Ethyl 1-[5-amino-1-<i>tert</i>-butyl-3-(methylsulfanyl)-1<i>H</i>-pyrazole-4-carbonyl]-5-methyl-3-(methylsulfanyl)-1<i>H</i>-pyrazole-4-carboxylate
Jun-Fei Li; Hai-Bin Song; You-Quan Zhu; Hua-Zheng Yang; Acta Crystallographica Section E 62 (2006) o1679–o1681; doi:10.1107/S1600536806011500

data_2208777
_publ_section_title
;Ethyl
 1-[5-amino-1-<i>tert</i>-butyl-3-(methylsulfanyl)-1<i>H</i>-pyrazole-4-carbonyl]-5-methyl-3-(methylsulfanyl)-1<i>H</i>-pyrazole-4-carboxylate
;
_journal_coeditor_code           AC2011
_journal_issue                   5
_journal_name_full               'Acta Crystallographica Section E'
_journal_page_first              o1679
_journal_page_last               o1681
_journal_paper_doi               10.1107/S1600536806011500
_journal_volume                  62
_journal_year                    2006
_chemical_formula_iupac          'C17 H25 N5 O3 S2'
_chemical_formula_moiety         'C17 H25 N5 O3 S2'
_chemical_formula_sum            'C17 H25 N5 O3 S2'
_chemical_formula_weight         411.54
_chemical_name_systematic
;
Ethyl
1-[5-amino-1-tert-butyl-3-(methylsulfanyl)-1H-pyrazole-4-carbonyl]-5-methyl-
3-(methylsulfanyl)-1H-pyrazole-4-carboxylate
;
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_cell_angle_alpha                90.00
_cell_angle_beta                 105.976(2)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   9.3972(14)
_cell_length_b                   22.870(3)
_cell_length_c                   10.4065(16)
_cell_measurement_reflns_used    4518
_cell_measurement_temperature    294(2)
_cell_measurement_theta_max      26.44
_cell_measurement_theta_min      2.25
_cell_volume                     2150.1(5)
_computing_cell_refinement       SMART
_computing_data_collection       'SMART (Bruker, 1999)'
_computing_data_reduction        'SAINT (Bruker, 1999)'
_computing_molecular_graphics    'SHELXTL (Bruker, 1999)'
_computing_publication_material  SHELXTL
_computing_structure_refinement  'SHELXL97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS97 (Sheldrick, 1997)'
_diffrn_ambient_temperature      294(2)
_diffrn_measured_fraction_theta_full 0.994
_diffrn_measured_fraction_theta_max 0.994
_diffrn_measurement_device_type  'Bruker SMART CCD area-detector'
_diffrn_measurement_method       '\f and \w'
_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  0.0333
_diffrn_reflns_av_sigmaI/netI    0.0403
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       -28
_diffrn_reflns_limit_l_max       9
_diffrn_reflns_limit_l_min       -13
_diffrn_reflns_number            12099
_diffrn_reflns_theta_full        26.49
_diffrn_reflns_theta_max         26.49
_diffrn_reflns_theta_min         2.22
_diffrn_standards_decay_%        0
_diffrn_standards_interval_count 0
_diffrn_standards_interval_time  0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.274
_exptl_absorpt_correction_T_max  0.968
_exptl_absorpt_correction_T_min  0.940
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   '(SADABS; Sheldrick, 1996)'
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.271
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             872
_exptl_crystal_size_max          0.20
_exptl_crystal_size_mid          0.16
_exptl_crystal_size_min          0.12
_refine_diff_density_max         0.268
_refine_diff_density_min         -0.252
_refine_ls_extinction_coef       0.0097(11)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     SHELXL97
_refine_ls_goodness_of_fit_ref   1.033
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     270
_refine_ls_number_reflns         4426
_refine_ls_number_restraints     14
_refine_ls_restrained_S_all      1.043
_refine_ls_R_factor_all          0.0663
_refine_ls_R_factor_gt           0.0430
_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^)+(0.0506P)^2^+0.8773P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1043
_refine_ls_wR_factor_ref         0.1174
_reflns_number_gt                3188
_reflns_number_total             4426
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            ac2011.cif
_cod_data_source_block           I
_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_cell_volume        2150.1(6)
_cod_original_sg_symbol_H-M      'P 21/c'
_cod_database_code               2208777
_cod_database_fobs_code          2208777