Reactivity of frustrated Lewis pairs with BOC protected diazocarboxylates: FLP capture of diazene.
Hussain, Zahid; Luo, Yong-An; Wu, Yile; Qu, Zheng-Wang; Grimme, Stefan; Stephan, Douglas W.; Chemical communications (Cambridge, England) 59 (2023) 6191–6194; doi:10.1039/d3cc01571h

data_7131579
_publ_section_title
;
 Reactivity of frustrated Lewis pairs with BOC protected
 diazocarboxylates: FLP capture of diazene.
;
_journal_issue                   41
_journal_name_full               'Chemical communications (Cambridge, England)'
_journal_page_first              6191
_journal_page_last               6194
_journal_paper_doi               10.1039/d3cc01571h
_journal_volume                  59
_journal_year                    2023
_chemical_formula_moiety         'B2 C38 F30 N2 O4, 2(C23 H18 N), 1.5(C6 H14)'
_chemical_formula_sum            'C93 H57 B2 F30 N4 O4'
_chemical_formula_weight         1886.04
_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   geom
_atom_sites_solution_primary     dual
_audit_creation_date             2022-12-11
_audit_creation_method
;
Olex2 1.5
(compiled 2022.04.07 svn.rca3783a0 for OlexSys, GUI svn.r6498)
;
_audit_update_record
;
2022-12-30 deposited with the CCDC.	2023-04-19 downloaded from the CCDC.
;
_cell_angle_alpha                77.149(2)
_cell_angle_beta                 78.570(3)
_cell_angle_gamma                72.546(3)
_cell_formula_units_Z            1
_cell_length_a                   12.0364(6)
_cell_length_b                   12.5026(5)
_cell_length_c                   15.3806(6)
_cell_measurement_reflns_used    5620
_cell_measurement_temperature    150.0
_cell_measurement_theta_max      62.28
_cell_measurement_theta_min      2.98
_cell_volume                     2131.08(16)
_computing_cell_refinement       'SAINT V8.40B (?, 2016)'
_computing_data_reduction        'SAINT V8.40B (?, 2016)'
_computing_molecular_graphics    'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_structure_refinement  'XL  (Sheldrick, 2008)'
_computing_structure_solution    'SHELXT 2018/2 (Sheldrick, 2018)'
_diffrn_ambient_temperature      150.0
_diffrn_measured_fraction_theta_full 0.991
_diffrn_measured_fraction_theta_max 0.991
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54178
_diffrn_reflns_av_R_equivalents  0.1090
_diffrn_reflns_av_unetI/netI     0.0752
_diffrn_reflns_Laue_measured_fraction_full 0.991
_diffrn_reflns_Laue_measured_fraction_max 0.991
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_number            44396
_diffrn_reflns_point_group_measured_fraction_full 0.991
_diffrn_reflns_point_group_measured_fraction_max 0.991
_diffrn_reflns_theta_full        67.057
_diffrn_reflns_theta_max         67.057
_diffrn_reflns_theta_min         2.977
_diffrn_source_current           1.2
_diffrn_source_power             0.06
_diffrn_source_voltage           50.0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    1.189
_exptl_absorpt_correction_T_max  0.7528
_exptl_absorpt_correction_T_min  0.6553
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2016/2 (Bruker,2016/2) was used for absorption correction.
wR2(int) was 0.1242 before and 0.0843 after correction.
The Ratio of minimum to maximum transmission is 0.8705.
The \l/2 correction factor is Not present.
;
_exptl_crystal_colour            colourless
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.470
_exptl_crystal_description       block
_exptl_crystal_F_000             955
_exptl_crystal_size_max          0.15
_exptl_crystal_size_mid          0.15
_exptl_crystal_size_min          0.06
_refine_diff_density_max         0.572
_refine_diff_density_min         -0.251
_refine_diff_density_rms         0.070
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.002
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     615
_refine_ls_number_reflns         7541
_refine_ls_number_restraints     9
_refine_ls_restrained_S_all      1.004
_refine_ls_R_factor_all          0.1015
_refine_ls_R_factor_gt           0.0696
_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^)+(0.1446P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2028
_refine_ls_wR_factor_ref         0.2392
_reflns_Friedel_coverage         0.000
_reflns_number_gt                4565
_reflns_number_total             7541
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d3cc01571h2.cif
_cod_data_source_block           4
_cod_depositor_comments
'Adding full bibliography for 7131578--7131581.cif.'
_cod_original_cell_volume        2131.08(17)
_cod_database_code               7131579
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   0.932
_shelx_estimated_absorpt_t_min   0.842
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups, All N(H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Rigid bond restraints
 C43, C45, C46, C44, C47, C48
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.02
3. Others
 Fixed Sof: C45(0.75) H45A(0.75) H45B(0.75) C43(0.75) H43A(0.75) H43B(0.75)
 H43C(0.75) C46(0.75) H46A(0.75) H46B(0.75) C44(0.75) H44A(0.75) H44B(0.75)
 C48(0.75) H48A(0.75) H48B(0.75) H48C(0.75) C47(0.75) H47A(0.75) H47B(0.75)
4.a Secondary CH2 refined with riding coordinates:
 C45(H45A,H45B), C46(H46A,H46B), C44(H44A,H44B), C47(H47A,H47B)
4.b Aromatic/amide H refined with riding coordinates:
 N2(H2), C21(H21), C23(H23), C38(H38), C42(H42), C40(H40), C36(H36), C39(H39),
 C34(H34), C41(H41), C30(H30), C35(H35), C32(H32), C26(H26), C28(H28), C27(H27),
  C29(H29), C33(H33)
4.c Idealised Me refined as rotating group:
 C43(H43A,H43B,H43C), C48(H48A,H48B,H48C)
;
_shelx_res_checksum              79633
_shelx_hkl_checksum              84335
_olex2_submission_special_instructions 'No special instructions were received'