Crystal Structures of Spiroborates Derived from [1,1'-Binaphthalene]-2,2'-diol (BINOL)
Tao Tu; Thierry Maris; James D. Wuest; Cryst. Growth & Design 8 (2008) 1541–1546; doi:10.1021/cg7008013

data_4500053
_publ_section_title
;
 Crystal Structures of Spiroborates Derived from
 [1,1'-Binaphthalene]-2,2'-diol (BINOL)
;
_journal_name_full               'Cryst. Growth & Design'
_journal_page_first              1541
_journal_page_last               1546
_journal_paper_doi               10.1021/cg7008013
_journal_volume                  8
_journal_year                    2008
_chemical_absolute_configuration rmad
_chemical_compound_source        'Synthesized by the authors. See text'
_chemical_formula_moiety         'C40 H24 B O4, C4 H12 N'
_chemical_formula_sum            'C44 H36 B N O4'
_chemical_formula_weight         653.55
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           18
_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_Hall  'P 2 2ab'
_symmetry_space_group_name_H-M   'P 21 21 2'
_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                 90.00
_cell_angle_gamma                90.00
_cell_formula_units_Z            6
_cell_length_a                   18.6055(5)
_cell_length_b                   21.7959(6)
_cell_length_c                   13.1561(4)
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      30.00
_cell_measurement_theta_min      15.00
_cell_volume                     5335.1(3)
_computing_cell_refinement       'SMART (Bruker, 2001)'
_computing_data_collection       'SMART (Bruker, 2001)'
_computing_data_reduction        'SAINT (Bruker, 2004)'
_computing_molecular_graphics    'SHELXTL (Bruker, 1997)'
_computing_publication_material  'UdMX (local program)'
_computing_structure_refinement  'SHELXL97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS97 (Sheldrick, 1997)'
_diffrn_ambient_temperature      100(2)
_diffrn_detector_area_resol_mean 5.5
_diffrn_measured_fraction_theta_full 0.978
_diffrn_measured_fraction_theta_max 0.978
_diffrn_measurement_device_type  'Bruker AXS Smart 4K/Platform'
_diffrn_measurement_method       \w
_diffrn_radiation_monochromator  'Montel 200 Optics'
_diffrn_radiation_source         'Rotating Anode'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54178
_diffrn_reflns_av_R_equivalents  0.070
_diffrn_reflns_av_sigmaI/netI    0.0640
_diffrn_reflns_limit_h_max       21
_diffrn_reflns_limit_h_min       -21
_diffrn_reflns_limit_k_max       26
_diffrn_reflns_limit_k_min       -26
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_number            31973
_diffrn_reflns_theta_full        68.41
_diffrn_reflns_theta_max         68.41
_diffrn_reflns_theta_min         3.12
_diffrn_standards_decay_%        -0.02
_diffrn_standards_interval_time  1440
_diffrn_standards_number         152
_exptl_absorpt_coefficient_mu    0.608
_exptl_absorpt_correction_T_max  0.9600
_exptl_absorpt_correction_T_min  0.8600
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'Twinabs (Sheldrick, 2004)'
_exptl_crystal_colour            Colourless
_exptl_crystal_density_diffrn    1.220
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       needle
_exptl_crystal_F_000             2064
_exptl_crystal_size_max          0.23
_exptl_crystal_size_mid          0.07
_exptl_crystal_size_min          0.06
_refine_diff_density_max         0.245
_refine_diff_density_min         -0.264
_refine_diff_density_rms         0.058
_refine_ls_abs_structure_details
'The crystal is a multiple twinned specimen, no reliable info'
_refine_ls_abs_structure_Flack   0.6(3)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.056
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     682
_refine_ls_number_reflns         10391
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.056
_refine_ls_R_factor_all          0.0889
_refine_ls_R_factor_gt           0.0684
_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^)+(0.0915P)^2^+0.0167P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1489
_refine_ls_wR_factor_ref         0.1586
_reflns_number_gt                8353
_reflns_number_total             10391
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            deposit.cif
_cod_data_source_block           jiw868
_cod_original_sg_symbol_H-M      P21212
_cod_database_code               4500053