Crystal Structures of Spiroborates Derived from 2,2'-Dihydroxybiphenyl
Emilie Voisin; Thierry Maris; James D. Wuest; Cryst. Growth & Design 8 (2008) 308–318; doi:10.1021/cg700803k

data_4500051
_publ_section_title
;
 Crystal Structures of Spiroborates Derived from 2,2'-Dihydroxybiphenyl
;
_journal_name_full               'Cryst. Growth & Design'
_journal_page_first              308
_journal_page_last               318
_journal_paper_doi               10.1021/cg700803k
_journal_volume                  8
_journal_year                    2008
_chemical_compound_source        'Synthesized by the authors. See text'
_chemical_formula_moiety         '2(C24 H16 B O4), C4 H8 Cl3 N O, 2(H4 N)'
_chemical_formula_sum            'C52 H48 B2 Cl3 N3 O9'
_chemical_formula_weight         986.90
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           13
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2yac'
_symmetry_space_group_name_H-M   'P 1 2/n 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                 90.344(2)
_cell_angle_gamma                90.00
_cell_formula_units_Z            2
_cell_length_a                   12.8717(4)
_cell_length_b                   12.0303(4)
_cell_length_c                   14.9133(5)
_cell_measurement_reflns_used    9037
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      71.70
_cell_measurement_theta_min      2.96
_cell_volume                     2309.29(13)
_computing_cell_refinement       'SMART (Bruker, 1999)'
_computing_data_collection       'SMART (Bruker, 1999)'
_computing_data_reduction        'SAINT (Bruker, 1999)'
_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 0.994
_diffrn_measured_fraction_theta_max 0.994
_diffrn_measurement_device_type  'Bruker Smart 2000'
_diffrn_measurement_method       \w
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'X-ray Sealed Tube'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54178
_diffrn_reflns_av_R_equivalents  0.033
_diffrn_reflns_av_sigmaI/netI    0.0227
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            24719
_diffrn_reflns_theta_full        72.03
_diffrn_reflns_theta_max         72.03
_diffrn_reflns_theta_min         3.67
_diffrn_standards_decay_%        -0.09
_diffrn_standards_number         133
_exptl_absorpt_coefficient_mu    2.318
_exptl_absorpt_correction_T_max  0.7200
_exptl_absorpt_correction_T_min  0.5200
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'Sadabs (Sheldrick,1996)'
_exptl_crystal_colour            Colorless
_exptl_crystal_density_diffrn    1.419
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             1028
_exptl_crystal_size_max          0.32
_exptl_crystal_size_mid          0.25
_exptl_crystal_size_min          0.14
_refine_diff_density_max         0.993
_refine_diff_density_min         -0.777
_refine_diff_density_rms         0.095
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.078
_refine_ls_matrix_type           full
_refine_ls_number_parameters     387
_refine_ls_number_reflns         4526
_refine_ls_number_restraints     93
_refine_ls_restrained_S_all      1.075
_refine_ls_R_factor_all          0.0861
_refine_ls_R_factor_gt           0.0768
_refine_ls_shift/su_max          0.005
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.1545P)^2^+2.4584P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2383
_refine_ls_wR_factor_ref         0.2474
_reflns_number_gt                3679
_reflns_number_total             4526
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            deposit.cif
_cod_data_source_block           jiw855
_cod_original_sg_symbol_H-M      P2/n
_cod_database_code               4500051