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_4312217
_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         'C28 H27 B3 N4 O6, 1.5(C2 H3 N)'
_chemical_formula_sum            'C31 H31.5 B3 N5.5 O6'
_chemical_formula_weight         609.55
_chemical_name_systematic
; 
 ? 
;
_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                 109.441(2)
_cell_angle_gamma                90.00
_cell_formula_units_Z            8
_cell_length_a                   19.790(3)
_cell_length_b                   14.4368(19)
_cell_length_c                   22.334(3)
_cell_measurement_reflns_used    5502
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      27.50
_cell_measurement_theta_min      2.35
_cell_volume                     6017.1(15)
_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      100(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  0.0487
_diffrn_reflns_av_sigmaI/netI    0.0437
_diffrn_reflns_limit_h_max       21
_diffrn_reflns_limit_h_min       -21
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_limit_l_min       -24
_diffrn_reflns_number            18103
_diffrn_reflns_theta_full        23.00
_diffrn_reflns_theta_max         23.00
_diffrn_reflns_theta_min         1.78
_exptl_absorpt_coefficient_mu    0.093
_exptl_absorpt_correction_T_max  1.00
_exptl_absorpt_correction_T_min  0.79
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_process_details   SADABS
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.346
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       rectangular
_exptl_crystal_F_000             2552
_exptl_crystal_size_max          0.27
_exptl_crystal_size_mid          0.21
_exptl_crystal_size_min          0.19
_refine_diff_density_max         0.768
_refine_diff_density_min         -0.287
_refine_diff_density_rms         0.067
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_goodness_of_fit_ref   1.291
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     432
_refine_ls_number_reflns         4204
_refine_ls_number_restraints     5
_refine_ls_restrained_S_all      1.290
_refine_ls_R_factor_all          0.0996
_refine_ls_R_factor_gt           0.0909
_refine_ls_shift/su_max          0.874
_refine_ls_shift/su_mean         0.006
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0417P)^2^+32.9652P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1768
_refine_ls_wR_factor_ref         0.1809
_reflns_number_gt                3827
_reflns_number_total             4204
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic048862erom20040817_081010.cif
_cod_data_source_block           gabisevm
_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_enum 1527 2010-12-29 10:47:43Z saulius 
;
_cod_original_cell_volume        6017.2(14)
_cod_original_formula_sum        'C31 H31.50 B3 N5.50 O6'
_cod_database_code               4312217