Access to adducts of parent iminoborane isomers, HBNH and NBH<sub>2</sub>, using frustrated Lewis pair chelation.
Frenette, Brandon L.; Omaña, Alvaro A; Ferguson, Michael J.; Zhou, Yuqiao; Rivard, Eric; Chemical communications (Cambridge, England) 57 (2021) 10895–10898; doi:10.1039/d1cc04923b

data_7129032
_publ_section_title
;
 Access to adducts of parent iminoborane isomers, HBNH and
 NBH<sub>2</sub>, using frustrated Lewis pair chelation.
;
_journal_issue                   83
_journal_name_full
'Chemical communications (Cambridge, England)'
_journal_page_first              10895
_journal_page_last               10898
_journal_paper_doi               10.1039/d1cc04923b
_journal_volume                  57
_journal_year                    2021
_chemical_formula_moiety         'C H2 Cl2, C31 H52 B2 N3 P'
_chemical_formula_sum            'C32 H54 B2 Cl2 N3 P'
_chemical_formula_weight         604.27
_chemical_name_common            PB(NBH2)-DMAP
_chemical_properties_physical    Air-sensitive,Moisture-sensitive
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     dual
_audit_creation_date             2021-09-16
_audit_creation_method
;
Olex2 1.3
(compiled 2020.11.12 svn.r5f609507 for OlexSys, GUI svn.r6272)
;
_audit_update_record
;
2021-09-18 deposited with the CCDC.	2021-09-22 downloaded from the CCDC.
;
_cell_angle_alpha                98.954(2)
_cell_angle_beta                 98.334(2)
_cell_angle_gamma                99.920(2)
_cell_formula_units_Z            2
_cell_length_a                   9.5926(12)
_cell_length_b                   11.0351(14)
_cell_length_c                   16.641(2)
_cell_measurement_reflns_used    4652
_cell_measurement_temperature    173.15
_cell_measurement_theta_max      22.64
_cell_measurement_theta_min      2.19
_cell_volume                     1687.1(4)
_computing_cell_refinement       'SAINT V8.38A (Bruker, 2018)'
_computing_data_reduction        'SAINT V8.38A (Bruker, 2018)'
_computing_publication_material  'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2018/3 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT 2018/2 (Sheldrick, 2018)'
_diffrn_ambient_temperature      173.15
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0498
_diffrn_reflns_av_unetI/netI     0.0457
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            30383
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.179
_diffrn_reflns_theta_min         1.259
_diffrn_source_current           30.0
_diffrn_source_power             1.35
_diffrn_source_voltage           45.0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.266
_exptl_absorpt_correction_T_max  1.0000
_exptl_absorpt_correction_T_min  0.9132
_exptl_absorpt_correction_type   numerical
_exptl_absorpt_process_details
'SADABS 2016/2: Krause, L., Herbst-Irmer, R., Sheldrick G.M. & Stalke D.,  J. Appl. Cryst. 48 (2015) 3-10'
_exptl_crystal_colour            colourless
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.189
_exptl_crystal_description       fragment
_exptl_crystal_F_000             652
_exptl_crystal_recrystallization_method
'Re-crystallisation from solvent: hexanes/DCM at -40C'
_exptl_crystal_size_max          0.186
_exptl_crystal_size_mid          0.169
_exptl_crystal_size_min          0.086
_refine_diff_density_max         0.312
_refine_diff_density_min         -0.341
_refine_diff_density_rms         0.044
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.023
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     403
_refine_ls_number_reflns         7484
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.023
_refine_ls_R_factor_all          0.0676
_refine_ls_R_factor_gt           0.0430
_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^)+(0.0477P)^2^+0.3880P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0991
_refine_ls_wR_factor_ref         0.1116
_reflns_Friedel_coverage         0.000
_reflns_number_gt                5428
_reflns_number_total             7484
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d1cc04923b2.cif
_cod_data_source_block           PB(NBH2)-DMAP
_cod_depositor_comments
'Adding full bibliography for 7129027--7129035.cif.'
_cod_database_code               7129032
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   0.978
_shelx_estimated_absorpt_t_min   0.952
_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. Others
 Sof(Cl1B)=Sof(Cl2B)=Sof(C32B)=Sof(H32C)=Sof(H32D)=1-FVAR(1)
 Sof(Cl1A)=Sof(Cl2A)=Sof(C32A)=Sof(H32A)=Sof(H32B)=FVAR(1)
3.a Ternary CH refined with riding coordinates:
 C7(H7), C10(H10), C13(H13), C19(H19)
3.b Secondary CH2 refined with riding coordinates:
 C14(H14A,H14B), C15(H15A,H15B), C16(H16A,H16B), C17(H17A,H17B), C18(H18A,
 H18B), C20(H20A,H20B), C21(H21A,H21B), C22(H22A,H22B), C23(H23A,H23B),
 C24(H24A,H24B), C32A(H32A,H32B), C32B(H32C,H32D)
3.c Aromatic/amide H refined with riding coordinates:
 C3(H3), C4(H4), C5(H5), C6(H6), C25(H25), C26(H26), C28(H28), C29(H29)
3.d Idealised Me refined as rotating group:
 C8(H8A,H8B,H8C), C9(H9A,H9B,H9C), C11(H11A,H11B,H11C), C12(H12A,H12B,H12C),
 C30(H30A,H30B,H30C), C31(H31A,H31B,H31C)
;
_shelx_res_checksum              54697
_olex2_date_sample_data_collection 2021-07-20
_olex2_date_sample_submission    2021-07-20
_olex2_exptl_crystal_mounting_method
'A suitable crystal was coated in Paratone oil and mounted on a loop.'
_olex2_submission_original_sample_id riv21a1
_olex2_submission_special_instructions 'No special instructions were received'