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_7714645
_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         'B0.5 C12 F10, C4 H9.5 N'
_chemical_formula_sum            'C16 H9.5 B0.5 F10 N'
_chemical_formula_weight         411.157
_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                 95.375(6)
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   20.394(3)
_cell_length_b                   8.2279(11)
_cell_length_c                   19.557(3)
_cell_measurement_reflns_used    3733
_cell_measurement_temperature    150.02
_cell_measurement_theta_max      21.96
_cell_measurement_theta_min      2.76
_cell_volume                     3267.2(8)
_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      150.02
_diffrn_measured_fraction_theta_full 0.9997
_diffrn_measured_fraction_theta_max 0.9997
_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  0.0749
_diffrn_reflns_av_unetI/netI     0.0520
_diffrn_reflns_Laue_measured_fraction_full 0.9997
_diffrn_reflns_Laue_measured_fraction_max 0.9997
_diffrn_reflns_limit_h_max       25
_diffrn_reflns_limit_h_min       -25
_diffrn_reflns_limit_k_max       10
_diffrn_reflns_limit_k_min       -10
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_limit_l_min       -24
_diffrn_reflns_number            32500
_diffrn_reflns_point_group_measured_fraction_full 0.9997
_diffrn_reflns_point_group_measured_fraction_max 0.9997
_diffrn_reflns_theta_full        24.9934
_diffrn_reflns_theta_max         24.99
_diffrn_reflns_theta_min         2.01
_diffrn_source_current           30.0
_diffrn_source_power             1.5
_diffrn_source_voltage           50.0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.178
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            orange
_exptl_crystal_colour_primary    orange
_exptl_crystal_density_diffrn    1.672
_exptl_crystal_description       Block
_exptl_crystal_F_000             1641.935
_exptl_crystal_size_max          0.34
_exptl_crystal_size_mid          0.24
_exptl_crystal_size_min          0.22
_refine_diff_density_max         0.4123
_refine_diff_density_min         -0.3941
_refine_diff_density_rms         0.1030
_refine_ls_d_res_high            0.8411
_refine_ls_d_res_low             10.1524
_refine_ls_goodness_of_fit_ref   1.0887
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_constraints    14
_refine_ls_number_parameters     252
_refine_ls_number_reflns         2869
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.0887
_refine_ls_R_factor_all          0.0832
_refine_ls_R_factor_gt           0.0395
_refine_ls_shift/su_max          -0.0002
_refine_ls_shift/su_mean         0.0000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0354P)^2^+3.1341P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0784
_refine_ls_wR_factor_ref         0.0992
_reflns_Friedel_coverage         0.0
_reflns_limit_h_max              24
_reflns_limit_h_min              -24
_reflns_limit_k_max              9
_reflns_limit_k_min              0
_reflns_limit_l_max              23
_reflns_limit_l_min              0
_reflns_number_gt                1869
_reflns_number_total             2869
_reflns_threshold_expression     I>=2u(I)
_cod_data_source_file            d3dt03506a2.cif
_cod_data_source_block           2
_cod_depositor_comments
'Adding full bibliography for 7714643--7714645.cif.'
_cod_database_code               7714645
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All N(H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Others
 Fixed Sof: H1(0.5)
3.a Aromatic/amide H refined with riding coordinates:
 N1(H1)
3.b Idealised Me refined as rotating group:
 C26(H26a,H26b,H26c), C27(H27a,H27b,H27c), C28(H28a,H28b,H28c)
;
_olex2_submission_special_instructions 'No special instructions were received'