Crystal structures of ethanol hemisolvates of (1S,3R,4S,8S,9R)-1N-boranyl-6'- methoxy-cinchonan-9-ol, C~20~H~27~BN~2~O~2~ · ½C~2~H~5~OH, and (1S,3S,4S,8S,9R)-1N-boranyl-10,11-didehydro-6'-methoxy-cinchonan-9-ol, C~20~H~25~BN~2~O~2~ · ½C~2~H~5~OH
R. Wartchow; S. Roeper; H. M. R. Hoffmann; Zeitschrift für Kristallographie - New Crystal Structures 220 (2005) 89–92; doi:

data_8101708
_publ_section_title
;
Crystal structures of ethanol hemisolvates of (1S,3R,4S,8S,9R)-1N-boranyl-6'-
methoxy-cinchonan-9-ol, C~20~H~27~BN~2~O~2~ &#x00B7; &#x00BD;C~2~H~5~OH, and 
(1S,3S,4S,8S,9R)-1N-boranyl-10,11-didehydro-6'-methoxy-cinchonan-9-ol, 
C~20~H~25~BN~2~O~2~ &#x00B7; &#x00BD;C~2~H~5~OH
;
_journal_issue                   1
_journal_name_full
'Zeitschrift f\"ur Kristallographie - New Crystal Structures'
_journal_page_first              89
_journal_page_last               92
_journal_volume                  220
_journal_year                    2005
_chemical_compound_source        'synthetic starting from a natural product'
_chemical_formula_moiety         'C20 H27 B N2 O2, 0.5(C2 H6 O)'
_chemical_formula_sum            'C21 H30 B N2 O2.5'
_chemical_formula_weight         361.28
_chemical_name_common            'quinineborane ethanol hemisolvate'
_chemical_name_systematic
;    
(1S,3R,4S,8S,9R)-1N-boranyl-6'-methoxy-cinchonan-9-ol ethanol hemisolvate
;
_space_group_IT_number           146
_symmetry_cell_setting           trigonal
_symmetry_Int_Tables_number      146
_symmetry_space_group_name_Hall  'R 3'
_symmetry_space_group_name_H-M   'R 3 :H'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                120.00
_cell_formula_units_Z            9
_cell_length_a                   26.759(5)
_cell_length_b                   26.759(5)
_cell_length_c                   7.431(2)
_cell_measurement_reflns_used    8000
_cell_measurement_temperature    300(2)
_cell_measurement_theta_max      25.25
_cell_measurement_theta_min      2.55
_cell_volume                     4608.1(17)
_computing_cell_refinement       'Stoe IPDS software'
_computing_data_collection       'Stoe IPDS software'
_computing_data_reduction        'Stoe IPDS software and SHELXL-93'
_computing_molecular_graphics    'PLATON (Spek, 1990)'
_computing_publication_material
;
 The first CIF was issued by SHELXL-93.
 The edited CIF is finally treated with the program CIF2SX 
 written by L. Farrugia, Univ. of Glasgow (1997) 
 and a refinement cycle is repeated to assure that 
 essential parameters were not changed. 
;
_computing_structure_refinement  'SHELXL-93 (Sheldrick, 1993)'
_computing_structure_solution    'SHELXS-86 (Sheldrick, 1990)'
_diffrn_ambient_temperature      300(2)
_diffrn_measured_fraction_theta_max 1.0
_diffrn_measurement_device       'Stoe IPDS area detector diffractometer'
_diffrn_measurement_method       '240 exposures, \D \f = 1.5\%'
_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  0.0616
_diffrn_reflns_av_sigmaI/netI    0.0462
_diffrn_reflns_limit_h_max       32
_diffrn_reflns_limit_h_min       -32
_diffrn_reflns_limit_k_max       31
_diffrn_reflns_limit_k_min       -32
_diffrn_reflns_limit_l_max       9
_diffrn_reflns_limit_l_min       -9
_diffrn_reflns_number            22063
_diffrn_reflns_theta_max         26.16
_diffrn_reflns_theta_min         2.64
_diffrn_standards_decay_%        0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.076
_exptl_absorpt_correction_T_max  1.0
_exptl_absorpt_correction_T_min  1.0
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            'colourless '
_exptl_crystal_density_diffrn    1.172
_exptl_crystal_description       'hexagonal prism'
_exptl_crystal_F_000             1755
_exptl_crystal_size_max          0.96
_exptl_crystal_size_mid          0.74
_exptl_crystal_size_min          0.63
_refine_diff_density_max         0.286
_refine_diff_density_min         -0.196
_refine_diff_density_rms         0.031
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   0.31(156)
_refine_ls_extinction_coef       0.0014(2)
_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_all   1.162
_refine_ls_goodness_of_fit_ref   1.419
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     281
_refine_ls_number_reflns         4023
_refine_ls_number_restraints     58
_refine_ls_restrained_S_all      1.292
_refine_ls_restrained_S_obs      1.584
_refine_ls_R_factor_all          0.0656
_refine_ls_R_factor_gt           0.0412
_refine_ls_shift/esd_mean        0.000
_refine_ls_shift/su_max          0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.04P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.0979
_refine_ls_wR_factor_ref         0.0942
_reflns_number_gt                2599
_reflns_number_total             4023
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            1267-1443.cff
_cod_data_source_block           1
_cod_original_sg_symbol_H-M      'R 3'
_cod_original_formula_sum        'C21 H30 B N2 O2.50'
_cod_database_code               8101708