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_7131578
_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         'C39 H23 B F15 N2 P, C H2 Cl2'
_chemical_formula_sum            'C40 H25 B Cl2 F15 N2 P'
_chemical_formula_weight         931.30
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2ybc'
_space_group_name_H-M_alt        'P 1 21/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_atom_sites_solution_secondary   difmap
_audit_creation_date             2022-09-12
_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                90.00
_cell_angle_beta                 105.0760(10)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   11.1950(3)
_cell_length_b                   18.3322(4)
_cell_length_c                   19.4142(5)
_cell_measurement_reflns_used    9873
_cell_measurement_temperature    150.0
_cell_measurement_theta_max      68.255
_cell_measurement_theta_min      3.372
_cell_volume                     3847.22(17)
_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    'SHELXS-97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      150.0
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54178
_diffrn_reflns_av_R_equivalents  0.0390
_diffrn_reflns_av_unetI/netI     0.0203
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       22
_diffrn_reflns_limit_k_min       -22
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_number            47599
_diffrn_reflns_theta_full        68.28
_diffrn_reflns_theta_max         68.28
_diffrn_reflns_theta_min         3.37
_diffrn_source                   'fine-focus sealed tube'
_diffrn_source_current           1.2
_diffrn_source_power             0.06
_diffrn_source_voltage           50.0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    2.894
_exptl_absorpt_correction_T_max  0.7531
_exptl_absorpt_correction_T_min  0.6608
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2016/2 (Bruker,2016/2) was used for absorption correction.
wR2(int) was 0.0961 before and 0.0503 after correction.
The Ratio of minimum to maximum transmission is 0.8774.
The \l/2 correction factor is Not present.
;
_exptl_crystal_colour            colourless
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.608
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             1872
_exptl_crystal_size_max          0.13
_exptl_crystal_size_mid          0.11
_exptl_crystal_size_min          0.06
_refine_diff_density_max         0.923
_refine_diff_density_min         -0.970
_refine_diff_density_rms         0.064
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.040
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     561
_refine_ls_number_reflns         7049
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.040
_refine_ls_R_factor_all          0.0502
_refine_ls_R_factor_gt           0.0480
_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^)+(0.0765P)^2^+4.3129P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1361
_refine_ls_wR_factor_ref         0.1380
_reflns_number_gt                6638
_reflns_number_total             7049
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            d3cc01571h2.cif
_cod_data_source_block           12
_cod_depositor_comments
'Adding full bibliography for 7131578--7131581.cif.'
_cod_database_code               7131578
_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:
 C01P(H01T,H01U)
2.b Aromatic/amide H refined with riding coordinates:
 C013(H013), C018(H018), C01A(H01A), C01D(H01E), C01E(H01F), C01F(H01G),
 C01G(H01H), C01H(H01I), C01J(H01M), C01K(H01N), C01L(H01O), C01O(H01S)
2.c Idealised Me refined as rotating group:
 C01B(H01B,H01C,H01D), C01I(H01J,H01K,H01L), C01M(H01P,H01Q,H01R)
;
_olex2_submission_special_instructions 'No special instructions were received'