(1<i>R</i>,3<i>R</i>,4<i>S</i>)-1-Benzyl-3-(<i>tert</i>-butyldimethylsilyloxy)-4-(hydroxymethyl)pyrrolidine–borane: novel B—H···H—O hydrogen bonding
Gainsford, Graeme J.; Luxenburger, Andreas; Woolhouse, Anthony D.; Acta Crystallographica Section C 66 (2010) o418–o420; doi:10.1107/S0108270110026879

data_2017751
_publ_section_title
;
 (1<i>R</i>,3<i>R</i>,4<i>S</i>)-1-Benzyl-3-(<i>tert</i>-butyldimethylsilyloxy)-4-(hydroxymethyl)pyrrolidine--borane:
 novel B---H&#x00B7;&#x00B7;&#x00B7;H---O hydrogen bonding
;
_journal_coeditor_code           GD3351
_journal_issue                   8
_journal_name_full               'Acta Crystallographica Section C'
_journal_page_first              o418
_journal_page_last               o420
_journal_paper_doi               10.1107/S0108270110026879
_journal_volume                  66
_journal_year                    2010
_chemical_formula_iupac          'C18 H34 B N O2 Si'
_chemical_formula_moiety         'C18 H34 B N O2 Si'
_chemical_formula_sum            'C18 H34 B N O2 Si'
_chemical_formula_weight         335.36
_chemical_name_systematic
'[(1<i>R</i>,3<i>R</i>,4<i>S</i>)-1-Benzyl-3-(<i>tert</i>-butyldimethylsilyloxy)-4-(hydroxymethyl)pyrrolidine--borane'
_space_group_IT_number           19
_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_Hall  'P 2ac 2ab'
_symmetry_space_group_name_H-M   'P 21 21 21'
_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            4
_cell_length_a                   7.8078(7)
_cell_length_b                   11.2328(10)
_cell_length_c                   23.639(2)
_cell_measurement_reflns_used    9852
_cell_measurement_temperature    113(2)
_cell_measurement_theta_max      27.52
_cell_measurement_theta_min      3.13
_cell_volume                     2073.2(3)
_computing_cell_refinement       'SAINT (Bruker, 2005)'
_computing_data_collection       'APEX2 (Bruker, 2005)'
_computing_data_reduction
;
SAINT  and SADABS (Bruker, 2005)
;
_computing_molecular_graphics
;
ORTEP-3 (Farrugia, 1997); PLATON (Spek, 2009)
;
_computing_publication_material
;
SHELXL97 (Sheldrick, 2008); PLATON (Spek, 2009)
;
_computing_structure_refinement  'SHELXL97 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      113(2)
_diffrn_detector_area_resol_mean 8.333
_diffrn_measured_fraction_theta_full 0.983
_diffrn_measured_fraction_theta_max 0.983
_diffrn_measurement_device_type  'Bruker APEXII CCD'
_diffrn_measurement_method       '\f and \w 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  0.0893
_diffrn_reflns_av_sigmaI/netI    0.0461
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       31
_diffrn_reflns_limit_l_min       -30
_diffrn_reflns_number            42018
_diffrn_reflns_theta_full        27.96
_diffrn_reflns_theta_max         27.96
_diffrn_reflns_theta_min         2.50
_diffrn_standards_decay_%        0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.121
_exptl_absorpt_correction_T_max  0.7456
_exptl_absorpt_correction_T_min  0.4180
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
(Blessing, 1995)
;
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.074
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             736
_exptl_crystal_size_max          0.65
_exptl_crystal_size_mid          0.60
_exptl_crystal_size_min          0.30
_refine_diff_density_max         0.627
_refine_diff_density_min         -0.443
_refine_ls_abs_structure_details 'Flack (1983), 2102 Friedel pairs'
_refine_ls_abs_structure_Flack   0.07(13)
_refine_ls_extinction_coef       0.014(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_ref   1.074
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     225
_refine_ls_number_reflns         4901
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.074
_refine_ls_R_factor_all          0.0565
_refine_ls_R_factor_gt           0.0491
_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^)+(0.0861P)^2^+0.2024P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1262
_refine_ls_wR_factor_ref         0.1336
_reflns_number_gt                4409
_reflns_number_total             4901
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            gd3351.cif
_cod_data_source_block           I
_cod_database_code               2017751
_cod_database_fobs_code          2017751