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_7129029
_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         'C27 H49 B N3 P Si'
_chemical_formula_sum            'C27 H49 B N3 P Si'
_chemical_formula_weight         485.56
_chemical_name_common            PB(N3SiMe3)
_chemical_properties_physical    Air-sensitive,Moisture-sensitive
_space_group_crystal_system      monoclinic
_space_group_IT_number           7
_space_group_name_Hall           'P -2yac'
_space_group_name_H-M_alt        'P 1 n 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_audit_creation_date             2021-08-12
_audit_creation_method
;
Olex2 1.5
(compiled 2021.07.19 svn.r715e62df for OlexSys, GUI svn.r6383)
;
_audit_update_record
;
2021-09-18 deposited with the CCDC.	2021-09-22 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 99.8940(10)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   9.4802(7)
_cell_length_b                   10.2175(8)
_cell_length_c                   15.3118(11)
_cell_measurement_reflns_used    9471
_cell_measurement_temperature    173.15
_cell_measurement_theta_max      27.01
_cell_measurement_theta_min      2.36
_cell_volume                     1461.10(19)
_computing_cell_refinement       'SAINT V8.38A (Bruker, 2018)'
_computing_data_reduction        'SAINT V8.38A (Bruker, 2018)'
_computing_molecular_graphics    'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.5 (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 0.999
_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  0.0302
_diffrn_reflns_av_unetI/netI     0.0277
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            26386
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.997
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.487
_diffrn_reflns_theta_min         1.993
_diffrn_source_current           30.0
_diffrn_source_power             1.35
_diffrn_source_voltage           45.0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.154
_exptl_absorpt_correction_T_max  1.0000
_exptl_absorpt_correction_T_min  0.9166
_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    1.104
_exptl_crystal_description       fragment
_exptl_crystal_F_000             532
_exptl_crystal_recrystallization_method
'Re-crystallisation from solvent: pentane at -40C'
_exptl_crystal_size_max          0.265
_exptl_crystal_size_mid          0.199
_exptl_crystal_size_min          0.192
_refine_diff_density_max         0.245
_refine_diff_density_min         -0.118
_refine_diff_density_rms         0.033
_refine_ls_abs_structure_details
;
 Flack x determined using 2960 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   0.00(2)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.031
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     305
_refine_ls_number_reflns         6671
_refine_ls_number_restraints     2
_refine_ls_restrained_S_all      1.031
_refine_ls_R_factor_all          0.0328
_refine_ls_R_factor_gt           0.0301
_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^)+(0.0430P)^2^+0.1245P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0737
_refine_ls_wR_factor_ref         0.0755
_reflns_Friedel_coverage         0.993
_reflns_Friedel_fraction_full    1.000
_reflns_Friedel_fraction_max     0.995
_reflns_number_gt                6306
_reflns_number_total             6671
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d1cc04923b2.cif
_cod_data_source_block           PB(N3SiMe3)
_cod_depositor_comments
'Adding full bibliography for 7129027--7129035.cif.'
_cod_database_code               7129029
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   0.971
_shelx_estimated_absorpt_t_min   0.960
_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 Ternary CH refined with riding coordinates:
 C13(H13), C10(H10), C19(H19), C7(H7)
2.b Secondary CH2 refined with riding coordinates:
 C24(H24A,H24B), C18(H18A,H18B), C20(H20A,H20B), C23(H23A,H23B), C22(H22A,
 H22B), C14(H14A,H14B), C15(H15A,H15B), C21(H21A,H21B), C16(H16A,H16B),
 C17(H17A,H17B)
2.c Aromatic/amide H refined with riding coordinates:
 C6(H6), C3(H3), C4(H4), C5(H5)
2.d Idealised Me refined as rotating group:
 C12(H12A,H12B,H12C), C9(H9A,H9B,H9C), C11(H11A,H11B,H11C), C8(H8A,H8B,H8C),
 C26(H26A,H26B,H26C), C25(H25A,H25B,H25C), C27(H27A,H27B,H27C)
;
_shelx_res_checksum              53813
_olex2_date_sample_data_collection 2021-08-11
_olex2_date_sample_submission    2021-08-11
_olex2_submission_original_sample_id riv21a7
_olex2_submission_special_instructions 'No special instructions were received'