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_7131580
_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         'C12 H28 P, B C19 F15 N O2, C0.5 H Cl'
_chemical_formula_sum            'C31.5 H29 B Cl F15 N O2 P'
_chemical_formula_weight         815.79
_space_group_crystal_system      orthorhombic
_space_group_IT_number           18
_space_group_name_Hall           'P 2 2ab'
_space_group_name_H-M_alt        'P 21 21 2'
_atom_sites_solution_hydrogens   mixed
_audit_creation_date             2022-09-10
_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
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   18.0505(4)
_cell_length_b                   21.0295(5)
_cell_length_c                   9.8168(2)
_cell_measurement_reflns_used    9303
_cell_measurement_temperature    150.0
_cell_measurement_theta_max      68.14
_cell_measurement_theta_min      3.23
_cell_volume                     3726.39(14)
_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  'SHELXL 2018/3 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT 2018/2 (Sheldrick, 2018)'
_diffrn_ambient_temperature      150.0
_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           CuK\a
_diffrn_radiation_wavelength     1.54178
_diffrn_reflns_av_R_equivalents  0.0803
_diffrn_reflns_av_unetI/netI     0.0517
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_limit_h_max       21
_diffrn_reflns_limit_h_min       -21
_diffrn_reflns_limit_k_max       25
_diffrn_reflns_limit_k_min       -22
_diffrn_reflns_limit_l_max       11
_diffrn_reflns_limit_l_min       -11
_diffrn_reflns_number            43471
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_theta_full        67.679
_diffrn_reflns_theta_max         68.423
_diffrn_reflns_theta_min         3.226
_diffrn_source_current           1.2
_diffrn_source_power             0.06
_diffrn_source_voltage           50.0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    2.282
_exptl_absorpt_correction_T_max  0.7531
_exptl_absorpt_correction_T_min  0.6392
_exptl_absorpt_correction_type   none
_exptl_absorpt_process_details
;
SADABS-2016/2 (Bruker,2016/2) was used for absorption correction.
wR2(int) was 0.1156 before and 0.0771 after correction.
The Ratio of minimum to maximum transmission is 0.8488.
The \l/2 correction factor is Not present.
;
_exptl_crystal_density_diffrn    1.454
_exptl_crystal_description       block
_exptl_crystal_F_000             1652
_refine_diff_density_max         0.426
_refine_diff_density_min         -0.393
_refine_diff_density_rms         0.050
_refine_ls_abs_structure_details
;
 Flack x determined using 1973 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   0.460(13)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.022
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     487
_refine_ls_number_reflns         6841
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.022
_refine_ls_R_factor_all          0.0589
_refine_ls_R_factor_gt           0.0478
_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^)+(0.0671P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1164
_refine_ls_wR_factor_ref         0.1224
_reflns_Friedel_coverage         0.779
_reflns_Friedel_fraction_full    0.999
_reflns_Friedel_fraction_max     0.998
_reflns_number_gt                5518
_reflns_number_total             6841
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d3cc01571h2.cif
_cod_data_source_block           1_sq
_cod_depositor_comments
'Adding full bibliography for 7131578--7131581.cif.'
_cod_original_formula_sum        'C31.50 H29 B Cl F15 N O2 P'
_cod_database_code               7131580
_shelx_shelxl_version_number     2018/3
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Others
 Fixed Sof: H3A(0.5) H3B(0.5)
3.a Secondary CH2 refined with riding coordinates:
 C3(H3A,H3B)
3.b Idealised Me refined as rotating group:
 C016(H01A,H01B,H01C), C018(H01D,H01E,H01F), C019(H01G,H01H,H01I), C01A(H01J,
 H01K,H01L), C01B(H01M,H01N,H01O), C01C(H01P,H01Q,H01R), C01D(H01S,H01T,H01U),
 C01F(H01V,H01W,H01X), C01G(H01Y,H,HA)
;
_shelx_res_checksum              94536
_shelx_hkl_checksum              55107
_shelx_fab_checksum              20329
_olex2_submission_special_instructions 'No special instructions were received'