Preparation and Structural Characterization of Three Types of Homo- and Heterotrinuclear Boron Complexes: Salen{[B-O-B][O2BOH]}, Salen{[B-O-B][O2BPh]}, and Salen{[B-O-B][O2P(O)Ph]}
Gabriela Vargas; Irán Hernández; Herbert Höpfl; María-Eugenia Ochoa; Dolores Castillo; Norberto Farfán; Rosa Santillan; Elizabeth Gómez; Inorganic Chemistry 43 (2004) 8490–8500; doi:10.1021/ic048862e

data_4312215
_publ_section_title
;
 Preparation and Structural Characterization of Three Types of Homo- and
 Heterotrinuclear Boron Complexes: Salen{[B-O-B][O2BOH]},
 Salen{[B-O-B][O2BPh]}, and Salen{[B-O-B][O2P(O)Ph]}
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              8490
_journal_page_last               8500
_journal_paper_doi               10.1021/ic048862e
_journal_volume                  43
_journal_year                    2004
_chemical_formula_moiety         'C16 H15 B3 N2 O6, C3 H6 O'
_chemical_formula_sum            'C19 H21 B3 N2 O7'
_chemical_formula_weight         421.81
_chemical_melting_point          623.15
_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-97
_cell_angle_alpha                90.00
_cell_angle_beta                 99.232(3)
_cell_angle_gamma                90.00
_cell_formula_units_Z            8
_cell_length_a                   25.148(3)
_cell_length_b                   12.0052(16)
_cell_length_c                   13.5464(19)
_cell_measurement_reflns_used    1188
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      17.4
_cell_measurement_theta_min      2.3
_cell_volume                     4036.8(9)
_computing_cell_refinement       'Bruker SAINT'
_computing_data_collection       'Bruker SMART'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 1.000
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       'phi and omega 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  0.1005
_diffrn_reflns_av_sigmaI/netI    0.0742
_diffrn_reflns_limit_h_max       27
_diffrn_reflns_limit_h_min       -27
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       14
_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_number            16058
_diffrn_reflns_theta_full        23.00
_diffrn_reflns_theta_max         23.00
_diffrn_reflns_theta_min         1.64
_exptl_absorpt_coefficient_mu    0.103
_exptl_absorpt_correction_T_max  1.00
_exptl_absorpt_correction_T_min  0.87
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_process_details   SADABS
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.388
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       rectangular
_exptl_crystal_F_000             1760
_exptl_crystal_size_max          0.31
_exptl_crystal_size_mid          0.18
_exptl_crystal_size_min          0.02
_refine_diff_density_max         0.243
_refine_diff_density_min         -0.224
_refine_diff_density_rms         0.050
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.081
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     283
_refine_ls_number_reflns         2815
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.081
_refine_ls_R_factor_all          0.1265
_refine_ls_R_factor_gt           0.0797
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0653P)^2^+7.8005P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1641
_refine_ls_wR_factor_ref         0.1851
_reflns_number_gt                1834
_reflns_number_total             2815
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic048862erom20040817_080945.cif
_cod_data_source_block           rgzvierm
_cod_depositor_comments
;
The following automatic conversions were performed:
'_symmetry_cell_setting' value 'Monoclinic' changed to 'monoclinic'
according to '/home/adriana/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_enum 1555 2011-01-17 13:19:09Z saulius 

The following automatic conversions were performed:

'_chemical_melting_point' value '350_C' was changed to '623.15' - it
was converted from degrees Celsius(C) to Kelvins(K).

Automatic conversion script
Id: cif_fix_values 1569 2011-02-09 13:29:24Z adriana 
;
_cod_original_cell_volume        4036.7(10)
_cod_database_code               4312215