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_7131581
_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         'C44 H31 B F15 N2 O2 P, 0.25(C2 H3 N)'
_chemical_formula_sum            'C44.5 H31.75 B F15 N2.25 O2 P'
_chemical_formula_weight         956.75
_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
_audit_creation_date             2022-12-19
_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                99.604(2)
_cell_angle_beta                 106.074(2)
_cell_angle_gamma                93.126(2)
_cell_formula_units_Z            4
_cell_length_a                   13.2472(4)
_cell_length_b                   18.1497(6)
_cell_length_c                   18.8421(6)
_cell_measurement_reflns_used    7653
_cell_measurement_temperature    302.00
_cell_measurement_theta_max      67.72
_cell_measurement_theta_min      2.49
_cell_volume                     4267.8(2)
_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      302.00
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.987
_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  0.1058
_diffrn_reflns_av_unetI/netI     0.1133
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.987
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       22
_diffrn_reflns_limit_k_min       -22
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            55658
_diffrn_reflns_point_group_measured_fraction_full 0.997
_diffrn_reflns_point_group_measured_fraction_max 0.987
_diffrn_reflns_theta_full        67.679
_diffrn_reflns_theta_max         70.305
_diffrn_reflns_theta_min         3.163
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    1.538
_exptl_absorpt_correction_type   none
_exptl_crystal_density_diffrn    1.489
_exptl_crystal_description       blocks
_exptl_crystal_F_000             1942
_refine_diff_density_max         0.896
_refine_diff_density_min         -0.937
_refine_diff_density_rms         0.113
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.963
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1211
_refine_ls_number_reflns         16076
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.963
_refine_ls_R_factor_all          0.1588
_refine_ls_R_factor_gt           0.1101
_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^)+(0.2000P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2720
_refine_ls_wR_factor_ref         0.3298
_reflns_Friedel_coverage         0.000
_reflns_number_gt                7922
_reflns_number_total             16076
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d3cc01571h2.cif
_cod_data_source_block           4_CCDC1
_cod_depositor_comments
'Adding full bibliography for 7131578--7131581.cif.'
_cod_original_formula_sum        'C44.50 H31.75 B F15 N2.25 O2 P'
_cod_database_code               7131581
_shelx_shelxl_version_number     2018/3
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All N(H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Others
 Fixed Sof: C29(0.5) H29A(0.5) H29B(0.5) H29C(0.5) C28(0.5) N2(0.5)
3.a Riding coordinates:
 N00P(H00P), N00X(H00X)
3.b Aromatic/amide H refined with riding coordinates:
 C01T(H01T), C01Z(H01Z), C026(H026), C24(H24), C02D(H02G), C02J(H02J),
 C02K(H02K), C02N(H02N), C02P(H02P), C02Q(H02Q), C02V(H02V), C02X(H02X), C1(H1),
  C5(H5), C13(H13), C7(H7), C8(H8), C9(H9), C10(H10), C11(H11), C14(H14),
 C19(H19), C21(H21), C25(H25)
3.c Idealised Me refined as rotating group:
 C02C(H02D,H02E,H02F), C02H(H02A,H02B,H02C), C3(H3A,H3B,H3C), C4(H4A,H4B,H4C),
 C16(H16A,H16B,H16C), C2(H2A,H2B,H2C), C17(H17A,H17B,H17C), C12(H12A,H12B,H12C),
  C15(H15A,H15B,H15C), C18(H18A,H18B,H18C), C20(H20A,H20B,H20C), C22(H22A,H22B,
 H22C), C29(H29A,H29B,H29C)
;
_shelx_res_checksum              96420
_shelx_hkl_checksum              66003
_olex2_submission_special_instructions 'No special instructions were received'