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_7027791
_publ_contact_author
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      Heinrich N\"oth
      Institut f\"ur anorganische Chemie
      Universit\"at M\"unchen
      Meiserstr. 1
      80333 M\"unchen
      Bundesrepublik Deutschland
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_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            'C6 H4 B N3 O2'
_chemical_formula_weight         160.93
_space_group_IT_number           61
_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_Hall  '-P 2ac 2ab'
_symmetry_space_group_name_H-M   'P b c a'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           'SHELXL-CIF-file updated by CIFRTF'
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                90.00
_cell_formula_units_Z            8
_cell_length_a                   7.6720(2)
_cell_length_b                   6.5437(2)
_cell_length_c                   28.2086(9)
_cell_measurement_temperature    293(2)
_cell_volume                     1416.16(7)
_computing_cell_refinement       'XSCANS (Ver. 2.00)'
_computing_data_collection       'XSCANS (Ver. 2.00)'
_computing_data_reduction        'XSCANS (Ver. 2.00)'
_computing_molecular_graphics    'XP (SHELXTL-Plus)'
_computing_publication_material  'SHELXL (Sheldrick 1993'
_computing_structure_refinement  'SHELXL (Sheldrick 1993)'
_computing_structure_solution    'XS (Siemens)'
_diffrn_ambient_temperature      193
_diffrn_detector_area_resol_mean 3
_diffrn_measured_fraction_theta_full 0.665
_diffrn_measured_fraction_theta_max 0.665
_diffrn_measurement_device_type  'Siemens P4'
_diffrn_measurement_method       \w
_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  0.0348
_diffrn_reflns_av_sigmaI/netI    0.0279
_diffrn_reflns_limit_h_max       8
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_k_max       8
_diffrn_reflns_limit_k_min       -8
_diffrn_reflns_limit_l_max       34
_diffrn_reflns_limit_l_min       -34
_diffrn_reflns_number            7184
_diffrn_reflns_theta_full        28.72
_diffrn_reflns_theta_max         28.72
_diffrn_reflns_theta_min         1.44
_diffrn_standards_interval_time  0
_diffrn_standards_number         100
_exptl_absorpt_coefficient_mu    0.114
_exptl_absorpt_correction_T_max  0.9977
_exptl_absorpt_correction_T_min  0.9775
_exptl_absorpt_correction_type   Semi-empirical
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.510
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             656
_exptl_crystal_size_max          0.20
_exptl_crystal_size_mid          0.20
_exptl_crystal_size_min          0.02
_refine_diff_density_max         0.197
_refine_diff_density_min         -0.220
_refine_diff_density_rms         0.049
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.165
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     109
_refine_ls_number_reflns         1429
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.165
_refine_ls_R_factor_all          0.0645
_refine_ls_R_factor_gt           0.0486
_refine_ls_shift/su_max          0.005
_refine_ls_shift/su_mean         0.001
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0369P)^2^+0.8507P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0991
_refine_ls_wR_factor_ref         0.1061
_reflns_number_gt                1159
_reflns_number_total             1429
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            907222esup1.cif
_cod_data_source_block           d:\nixbak\wolfi1
_cod_depositor_comments
;
The following automatic conversions were performed:

'_symmetry_cell_setting' value 'Orthorhombic' changed to
'orthorhombic' according to
/home/saulius/struct/CIF-dictionaries/cif_core.dic dictionary named
'cif_core.dic' version 2.4.2 from
2011-04-26.

'_refine_ls_hydrogen_treatment' value 'mixed ' changed
to 'mixed' according to
/home/saulius/struct/CIF-dictionaries/cif_core.dic dictionary named
'cif_core.dic' version 2.4.2 from 2011-04-26.

Automatic conversion script
Id: cif_fix_values 1891 2012-01-12 08:04:46Z andrius 

The following automatic conversions were performed:

'_refine_ls_weighting_scheme' value 'calc
w=1/[\s^2^(Fo^2^)+(0.0369P)^2^+0.8507P] 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^)+(0.0369P)^2^+0.8507P] where P=(Fo^2^+2Fc^2^)/3'.

Automatic conversion script
Id: cif_fix_values 3143 2015-03-26 13:38:13Z robertas 

The following automatic conversions were performed:

'_atom_sites_solution_primary' value 'direct methods' was changed to
'direct'.

'_atom_sites_solution_hydrogens' value 'geometrically' was changed to
'geom'.

Automatic conversion script
Id: cif_fix_values 6452 2018-10-05 10:23:21Z andrius 
;
_cod_original_sg_symbol_H-M      Pbca
_cod_database_code               7027791