Boryl azides in 1,3-dipolar cycloadditions.
Müller, Matthias; Maichle-Mössmer, Cäcilia; Bettinger, Holger F.; The Journal of organic chemistry 79 (2014) 5478–5483; doi:10.1021/jo500549m

data_4029482
_publ_section_title
;
 Boryl azides in 1,3-dipolar cycloadditions.
;
_journal_issue                   12
_journal_name_full               'The Journal of organic chemistry'
_journal_page_first              5478
_journal_page_last               5483
_journal_paper_doi               10.1021/jo500549m
_journal_volume                  79
_journal_year                    2014
_chemical_formula_sum            'C20 H37 B2 N3 O5'
_chemical_formula_weight         421.15
_space_group_IT_number           19
_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_Hall  'P 2ac 2ab'
_symmetry_space_group_name_H-M   'P 21 21 21'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   10.4871(5)
_cell_length_b                   11.1272(5)
_cell_length_c                   19.6809(9)
_cell_measurement_reflns_used    6363
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      66.4
_cell_measurement_theta_min      4.493
_cell_volume                     2296.60(18)
_computing_cell_refinement       SAINT
_computing_data_collection       COSMO
_computing_data_reduction        SAINT
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device_type  'APEX II DUO'
_diffrn_measurement_method       'omega/phi scans'
_diffrn_radiation_monochromator  multilayer
_diffrn_radiation_source         'Imus-focus tube'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54178
_diffrn_reflns_av_R_equivalents  0.0274
_diffrn_reflns_av_sigmaI/netI    0.0257
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_number            14432
_diffrn_reflns_theta_full        66.66
_diffrn_reflns_theta_max         66.66
_diffrn_reflns_theta_min         4.49
_exptl_absorpt_coefficient_mu    0.687
_exptl_absorpt_correction_T_max  1.0000
_exptl_absorpt_correction_T_min  0.9472
_exptl_absorpt_correction_type   numerical
_exptl_absorpt_process_details   sadabs
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.218
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       needle
_exptl_crystal_F_000             912
_exptl_crystal_size_max          0.38
_exptl_crystal_size_mid          0.09
_exptl_crystal_size_min          0.03
_refine_diff_density_max         0.203
_refine_diff_density_min         -0.136
_refine_diff_density_rms         0.032
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   -0.02(13)
_refine_ls_extinction_coef       0.00143(14)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     SHELXL
_refine_ls_goodness_of_fit_ref   1.003
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     292
_refine_ls_number_reflns         4041
_refine_ls_number_restraints     19
_refine_ls_restrained_S_all      1.002
_refine_ls_R_factor_all          0.0306
_refine_ls_R_factor_gt           0.0277
_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^)+(0.0347P)^2^+0.3861P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0641
_refine_ls_wR_factor_ref         0.0656
_reflns_number_gt                3805
_reflns_number_total             4041
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            jo500549m_si_003.cif
_cod_data_source_block           neucu_mm779_3
_cod_depositor_comments
'Adding full bibliography for 4029482--4029483.cif.'
_cod_original_sg_symbol_H-M      P212121
_cod_database_code               4029482