Racemic 3-Methyl-<i>r</i>-2,<i>c</i>-3,<i>c</i>-5-triphenylpyrrolidine and 3-Methyl-<i>r</i>-2,<i>t</i>-3,<i>c</i>-5-triphenylpyrrolidine
Lucjan B. Jerzykiewicz; Tadeusz Lis; Janusz Baran; Danuta Dziewońska-Baran; Acta Crystallographica Section C 54 (1998) 867–870; doi:10.1107/S0108270197018155

data_2007352
_publ_section_title
;
 Racemic 3-Methyl-<i>r</i>-2,<i>c</i>-3,<i>c</i>-5-triphenylpyrrolidine
 and 3-Methyl-<i>r</i>-2,<i>t</i>-3,<i>c</i>-5-triphenylpyrrolidine
;
_journal_issue                   6
_journal_name_full               'Acta Crystallographica Section C'
_journal_page_first              867
_journal_page_last               870
_journal_paper_doi               10.1107/S0108270197018155
_journal_volume                  54
_journal_year                    1998
_chemical_formula_sum            'C23 H23 N'
_chemical_formula_weight         313.42
_chemical_melting_point          351.6(5)
_chemical_name_systematic
;
3-methyl-r-2,t-3,c-5-triphenylpyrrolidine
;
_space_group_IT_number           29
_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_Hall  'P 2c -2ac'
_symmetry_space_group_name_H-M   'P c a 21'
_audit_creation_method           SHELXL
_cell_angle_alpha                90.
_cell_angle_beta                 90.
_cell_angle_gamma                90.
_cell_formula_units_Z            8
_cell_length_a                   24.52(2)
_cell_length_b                   6.369(6)
_cell_length_c                   22.40(2)
_cell_measurement_reflns_used    67
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      13
_cell_measurement_theta_min      9
_cell_volume                     3498(5)
_computing_cell_refinement       'Kuma KM4 Software'
_computing_data_collection       'Kuma KM4 Software (Kuma Diffraction, 1989)'
_computing_data_reduction        'Kuma KM4 Software'
_computing_molecular_graphics    'ORTEP (Johnson, 1976)'
_computing_structure_refinement  'SHELXL93 (Sheldrick, 1994)'
_computing_structure_solution    'SHELXS86 (Sheldrick, 1990)'
_diffrn_ambient_temperature      100(2)
_diffrn_measurement_device       'Kuma KM4 automatic diffractometer'
_diffrn_measurement_method       'profile data from omega/2theta 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_sigmaI/netI    0.0814
_diffrn_reflns_limit_h_max       36
_diffrn_reflns_limit_h_min       0
_diffrn_reflns_limit_k_max       8
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       33
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_number            4391
_diffrn_reflns_theta_max         32.5
_diffrn_reflns_theta_min         2
_diffrn_standards_decay_%        3
_diffrn_standards_interval_count 100
_diffrn_standards_number         3
_exptl_absorpt_coefficient_mu    0.068
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.190
_exptl_crystal_density_meas      ?
_exptl_crystal_description       needle
_exptl_crystal_F_000             1344
_exptl_crystal_size_max          0.8
_exptl_crystal_size_mid          0.3
_exptl_crystal_size_min          0.2
_refine_diff_density_max         0.38
_refine_diff_density_min         -0.23
_refine_ls_abs_structure_details 'see experimental'
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_all   1.012
_refine_ls_goodness_of_fit_obs   1.124
_refine_ls_hydrogen_treatment    'see experimental'
_refine_ls_matrix_type           full
_refine_ls_number_parameters     438
_refine_ls_number_reflns         4391
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.012
_refine_ls_restrained_S_obs      1.124
_refine_ls_R_factor_all          0.1080
_refine_ls_R_factor_obs          .0580
_refine_ls_shift/esd_max         0.036
_refine_ls_shift/esd_mean        0.004
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w = 1/[\s^2^(Fo^2^)+(0.088P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.1540
_refine_ls_wR_factor_obs         .1355
_reflns_number_observed          2899
_reflns_number_total             4391
_reflns_observed_criterion       >2sigma(I)
_cod_data_source_file            ln1033.cif
_cod_data_source_block           II
_cod_depositor_comments
;
The following automatic conversions were performed:

'_chemical_melting_point' value '78-79 \oC' was changed to '351.6(5)'
- it was converted from degrees Celsius(C) to Kelvins(K), the average
value was taken and precision was estimated.

Automatic conversion script
Id: cif_fix_values 1646 2011-03-28 12:23:43Z adriana 

The following automatic conversions were performed:

'_chemical_melting_point' value '78-79 \oC' was changed to '351.6(5)'
- it was converted from degrees Celsius(C) to Kelvins(K), the average
value was taken and precision was estimated.

Automatic conversion script
Id: cif_fix_values 1715 2011-07-08 13:25:40Z adriana 

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 

The following automatic conversions were performed:

'_refine_ls_weighting_scheme' value 'calc w =
1/[\s^2^(Fo^2^)+(0.088P)^2^] 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^)+(0.088P)^2^] 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        3498(6)
_cod_original_formula_sum        'C23 H23 N1'
_cod_database_code               2007352