Synthesis and Structural Studies of (R)-(+)-1-[(1-Methylpyrrol-2-yl)acetyl]-4-(1-phenylethyl)semicarbazide
PITUCHA, Monika; RZACZYNSKA, Zofia; MAZUR, Liliana; X-ray Structure Analysis Online 25 (2009) 67–; doi:10.2116/xraystruct.25.67

data_1551808
_publ_section_title
;
 Synthesis and Structural Studies of
 (R)-(+)-1-[(1-Methylpyrrol-2-yl)acetyl]-4-(1-phenylethyl)semicarbazide
;
_journal_name_full               'X-ray Structure Analysis Online'
_journal_page_first              67
_journal_paper_doi               10.2116/xraystruct.25.67
_journal_volume                  25
_journal_year                    2009
_chemical_absolute_configuration syn
_chemical_formula_moiety         'C16 H20 N4 O2'
_chemical_formula_sum            'C16 H20 N4 O2'
_chemical_formula_weight         300.36
_chemical_name_systematic
; 
 (R)-(+)-1-[1-methylpyrrol-2-yl)acetyl]-4-[(1-phenylethyl)semicarbazide 
;
_space_group_IT_number           4
_space_group_name_Hall           'P 2yb'
_space_group_name_H-M_alt        'P 1 21 1'
_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                 103.09(2)
_cell_angle_gamma                90.00
_cell_formula_units_Z            2
_cell_length_a                   10.887(3)
_cell_length_b                   4.6630(10)
_cell_length_c                   15.784(3)
_cell_measurement_reflns_used    69
_cell_measurement_temperature    295(2)
_cell_measurement_theta_max      16
_cell_measurement_theta_min      5
_cell_volume                     780.5(3)
_computing_cell_refinement       'CRYSALIS RED (Oxford Diffraction, 2005b)'
_computing_data_collection       'CRYSALIS CCD (Oxford Diffraction, 2005a)'
_computing_data_reduction        'CRYSALIS RED (Oxford Diffraction, 2005b)'
_computing_molecular_graphics    'SHELXTL/PC (Sheldrick, 1997)'
_computing_publication_material  'SHELXL97 and enCIFer (Allen et al., 2004)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1997)'
_diffrn_ambient_temperature      295(2)
_diffrn_measured_fraction_theta_full 0.996
_diffrn_measured_fraction_theta_max 0.996
_diffrn_measurement_device_type  'Oxford Diffraction Xcalibur diffractometer'
_diffrn_measurement_method       '\w-2\q scan'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0562
_diffrn_reflns_av_sigmaI/netI    0.1198
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       6
_diffrn_reflns_limit_k_min       -6
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_number            3706
_diffrn_reflns_theta_full        27.55
_diffrn_reflns_theta_max         27.55
_diffrn_reflns_theta_min         2.57
_diffrn_standards_decay_%        0.18
_diffrn_standards_interval_count 100
_diffrn_standards_number         3
_exptl_absorpt_coefficient_mu    0.087
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            orange
_exptl_crystal_density_diffrn    1.278
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             320
_exptl_crystal_size_max          0.52
_exptl_crystal_size_mid          0.35
_exptl_crystal_size_min          0.09
_refine_diff_density_max         0.130
_refine_diff_density_min         -0.141
_refine_diff_density_rms         0.032
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   0.04(17)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.969
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     199
_refine_ls_number_reflns         3585
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      0.969
_refine_ls_R_factor_all          0.1979
_refine_ls_R_factor_gt           0.0568
_refine_ls_shift/su_max          0.008
_refine_ls_shift/su_mean         0.001
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0464P)^2^+0.0570P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0904
_refine_ls_wR_factor_ref         0.1247
_reflns_number_gt                1421
_reflns_number_total             3585
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            25_67_1.cif
_cod_data_source_block           I
_cod_original_sg_symbol_H-M      'P 21'
_cod_database_code               1551808