Crystal structure of <i>S</i>,<i>N</i>-dibenzyl-<small>D</small>-penicillamine monohydrate
Yoshinari, Nobuto; Konno, Takumi; Acta Crystallographica Section E 70 (2014) o1209–; doi:10.1107/S1600536814023459

data_2240137
_publ_section_title
;
 Crystal structure of
 <i>S</i>,<i>N</i>-dibenzyl-<small>D</small>-penicillamine monohydrate
;
_journal_issue                   11
_journal_name_full               'Acta Crystallographica Section E'
_journal_page_first              o1209
_journal_paper_doi               10.1107/S1600536814023459
_journal_volume                  70
_journal_year                    2014
_chemical_formula_iupac          'C19 H23 N O2 S, H2 O'
_chemical_formula_moiety         'C19 H23 N O2 S, H2 O'
_chemical_formula_sum            'C19 H25 N O3 S'
_chemical_formula_weight         347.46
_chemical_name_systematic
;
<i>S</i>,<i>N</i>-Dibenzyl-<i>D</i>-penicillamine monohydrate
;
_space_group_crystal_system      monoclinic
_space_group_IT_number           5
_space_group_name_Hall           'C 2y'
_space_group_name_H-M_alt        'C 1 2 1'
_symmetry_space_group_name_Hall  'C 2y'
_symmetry_space_group_name_H-M   'C 1 2 1'
_atom_sites_solution_hydrogens   mixed
_audit_creation_method           SHELXL-2014
_cell_angle_alpha                90
_cell_angle_beta                 98.715(7)
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   19.930(2)
_cell_length_b                   6.2500(7)
_cell_length_c                   30.645(4)
_cell_measurement_reflns_used    786
_cell_measurement_temperature    200(2)
_cell_measurement_theta_max      27.46
_cell_measurement_theta_min      3.42
_cell_volume                     3773.1(8)
_computing_cell_refinement
;
PROCESS-AUTO (Rigaku, 2000)
;
_computing_data_collection
;
PROCESS-AUTO (Rigaku, 2000)
;
_computing_data_reduction
;
PROCESS-AUTO (Rigaku, 2000)
;
_computing_molecular_graphics
;
<i>Yadokari-XG</i> (Kabuto <i>et al.</i>,  2009)
;
_computing_publication_material
;
<i>Yadokari-XG</i> (Kabuto <i>et al.</i>,  2009)
;
_computing_structure_refinement
;
SHELXL2013 (Sheldrick, 2008)
;
_computing_structure_solution
;
SHELXS2013 (Sheldrick, 2008)
;
_diffrn_ambient_temperature      200(2)
_diffrn_detector_area_resol_mean 10.00
_diffrn_measured_fraction_theta_full 0.996
_diffrn_measured_fraction_theta_max 0.991
_diffrn_measurement_device_type  'Rigaku R-AXIS RAPID'
_diffrn_measurement_method       \w
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71075
_diffrn_reflns_av_R_equivalents  0.0268
_diffrn_reflns_limit_h_max       25
_diffrn_reflns_limit_h_min       -25
_diffrn_reflns_limit_k_max       8
_diffrn_reflns_limit_k_min       -8
_diffrn_reflns_limit_l_max       39
_diffrn_reflns_limit_l_min       -39
_diffrn_reflns_number            15147
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.485
_diffrn_reflns_theta_min         3.100
_exptl_absorpt_coefficient_mu    0.187
_exptl_absorpt_correction_T_max  0.994
_exptl_absorpt_correction_T_min  0.778
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
(ABSCOR; Higashi, 1995)
;
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.223
_exptl_crystal_description       platelet
_exptl_crystal_F_000             1488
_exptl_crystal_size_max          0.150
_exptl_crystal_size_mid          0.100
_exptl_crystal_size_min          0.030
_refine_diff_density_max         0.435
_refine_diff_density_min         -0.252
_refine_ls_abs_structure_details
;
Flack <i>x</i> determined using 2566 quotients
[(<i>I</i>^+^)-(<i>I</i>^-^)]/[(<i>I</i>^+^)+(<i>I</i>^-^)]
(Parsons <i>et al.</i>,  2013)
;
_refine_ls_abs_structure_Flack   0.03(2)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.063
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     461
_refine_ls_number_reflns         7694
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.063
_refine_ls_R_factor_all          0.0473
_refine_ls_R_factor_gt           0.0410
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0482P)^2^+1.2220P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0906
_refine_ls_wR_factor_ref         0.0934
_reflns_number_gt                7006
_reflns_number_total             7694
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            is5378sup1.cf
_cod_data_source_block           I
_cod_original_cell_volume        3773.2(8)
_cod_database_code               2240137
_cod_database_fobs_code          2240137
_shelx_estimated_absorpt_t_min   0.972
_shelx_estimated_absorpt_t_max   0.994
_shelx_hkl_checksum              45715
_shelx_res_checksum              33934
_shelxl_version_number           2014-3