Convenient Method To Access New 4,4-Dialkoxy- and 4,4-Diaryloxy-diaza-s-indacene Dyes: Synthesis and Spectroscopic Evaluation
Chouaib Tahtaoui; Cécile Thomas; François Rohmer; Philippe Klotz; Guy Duportail; Yves Mély; Dominique Bonnet; Marcel Hibert; Journal of Organic Chemistry 72 (2007) 269–272; doi:10.1021/jo061567m

data_4022604
_publ_section_title
;
 Convenient Method To Access New 4,4-Dialkoxy- and
 4,4-Diaryloxy-diaza-s-indacene Dyes: Synthesis
 and Spectroscopic Evaluation
;
_journal_name_full               'Journal of Organic Chemistry'
_journal_page_first              269
_journal_page_last               272
_journal_paper_doi               10.1021/jo061567m
_journal_volume                  72
_journal_year                    2007
_chemical_formula_moiety         'C21 H24 B I N2 O2'
_chemical_formula_sum            'C21 H24 B I N2 O2'
_chemical_formula_weight         474.15
_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'
_audit_creation_date             23-10-00
_cell_angle_alpha                90
_cell_angle_beta                 116.948(5)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   13.2339(4)
_cell_length_b                   13.8249(7)
_cell_length_c                   12.6481(6)
_cell_measurement_temperature    174
_cell_volume                     2062.8(2)
_computing_publication_material  CIFGEN_IN_OpenMoleN_(_1997)
_computing_structure_refinement  LSFM_OpenMoleN_(_1997)
_computing_structure_solution    Direct_methods_(SIR,_Burla_et_al.,_1989)
_diffrn_ambient_temperature      174
_diffrn_measurement_details
;
   8085 reflections were collected using program Collect
 ("Collect" Data collection software, Nonius B.V., 1998)
 The conditions were as follow : crystal to detector distance =  36. mm.
 Scan angle =  2.0 deg 1 scans of   50 sec per frame.
 Data collection was divided into  2 set(s)
 with the following starting angles and number of frames :

 Set 1 Theta =    6.30 Omega =    0.00 Kappa =    0.00   90 frames
 Set 2 Theta =   -6.30 Kappa =  134.00 Phi   =    0.00   17 frames
 Friedel pairs were averaged. Internal R = 0.04
;
_diffrn_measurement_device_type  KappaCCD
_diffrn_measurement_method       '\p scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           Mo-K\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.040
_diffrn_reflns_av_sigmaI/netI    0.333
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            8085
_diffrn_reflns_theta_max         27.46
_diffrn_reflns_theta_min         2.5
_diffrn_source                   xray_tube
_diffrn_standards_decay_%        0
_exptl_absorpt_coefficient_mu    1.570
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    1.53
_exptl_crystal_density_method    none
_exptl_crystal_description       prism
_exptl_crystal_F_000             952
_exptl_crystal_size_max          0.20
_exptl_crystal_size_mid          0.18
_exptl_crystal_size_min          0.08
_refine_diff_density_max         0.425
_refine_diff_density_min         -0.195
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_all   2.474
_refine_ls_goodness_of_fit_ref   1.054
_refine_ls_hydrogen_treatment    noref
_refine_ls_matrix_type           full
_refine_ls_number_constraints    0
_refine_ls_number_parameters     244
_refine_ls_number_reflns         3106
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.052
_refine_ls_R_factor_gt           0.028
_refine_ls_shift/esd_mean        0.000
_refine_ls_shift/su_max          0.002
_refine_ls_structure_factor_coef F
_refine_ls_weighting_scheme      sigma
_refine_ls_wR_factor_all         0.078
_refine_ls_wR_factor_ref         0.033
_reflns_number_gt                3106
_reflns_number_total             4907
_reflns_threshold_expression     >3.0\s(I)
_cod_data_source_file            jo061567msi20060728_101159.cif
_cod_data_source_block           st733
_cod_original_sg_symbol_H-M      'P 21/c'
_cod_database_code               4022604