Atropisomeric benzamides and naphthamides as chiral auxiliaries †
Clayden, Jonathan; Helliwell, Madeleine; McCarthy, Catherine; Westlund, Neil; Journal of the Chemical Society, Perkin Transactions 1  (2000) 3232–; doi:10.1039/b004682p

data_7213395
_publ_contact_author
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    ENTER NAME
 ENTER ADDRESS
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_publ_section_title
;
 Atropisomeric benzamides and naphthamides as chiral
 auxiliaries&#x200A;&#x2020;
;
_journal_issue                   19
_journal_name_full
'Journal of the Chemical Society, Perkin Transactions 1'
_journal_page_first              3232
_journal_paper_doi               10.1039/b004682p
_journal_year                    2000
_chemical_formula_sum            'C27 H37 N O3'
_chemical_formula_weight         423.58
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_symmetry_Int_Tables_number      2
_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_date             1999-06-15
_audit_creation_method           'by teXsan v1.7'
_audit_update_record
;
?
;
_cell_angle_alpha                103.229(13)
_cell_angle_beta                 94.072(14)
_cell_angle_gamma                113.705(11)
_cell_formula_units_Z            2
_cell_length_a                   11.0048(15)
_cell_length_b                   12.0970(18)
_cell_length_c                   10.7206(16)
_cell_measurement_reflns_used    19
_cell_measurement_temperature    296.2
_cell_measurement_theta_max      17.0
_cell_measurement_theta_min      14.5
_cell_volume                     1250.6(4)
_computing_cell_refinement       'MSC/AFC Diffractometer Control'
_computing_data_collection       'MSC/AFC Diffractometer Control'
_computing_data_reduction        'teXsan (MSC, 1995)'
_computing_publication_material  'teXsan (MSC, 1995)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution
;
SHELXS86 (Sheldrick, 1985)
;
_diffrn_ambient_temperature      296.2
_diffrn_measured_fraction_theta_full 0.926
_diffrn_measured_fraction_theta_max 0.926
_diffrn_measurement_device       'Rigaku AFC5R'
_diffrn_measurement_method       \w-2\q
_diffrn_orient_matrix_UB_11      0.00615
_diffrn_orient_matrix_UB_12      0.02456
_diffrn_orient_matrix_UB_13      -0.08310
_diffrn_orient_matrix_UB_21      -0.02719
_diffrn_orient_matrix_UB_22      -0.08950
_diffrn_orient_matrix_UB_23      -0.04998
_diffrn_orient_matrix_UB_31      -0.09702
_diffrn_orient_matrix_UB_32      -0.01553
_diffrn_orient_matrix_UB_33      -0.00981
_diffrn_radiation_detector       'scintillation counter'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'Rigaku rotating anode'
_diffrn_radiation_type           'Cu K\a'
_diffrn_radiation_wavelength     1.5418
_diffrn_reflns_av_R_equivalents  0.0154
_diffrn_reflns_av_sigmaI/netI    0.0380
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       13
_diffrn_reflns_limit_l_min       -13
_diffrn_reflns_number            5244
_diffrn_reflns_reduction_process 'Lp corrections applied'
_diffrn_reflns_theta_full        78.20
_diffrn_reflns_theta_max         78.20
_diffrn_reflns_theta_min         4.16
_diffrn_standards_decay_%        1.37
_diffrn_standards_interval_count 150
_diffrn_standards_number         3
_exptl_absorpt_coefficient_mu    0.566
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.866
_exptl_absorpt_correction_type
;
\y scans (North,Phillips & Matthews, 1968)
;
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.125
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             460
_exptl_crystal_size_max          0.50
_exptl_crystal_size_mid          0.37
_exptl_crystal_size_min          0.35
_refine_diff_density_max         0.271
_refine_diff_density_min         -0.217
_refine_diff_density_rms         0.037
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.048
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     290
_refine_ls_number_reflns         4966
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.048
_refine_ls_R_factor_all          0.1272
_refine_ls_R_factor_gt           0.0728
_refine_ls_shift/su_max          0.003
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.1025P)^2^+0.3595P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2005
_refine_ls_wR_factor_ref         0.2382
_reflns_number_gt                2850
_reflns_number_total             4966
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            b004682psup1.cif
_cod_data_source_block           s744
_cod_depositor_comments
;
The following automatic conversions were performed:

'_refine_ls_weighting_scheme' value 'calc
w=1/[\s^2^(Fo^2^)+(0.1025P)^2^+0.3595P] where P=(Fo^2^+2Fc^2^)/3' was
changed to 'calc'. New tag '_refine_ls_weighting_details' was
created. The value of the new tag was set to
'w=1/[\s^2^(Fo^2^)+(0.1025P)^2^+0.3595P] where P=(Fo^2^+2Fc^2^)/3'.

Automatic conversion script
Id: cif_fix_values 3143 2015-03-26 13:38:13Z robertas 
;
_cod_original_cell_volume        1250.6(3)
_cod_original_sg_symbol_H-M      'P -1       '
_cod_database_code               7213395