The impact of Lewis acid variation on reactions with di-<i>tert</i>-butyl diazo diesters.
Bedi, Vaibhav; Mandal, Dipendu; Hussain, Zahid; Chen, Shi-Ming; Wu, Yile; Qu, Zheng-Wang; Grimme, Stefan; Stephan, Douglas W.; Dalton transactions (Cambridge, England : 2003) 53 (2024) 439–443; doi:10.1039/d3dt03506a

data_7714643
_publ_section_title
;
 The impact of Lewis acid variation on reactions with di-<i>tert</i>-butyl
 diazo diesters.
;
_journal_issue                   2
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              439
_journal_page_last               443
_journal_paper_doi               10.1039/d3dt03506a
_journal_volume                  53
_journal_year                    2024
_chemical_formula_moiety         'C13 H23 B N O2'
_chemical_formula_sum            'C13 H23 B N O2'
_chemical_formula_weight         236.157
_space_group_crystal_system      monoclinic
_space_group_IT_number           15
_space_group_name_Hall           '-C 2yc'
_space_group_name_H-M_alt        'C 1 2/c 1'
_symmetry_Int_Tables_number      15
_audit_creation_date             2023-09-26
_audit_creation_method
;
Olex2 1.5
(compiled 2023.08.24 svn.re1ec1418 for OlexSys, GUI svn.r6817)
;
_audit_update_record
;
2023-10-19 deposited with the CCDC.	2023-11-30 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 93.667(8)
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   18.1833(14)
_cell_length_b                   12.0913(14)
_cell_length_c                   12.3509(12)
_cell_measurement_reflns_used    6252
_cell_measurement_temperature    150.01
_cell_measurement_theta_max      27.52
_cell_measurement_theta_min      2.24
_cell_volume                     2709.9(5)
_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  'olex2.refine 1.5 (Bourhis et al., 2015)'
_diffrn_ambient_temperature      150.01
_diffrn_measured_fraction_theta_full 0.9992
_diffrn_measured_fraction_theta_max 0.9992
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0470
_diffrn_reflns_av_unetI/netI     0.0321
_diffrn_reflns_Laue_measured_fraction_full 0.9992
_diffrn_reflns_Laue_measured_fraction_max 0.9992
_diffrn_reflns_limit_h_max       23
_diffrn_reflns_limit_h_min       -23
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_number            25630
_diffrn_reflns_point_group_measured_fraction_full 0.9992
_diffrn_reflns_point_group_measured_fraction_max 0.9992
_diffrn_reflns_theta_full        24.9942
_diffrn_reflns_theta_max         24.99
_diffrn_reflns_theta_min         2.02
_diffrn_source_current           30.0
_diffrn_source_power             1.5
_diffrn_source_voltage           50.0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.075
_exptl_absorpt_correction_T_max  0.7456
_exptl_absorpt_correction_T_min  0.7126
_exptl_absorpt_correction_type   none
_exptl_absorpt_process_details
;
SADABS-2016/2 (Bruker,2016/2) was used for absorption correction.
wR2(int) was 0.0714 before and 0.0479 after correction.
The Ratio of minimum to maximum transmission is 0.9557.
The \l/2 correction factor is Not present.
;
_exptl_crystal_density_diffrn    1.158
_exptl_crystal_description       blocks
_exptl_crystal_F_000             1032.605
_exptl_crystal_size_max          0.3
_exptl_crystal_size_mid          0.1
_exptl_crystal_size_min          0.01
_refine_diff_density_max         0.6250
_refine_diff_density_min         -0.2473
_refine_diff_density_rms         0.0537
_refine_ls_d_res_high            0.8410
_refine_ls_d_res_low             10.0621
_refine_ls_goodness_of_fit_ref   1.0796
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_constraints    34
_refine_ls_number_parameters     157
_refine_ls_number_reflns         2388
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.0796
_refine_ls_R_factor_all          0.0621
_refine_ls_R_factor_gt           0.0481
_refine_ls_shift/su_max          -0.0004
_refine_ls_shift/su_mean         0.0001
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0546P)^2^+4.2702P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1201
_refine_ls_wR_factor_ref         0.1347
_reflns_Friedel_coverage         0.0
_reflns_limit_h_max              21
_reflns_limit_h_min              -21
_reflns_limit_k_max              14
_reflns_limit_k_min              0
_reflns_limit_l_max              14
_reflns_limit_l_min              0
_reflns_number_gt                1922
_reflns_number_total             2388
_reflns_threshold_expression     I>=2u(I)
_cod_data_source_file            d3dt03506a2.cif
_cod_data_source_block           1
_cod_depositor_comments
'Adding full bibliography for 7714643--7714645.cif.'
_cod_database_code               7714643
_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:
 C5(H5), C7(H7)
2.b Secondary CH2 refined with riding coordinates:
 C6(H6a,H6b), C8(H8a,H8b), C11(H11a,H11b), C12(H12a,H12b), C13(H13a,H13b),
 C14(H14a,H14b)
2.c Idealised Me refined as rotating group:
 C9(H9a,H9b,H9c), C3(H3a,H3b,H3c), C2(H2a,H2b,H2c)
;
_olex2_submission_special_instructions 'No special instructions were received'