C50(H50A,H50B,H50C), C51(H51A,H51B,H51C),
 C53(H53A,H53B,H53C), C54(H54A,H54B,H54C), C61(H61A,H61B,H61C)
;
_olex2_submission_special_instructions 'No special instructions were received'