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_4500052
_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
'2(C40 H24 B O4), 2(C14 H16 N), C2 H3 N, 3(H2 O)'
_chemical_formula_sum            'C110 H89 B2 N3 O11'
_chemical_formula_weight         1650.46
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           4
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  'P 2yb'
_symmetry_space_group_name_H-M   'P 1 21 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                 108.837(1)
_cell_angle_gamma                90.00
_cell_formula_units_Z            2
_cell_length_a                   15.2276(3)
_cell_length_b                   15.6443(3)
_cell_length_c                   19.1539(3)
_cell_measurement_reflns_used    41255
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      68.75
_cell_measurement_theta_min      2.44
_cell_volume                     4318.55(14)
_computing_cell_refinement       'SMART (Bruker, 2003)'
_computing_data_collection       'SMART (Bruker, 2003)'
_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 Smart 6000'
_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  0.026
_diffrn_reflns_av_sigmaI/netI    0.0193
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_h_min       -18
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_number            59036
_diffrn_reflns_theta_full        69.03
_diffrn_reflns_theta_max         69.03
_diffrn_reflns_theta_min         2.44
_diffrn_standards_decay_%        0.60
_diffrn_standards_number         452
_exptl_absorpt_coefficient_mu    0.643
_exptl_absorpt_correction_T_max  0.9600
_exptl_absorpt_correction_T_min  0.9200
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'Sadabs (Sheldrick,1996)'
_exptl_crystal_colour            Colorless
_exptl_crystal_density_diffrn    1.269
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             1736
_exptl_crystal_size_max          0.12
_exptl_crystal_size_mid          0.11
_exptl_crystal_size_min          0.07
_refine_diff_density_max         0.456
_refine_diff_density_min         -0.327
_refine_diff_density_rms         0.039
_refine_ls_abs_structure_details 'Flack H D (1983), XXXX Friedel Pairs'
_refine_ls_abs_structure_Flack   0.05(12)
_refine_ls_extinction_coef       0.00086(10)
_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   1.038
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1149
_refine_ls_number_reflns         13980
_refine_ls_number_restraints     12
_refine_ls_restrained_S_all      1.087
_refine_ls_R_factor_all          0.0445
_refine_ls_R_factor_gt           0.0437
_refine_ls_shift/su_max          0.004
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0881P)^2^+0.9650P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1195
_refine_ls_wR_factor_ref         0.1213
_reflns_number_gt                13628
_reflns_number_total             13980
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            deposit.cif
_cod_data_source_block           jiw955
_cod_original_sg_symbol_H-M      P21
_cod_database_code               4500052