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_4029483
_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            'C8 H15 N3 O'
_chemical_formula_weight         169.23
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2yn'
_space_group_name_H-M_alt        'P 1 21/n 1'
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 1'
_atom_sites_solution_hydrogens   mixed
_audit_creation_method           SHELXL-2013
_cell_angle_alpha                90
_cell_angle_beta                 107.665(5)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   7.2695(9)
_cell_length_b                   15.2273(19)
_cell_length_c                   8.6831(11)
_cell_measurement_reflns_used    2784
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      24.35
_cell_measurement_theta_min      2.67
_cell_volume                     915.9(2)
_computing_cell_refinement       SAINT
_computing_data_collection       'APEX II'
_computing_data_reduction        SAINT
_computing_structure_refinement  'SHELXL-2013 (Sheldrick, 2013)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      150(2)
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.983
_diffrn_measurement_device_type  'Smart Apex II Duo'
_diffrn_measurement_method       omega/phi-scans
_diffrn_radiation_monochromator  multilayer
_diffrn_radiation_source         'Imus-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0400
_diffrn_reflns_av_unetI/netI     0.0366
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.983
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       10
_diffrn_reflns_limit_l_min       -10
_diffrn_reflns_number            11963
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.983
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.182
_diffrn_reflns_theta_min         2.675
_exptl_absorpt_coefficient_mu    0.084
_exptl_absorpt_correction_T_max  0.9923
_exptl_absorpt_correction_T_min  0.9608
_exptl_absorpt_correction_type   numerical
_exptl_absorpt_process_details   sadabs
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.227
_exptl_crystal_description       Needle
_exptl_crystal_F_000             368
_exptl_crystal_size_max          0.479
_exptl_crystal_size_mid          0.135
_exptl_crystal_size_min          0.092
_refine_diff_density_max         0.202
_refine_diff_density_min         -0.200
_refine_diff_density_rms         0.040
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.874
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     146
_refine_ls_number_reflns         2006
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.874
_refine_ls_R_factor_all          0.0721
_refine_ls_R_factor_gt           0.0444
_refine_ls_shift/su_max          0.008
_refine_ls_shift/su_mean         0.001
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0758P)^2^+0.4359P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1122
_refine_ls_wR_factor_ref         0.1309
_reflns_Friedel_coverage         0.000
_reflns_number_gt                1459
_reflns_number_total             2006
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            jo500549m_si_002.cif
_cod_data_source_block           mo_mmh758_0m
_cod_depositor_comments
'Adding full bibliography for 4029482--4029483.cif.'
_cod_database_code               4029483
_shelx_estimated_absorpt_t_min   0.961
_shelx_estimated_absorpt_t_max   0.992
_shelxl_version_number           2013-3
_shelx_res_checksum              65290
_shelx_hkl_checksum              10597