Ethyl (<i>O</i>–<i>B</i>)-5-(difluoroboryloxy)tricyclo[4.3.1.1^3,8^]undecane-4-carboxylate
Argay, Gyula; Kálmán, Alajos; Bernáth, Gábor; Cs. Gyarmati, Zsuzsanna; Acta Crystallographica Section E 59 (2003) o1554–o1555; doi:10.1107/S160053680302066X

data_2202958
_publ_section_title
;Ethyl
 (<i>O</i>--<i>B</i>)-5-(difluoroboryloxy)tricyclo[4.3.1.1^3,8^]undecane-4-carboxylate
;
_journal_issue                   10
_journal_name_full               'Acta Crystallographica Section E'
_journal_page_first              o1554
_journal_page_last               o1555
_journal_paper_doi               10.1107/S160053680302066X
_journal_volume                  59
_journal_year                    2003
_chemical_formula_iupac          'C14 H19 B F2 O3'
_chemical_formula_moiety         'C14 H19 B F2 O3'
_chemical_formula_sum            'C14 H19 B F2 O3'
_chemical_formula_weight         284.10
_chemical_name_systematic
;
ethyl 5-oxotricyclo[4.3.1.1^3,8^]undecane-4-carboxylate difluoroborate
;
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                89.060(10)
_cell_angle_beta                 83.360(10)
_cell_angle_gamma                87.220(10)
_cell_formula_units_Z            2
_cell_length_a                   7.1690(10)
_cell_length_b                   8.0490(10)
_cell_length_c                   11.8580(10)
_cell_measurement_reflns_used    25
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      18.92
_cell_measurement_theta_min      17.97
_cell_volume                     678.82(14)
_computing_cell_refinement       'CAD-4 EXPRESS'
_computing_data_collection       'CAD-4 EXPRESS (Enraf-Nonius, 1992)'
_computing_data_reduction        'XCAD4 (Harms, 1996)'
_computing_molecular_graphics    'ORTEP-3 (Farrugia, 1997)'
_computing_publication_material  SHELXL97
_computing_structure_refinement  'SHELXL97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS97 (Sheldrick, 1997)'
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 1.000
_diffrn_measurement_device       'Enraf-Nonius CAD-4'
_diffrn_measurement_method       \w-\q
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71070
_diffrn_reflns_av_R_equivalents  0.0110
_diffrn_reflns_av_sigmaI/netI    0.0262
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -6
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            6462
_diffrn_reflns_theta_full        34.96
_diffrn_reflns_theta_max         34.96
_diffrn_reflns_theta_min         2.53
_diffrn_standards_decay_%        2
_diffrn_standards_interval_time  60
_diffrn_standards_number         3
_exptl_absorpt_coefficient_mu    0.112
_exptl_absorpt_correction_T_max  0.9513
_exptl_absorpt_correction_T_min  0.9359
_exptl_absorpt_correction_type   psi-scan
_exptl_absorpt_process_details   '(North et al., 1968)'
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.390
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             300
_exptl_crystal_size_max          0.50
_exptl_crystal_size_mid          0.50
_exptl_crystal_size_min          0.45
_refine_diff_density_max         0.302
_refine_diff_density_min         -0.225
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.102
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     182
_refine_ls_number_reflns         5947
_refine_ls_number_restraints     179
_refine_ls_restrained_S_all      1.085
_refine_ls_R_factor_all          0.0893
_refine_ls_R_factor_gt           0.0494
_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^)+(0.0914P)^2^] where P = (Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1583
_refine_ls_wR_factor_ref         0.1700
_reflns_number_gt                3332
_reflns_number_total             5947
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            wn6178.cif
_cod_data_source_block           2
_cod_database_code               2202958
_cod_database_fobs_code          2202958