Novel 5-(4-Substituted-phenyldiazenyl)-1,3,2λ4-oxazaborines and Their Rearrangement to 1,2,4,3λ4-Triazaborines
Pešková, Markéta; Šimůnek, Petr; Bertolasi, Valerio; Macháček, Vladimír; Lyčka, Antonín; Organometallics 25 (2006) 2025–; doi:10.1021/om051078x

data_4074995
_publ_section_title
;
 Novel 5-(4-Substituted-phenyldiazenyl)-1,3,2\l4-oxazaborines and Their
 Rearrangement to 1,2,4,3\l4-Triazaborines
;
_journal_issue                   8
_journal_name_full               Organometallics
_journal_page_first              2025
_journal_paper_doi               10.1021/om051078x
_journal_volume                  25
_journal_year                    2006
_chemical_formula_moiety         'C30 H28 B N3 O2'
_chemical_formula_sum            'C30 H28 B N3 O2'
_chemical_formula_weight         473.36
_chemical_name_systematic
;
 ?
;
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/c 1'
_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                 104.649(1)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   9.6520(1)
_cell_length_b                   18.6355(3)
_cell_length_c                   15.0383(3)
_cell_measurement_reflns_used    7490
_cell_measurement_temperature    295
_cell_measurement_theta_max      27.0
_cell_measurement_theta_min      3.0
_cell_volume                     2617.01(7)
_computing_cell_refinement       'Denzo SMN (Otwinowki & Minor, 1997)'
_computing_data_collection       'COLLECT (Nonius, 1997)'
_computing_data_reduction        'Denzo SMN (Otwinowki & Minor, 1997)'
_computing_molecular_graphics    'ORTEP III (Burnett & Johnson)'
_computing_publication_material
;
SHELXL-97 (Sheldrick, 1997), PARTS (Nardelli, 1995)
;
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SIR97 (Altomare et al., 1999)'
_diffrn_ambient_temperature      295
_diffrn_measured_fraction_theta_full 0.994
_diffrn_measured_fraction_theta_max 0.994
_diffrn_measurement_device_type  'Nonius Kappa CCD'
_diffrn_measurement_method       '\f scans and \w scans'
_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  0.0202
_diffrn_reflns_av_sigmaI/netI    0.0306
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       23
_diffrn_reflns_limit_k_min       -22
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            10874
_diffrn_reflns_theta_full        27.00
_diffrn_reflns_theta_max         27.0
_diffrn_reflns_theta_min         3.0
_exptl_absorpt_coefficient_mu    0.075
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    1.201
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       irregular
_exptl_crystal_F_000             1000
_exptl_crystal_size_max          0.38
_exptl_crystal_size_mid          0.35
_exptl_crystal_size_min          0.18
_refine_diff_density_max         0.716
_refine_diff_density_min         -0.312
_refine_diff_density_rms         0.043
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.038
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     328
_refine_ls_number_reflns         5678
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.038
_refine_ls_R_factor_all          0.1010
_refine_ls_R_factor_gt           0.0766
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.1102P)^2^+1.2053P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2046
_refine_ls_wR_factor_ref         0.2307
_reflns_number_gt                4153
_reflns_number_total             5678
_reflns_threshold_expression     I>2sigma(I)
_cod_data_source_file            om051078xsi20060202_021337.cif
_cod_data_source_block           (12)
_cod_depositor_comments
;
The following automatic conversions were performed:

'_symmetry_cell_setting' value 'Monoclinic' changed to 'monoclinic'
according to /home/saulius/struct/CIF-dictionaries/cif_core.dic
dictionary named 'cif_core.dic' version 2.4.1 from 2010-06-29.

Automatic conversion script
Id: cif_fix_values 1715 2011-07-08 13:25:40Z adriana 
;
_cod_original_sg_symbol_H-M      'P 21/c'
_cod_database_code               4074995