Synthesis, characterization and X-ray studies of new six-seven membered rings [4.5.0] heterobicyclic system of monomeric boronates
Riveraa, Jose Maria; Mendeza, Enrique; Colorado-Peraltab, Raul; Rinconc, Susana; Farfanb, Norberto; Santillan, Rosa; Inorganica Chimica Acta 390 (2012) 26–32; doi:10.1016/j.ica.2012.03.055

data_1508215
_publ_section_title
;
 Synthesis, characterization and X-ray studies of new six-seven membered
 rings [4.5.0] heterobicyclic system of monomeric boronates
;
_journal_name_full
;
Inorganica Chimica Acta
;
_journal_page_first              26
_journal_page_last               32
_journal_paper_doi               10.1016/j.ica.2012.03.055
_journal_volume                  390
_journal_year                    2012
_chemical_formula_moiety         'C22 H21 B2 N O3'
_chemical_formula_sum            'C22 H21 B2 N O3'
_chemical_formula_weight         369.02
_chemical_melting_point          478(2)
_chemical_name_common            Diboronates
_chemical_name_systematic
;
9-methyl-2,4-diphenylbenzo[j]-8-aza-1,3,5,2,4-trioxadiboraciclo
undec-8-ene
;
_space_group_IT_number           9
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  'C -2yc'
_symmetry_space_group_name_H-M   'C 1 c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_cell_angle_alpha                90.00
_cell_angle_beta                 122.5560(10)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   14.8600(3)
_cell_length_b                   14.4010(4)
_cell_length_c                   10.8940(3)
_cell_measurement_temperature    293(2)
_cell_volume                     1964.98(9)
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 0.958
_diffrn_measured_fraction_theta_max 0.958
_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  0.0076
_diffrn_reflns_av_sigmaI/netI    0.0409
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       14
_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_number            4013
_diffrn_reflns_theta_full        27.46
_diffrn_reflns_theta_max         27.46
_diffrn_reflns_theta_min         3.60
_exptl_absorpt_coefficient_mu    0.061
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    0.936
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             582
_exptl_crystal_size_max          0.1x0.2x0.1
_refine_diff_density_max         0.157
_refine_diff_density_min         -0.108
_refine_diff_density_rms         0.026
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   0.9(11)
_refine_ls_extinction_coef       0.018(2)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     SHELXL
_refine_ls_goodness_of_fit_ref   0.992
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     270
_refine_ls_number_reflns         4006
_refine_ls_number_restraints     2
_refine_ls_restrained_S_all      0.991
_refine_ls_R_factor_all          0.0619
_refine_ls_R_factor_gt           0.0415
_refine_ls_shift/su_max          0.047
_refine_ls_shift/su_mean         0.006
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0621P)^2^+0.3552P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1019
_refine_ls_wR_factor_ref         0.1157
_reflns_number_gt                3104
_reflns_number_total             4006
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            6b.cif.txt
_cod_data_source_block           publication_text
_cod_depositor_comments
;
The following automatic conversions were performed:

'_chemical_melting_point' value '203-207 C' was changed to '478(2)' -
it was converted from degrees Celsius(C) to Kelvins(K), the average
value was taken and precision was estimated.

Automatic conversion script
Id: cif_fix_values 1715 2011-07-08 13:25:40Z adriana 

2017-03-17
Fixing wrong Z value                 miguel
;
_cod_original_sg_symbol_H-M      'C c'
_cod_original_formula_units_Z    3
_cod_database_code               1508215