Synthesis and characterization of new azido(o-phenylenedioxy)boranes and azidobicyclononylboranes †
Fraenk, Wolfgang; Habereder, Tassilo; Klapötke, Thomas M.; Nöth, Heinrich; Polborn, Kurt; Journal of the Chemical Society, Dalton Transactions  (1999) 4283–; doi:10.1039/a907222e

data_7027792
_publ_section_title
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 Synthesis and characterization of new azido(o-phenylenedioxy)boranes and
 azidobicyclononylboranes&#x200A;&#x2020;
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_journal_issue                   23
_journal_name_full
'Journal of the Chemical Society, Dalton Transactions'
_journal_page_first              4283
_journal_paper_doi               10.1039/a907222e
_journal_year                    1999
_chemical_formula_sum            'C16 H28 B2 N4'
_chemical_formula_weight         298.04
_chemical_name_systematic
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 ? 
;
_space_group_IT_number           15
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-C 2yc'
_symmetry_space_group_name_H-M   'C 1 2/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL
_cell_angle_alpha                90.000(13)
_cell_angle_beta                 106.29(2)
_cell_angle_gamma                90.00(2)
_cell_formula_units_Z            8
_cell_length_a                   24.819(6)
_cell_length_b                   7.4217(14)
_cell_length_c                   19.099(3)
_cell_measurement_reflns_used    25
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      18
_cell_measurement_theta_min      9
_cell_volume                     3376.8(12)
_computing_cell_refinement       CAD4(Nonius,_1977)
_computing_data_collection       CAD4(Nonius,_1977)
_computing_data_reduction        process_MOLEN(Fair,_1990)
_computing_molecular_graphics    ZORTEP(Zsolnai,_1994)
_computing_publication_material  'SHELXL-93 (Sheldrick, 1993)'
_computing_structure_refinement  'SHELXL-93 (Sheldrick, 1993)'
_computing_structure_solution    'SHELXS-86 (Sheldrick, 1990)'
_diffrn_ambient_temperature      293(2)
_diffrn_measurement_device       Nonius_CAD4
_diffrn_measurement_method       \o-scan
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0201
_diffrn_reflns_av_sigmaI/netI    0.0282
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_diffrn_reflns_limit_h_min       -28
_diffrn_reflns_limit_k_max       0
_diffrn_reflns_limit_k_min       -8
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -20
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_diffrn_reflns_theta_max         23.98
_diffrn_reflns_theta_min         2.39
_diffrn_standards_decay_%        -7.9
_diffrn_standards_interval_time  7200
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_exptl_absorpt_coefficient_mu    0.069
_exptl_absorpt_correction_T_max  0.9998
_exptl_absorpt_correction_T_min  0.8945
_exptl_absorpt_correction_type   empirical
_exptl_crystal_colour            transparent
_exptl_crystal_density_diffrn    1.172
_exptl_crystal_description       plate
_exptl_crystal_F_000             1296
_exptl_crystal_size_max          0.53
_exptl_crystal_size_mid          0.37
_exptl_crystal_size_min          0.23
_refine_diff_density_max         0.147
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_refine_diff_density_rms         0.044
_refine_ls_extinction_method     none
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_refine_ls_restrained_S_obs      1.140
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_refine_ls_R_factor_obs          0.0559
_refine_ls_shift/esd_max         -0.011
_refine_ls_shift/esd_mean        0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0705P)^2^+2.4619P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.1493
_refine_ls_wR_factor_obs         0.1319
_reflns_number_observed          1967
_reflns_number_total             2648
_reflns_observed_criterion       >2sigma(I)
_cod_data_source_file            907222esup1.cif
_cod_data_source_block           fraenka
_cod_depositor_comments
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The following automatic conversions were performed:

'_refine_ls_weighting_scheme' value 'calc
w=1/[\s^2^(Fo^2^)+(0.0705P)^2^+2.4619P] where P=(Fo^2^+2Fc^2^)/3' was
changed to 'calc'. New tag '_refine_ls_weighting_details' was
created. The value of the new tag was set to
'w=1/[\s^2^(Fo^2^)+(0.0705P)^2^+2.4619P] where P=(Fo^2^+2Fc^2^)/3'.

Automatic conversion script
Id: cif_fix_values 3143 2015-03-26 13:38:13Z robertas 
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_cod_original_cell_volume        3376.9(12)
_cod_original_sg_symbol_H-M      C2/c
_cod_database_code               7027792