(1<i>R</i>)-2-[(3<i>R</i>,4<i>S</i>)-3-Methyl-4-(<i>N</i>-phenyl-<i>N</i>-propionylamino)piperidin-1-yl]-1-phenylethyl <i>p</i>-bromobenzoate and <i>N</i>-{(3<i>R</i>,4<i>S</i>)-1-[(2<i>S</i>)-2-(4-bromophenyl)-2-hydroxyethyl]-3-methyl-piperidin-4-yl}-<i>N</i>-phenylacrylamide
Deschamps, Jeffrey R.; George, Clifford; Flippen-Anderson, Judith L.; Acta Crystallographica Section C 58 (2002) o362–o364; doi:10.1107/S0108270102006443

data_2012770
_publ_section_title
;(1<i>R</i>)-2-[(3<i>R</i>,4<i>S</i>)-3-Methyl-4-(<i>N</i>-phenyl-<i>N</i>-propionylamino)piperidin-1-yl]-1-phenylethyl
 <i>p</i>-bromobenzoate and
 <i>N</i>-{(3<i>R</i>,4<i>S</i>)-1-[(2<i>S</i>)-2-(4-bromophenyl)-2-hydroxyethyl]-3-methyl-piperidin-4-yl}-<i>N</i>-phenylacrylamide
;
_journal_issue                   6
_journal_name_full               'Acta Crystallographica Section C'
_journal_page_first              o362
_journal_page_last               o364
_journal_paper_doi               10.1107/S0108270102006443
_journal_volume                  58
_journal_year                    2002
_chemical_formula_iupac          'C30 H33 Br N2 O3'
_chemical_formula_moiety         'C30 H33 Br N2 O3'
_chemical_formula_sum            'C30 H33 Br N2 O3'
_chemical_formula_weight         549.49
_chemical_name_systematic
;
(1R)-2-[(3R,4S)-3-Methyl-4-(N-phenyl-N-propionylamino)pyridyl]-1-
phenylethyl p-bromobenzoate
;
_space_group_IT_number           4
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  'P 2yb'
_symmetry_space_group_name_H-M   'P 1 21 1'
_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                 92.2080(10)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   10.8806(2)
_cell_length_b                   22.4670(5)
_cell_length_c                   11.5313(3)
_cell_measurement_reflns_used    6392
_cell_measurement_temperature    153(2)
_cell_measurement_theta_max      66.8
_cell_measurement_theta_min      3.93
_cell_volume                     2816.78(11)
_computing_cell_refinement       'SAINT (Bruker, 2001)'
_computing_data_collection       'SMART (Bruker 2001)'
_computing_data_reduction        SAINT
_computing_molecular_graphics    'SHELXTL (Bruker, 2001)'
_computing_structure_refinement  'SHELXTL (Sheldrick, 1997)'
_computing_structure_solution    'SHELXTL (Sheldrick, 1997)'
_diffrn_ambient_temperature      153(2)
_diffrn_measured_fraction_theta_full 0.921
_diffrn_measured_fraction_theta_max 0.921
_diffrn_measurement_device_type  'Bruker CCD area-detector'
_diffrn_measurement_method       \w
_diffrn_radiation_monochromator  'Gobel mirrors'
_diffrn_radiation_source         'rotating anode'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54178
_diffrn_reflns_av_R_equivalents  0.0242
_diffrn_reflns_av_sigmaI/netI    0.0469
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       26
_diffrn_reflns_limit_k_min       -23
_diffrn_reflns_limit_l_max       13
_diffrn_reflns_limit_l_min       -12
_diffrn_reflns_number            13643
_diffrn_reflns_theta_full        67.03
_diffrn_reflns_theta_max         67.03
_diffrn_reflns_theta_min         3.93
_diffrn_standards_decay_%        0.0
_diffrn_standards_interval_time  variable
_diffrn_standards_number         88
_exptl_absorpt_coefficient_mu    2.240
_exptl_absorpt_correction_T_max  0.9307
_exptl_absorpt_correction_T_min  0.6084
_exptl_absorpt_correction_type   integration
_exptl_absorpt_process_details   '(Bruker, 2001)'
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.296
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             1144
_exptl_crystal_size_max          0.56
_exptl_crystal_size_mid          0.44
_exptl_crystal_size_min          0.24
_refine_diff_density_max         0.225
_refine_diff_density_min         -0.445
_refine_ls_abs_structure_details 'Flack (1983)'
_refine_ls_abs_structure_Flack   0.032(15)
_refine_ls_extinction_coef       0.0386(10)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     SHELXTL
_refine_ls_goodness_of_fit_ref   1.066
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     650
_refine_ls_number_reflns         7419
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.066
_refine_ls_R_factor_all          0.0485
_refine_ls_R_factor_gt           0.0471
_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^)+(0.0803P)^2^+0.1540P] where P = (Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1201
_refine_ls_wR_factor_ref         0.1215
_reflns_number_gt                6654
_reflns_number_total             7419
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            sk1544.cif
_cod_data_source_block           II
_cod_depositor_comments
;
The following automatic conversions were performed:
'_symmetry_cell_setting' value 'Monoclinic' changed to 'monoclinic'
according to '/home/saulius/struct/CIF-dictionaries/cif_core.dic'
dictionary named 'cif_core.dic' version 2.4.1 from 2010-06-29.

Automatic conversion script
Id: cif_fix_enum 1527 2010-12-29 10:47:43Z saulius 

The following automatic conversions were performed:

'_symmetry_cell_setting' value 'Monoclinic' changed to 'monoclinic'
according to /home/saulius/struct/CIF-dictionaries/cif_core.dic
dictionary named 'cif_core.dic' version 2.4.1 from 2010-06-29.

Automatic conversion script
Id: cif_fix_values 1715 2011-07-08 13:25:40Z adriana 
;
_cod_original_sg_symbol_H-M      'P 21'
_cod_database_code               2012770
_cod_database_fobs_code          2012770