π-Facial selectivities of diastereotopic ketones: <i>p</i>-bromobenzoates of 4-hetero-1-decalinols
Parvez, Masood; Yadav, Veejendra K.; Balamurugan, Rengarajan; Acta Crystallographica Section C 57 (2001) 1084–1088; doi:10.1107/S0108270101009544

data_2012191
_publ_section_title
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 \p-Facial selectivities of diastereotopic ketones:
 <i>p</i>-bromobenzoates of 4-hetero-1-decalinols
;
_journal_issue                   9
_journal_name_full               'Acta Crystallographica Section C'
_journal_page_first              1084
_journal_page_last               1088
_journal_paper_doi               10.1107/S0108270101009544
_journal_volume                  57
_journal_year                    2001
_chemical_formula_moiety         'C23 H26 Br N O2'
_chemical_formula_sum            'C23 H26 Br N O2'
_chemical_formula_weight         428.36
_chemical_name_common
'N-benzyl-trans-4-aza-1-decalinol p-bromobenzoate'
_chemical_name_systematic
'N-benzyl-trans-4-aza-1-decalinyl p-bromobenzoate'
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_audit_creation_method           SHELXL97
_cell_angle_alpha                78.34(2)
_cell_angle_beta                 78.21(2)
_cell_angle_gamma                61.92(3)
_cell_formula_units_Z            2
_cell_length_a                   9.561(2)
_cell_length_b                   9.822(2)
_cell_length_c                   13.202(3)
_cell_measurement_reflns_used    25
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      25
_cell_measurement_theta_min      20
_cell_volume                     1062.7(5)
_computing_cell_refinement       'CAD-4 Software'
_computing_data_collection       'CAD-4 Software (Enraf-Nonius, 1989)'
_computing_data_reduction
'TEXSAN (Molecular Structure Corporation, 1994)'
_computing_molecular_graphics    'ORTEPII (Johnson, 1976)'
_computing_publication_material  SHELXL97
_computing_structure_refinement  'SHELXL97 (Sheldrick, 1997)'
_computing_structure_solution    'SAPI91 (Fan, 1991)'
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 1.000
_diffrn_measurement_device_type  'Enraf-Nonius CAD-4'
_diffrn_measurement_method       \w/2\q
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54178
_diffrn_reflns_av_R_equivalents  .02
_diffrn_reflns_av_sigmaI/netI    .04
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       0
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_k_min       -9
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_number            3862
_diffrn_reflns_theta_full        67.85
_diffrn_reflns_theta_max         68.0
_diffrn_reflns_theta_min         5.0
_diffrn_standards_decay_%        <2.0
_diffrn_standards_interval_count 200
_diffrn_standards_number         3
_exptl_absorpt_coefficient_mu    2.76
_exptl_absorpt_correction_T_max  .63
_exptl_absorpt_correction_T_min  .31
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_process_details   '\y-scan (3 reflections) (North et al., 1968)'
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.339
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             444
_exptl_crystal_size_max          .52
_exptl_crystal_size_mid          .40
_exptl_crystal_size_min          .17
_refine_diff_density_max         .33
_refine_diff_density_min         -.38
_refine_ls_extinction_coef       .0052(5)
_refine_ls_extinction_method     'SHELXL97 (Sheldrick, 1997)'
_refine_ls_goodness_of_fit_ref   1.03
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     245
_refine_ls_number_reflns         3862
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.03
_refine_ls_R_factor_all          .074
_refine_ls_R_factor_gt           .046
_refine_ls_shift/su_max          <0.001
_refine_ls_shift/su_mean         .00
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w = 1/[\s^2^(Fo^2^)+(0.0545P)^2^+0.43P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_ref         .135
_reflns_number_gt                2585
_reflns_number_total             3862
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            da1192.cif
_cod_data_source_block           XIX
_cod_depositor_comments
;
The following automatic conversions were performed:

'_exptl_crystal_density_meas' value 'not measured' was changed to '?'
- the value is perceived as not measured.

Automatic conversion script
Id: cif_fix_values 3008 2015-01-20 13:52:24Z robertas 
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_cod_original_cell_volume        1062.7(4)
_cod_database_code               2012191
_cod_database_fobs_code          2012191