<i>tert</i>-Butyl 4-(1-methyl-1<i>H</i>-pyrazol-5-yl)piperidine-1-carboxylate
Richter, Daniel; Kath, John C.; Rheingold, Arnold L.; DiPasquale, Antonio; Yanovsky, Alex; Acta Crystallographica Section E 65 (2009) o870–; doi:10.1107/S1600536809010332

data_2221485
_publ_section_title
;
 <i>tert</i>-Butyl
 4-(1-methyl-1<i>H</i>-pyrazol-5-yl)piperidine-1-carboxylate
;
_journal_coeditor_code           RZ2303
_journal_issue                   4
_journal_name_full               'Acta Crystallographica Section E'
_journal_page_first              o870
_journal_paper_doi               10.1107/S1600536809010332
_journal_volume                  65
_journal_year                    2009
_chemical_formula_iupac          'C14 H23 N3 O2'
_chemical_formula_moiety         'C14 H23 N3 O2'
_chemical_formula_sum            'C14 H23 N3 O2'
_chemical_formula_weight         265.35
_chemical_name_common            0110422-0159-002
_chemical_name_systematic
;
<i>tert</i>-Butyl 4-(1-methyl-1<i>H</i>-pyrazol-5-yl)piperidine-1-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                 100.224(3)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   11.356(3)
_cell_length_b                   11.735(3)
_cell_length_c                   11.245(2)
_cell_measurement_reflns_used    4631
_cell_measurement_temperature    198(2)
_cell_measurement_theta_max      26.9
_cell_measurement_theta_min      2.5
_cell_volume                     1474.7(6)
_computing_cell_refinement       'SAINT (Bruker, 1997)'
_computing_data_collection       'SMART (Bruker, 1997)'
_computing_data_reduction        'SAINT (Bruker, 1997)'
_computing_molecular_graphics    'ORTEP-32 (Farrugia, 1997)'
_computing_publication_material  'WinGX (Farrugia, 1999)'
_computing_structure_refinement  'SHELXL97 (Sheldrick, 2008)'
_computing_structure_solution    'SIR2004 (Burla <i>et al.</i>,  2005)'
_diffrn_ambient_temperature      198(2)
_diffrn_measured_fraction_theta_full 0.995
_diffrn_measured_fraction_theta_max 0.894
_diffrn_measurement_device_type  'Siemens P4 APEX 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  0.063
_diffrn_reflns_av_sigmaI/netI    0.052
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       5
_diffrn_reflns_limit_l_min       -13
_diffrn_reflns_number            14589
_diffrn_reflns_theta_full        25.0
_diffrn_reflns_theta_max         28.2
_diffrn_reflns_theta_min         1.8
_exptl_absorpt_coefficient_mu    0.081
_exptl_absorpt_correction_T_max  0.995
_exptl_absorpt_correction_T_min  0.990
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   '(SADABS; Bruker, 2001)'
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.195
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             576
_exptl_crystal_size_max          0.12
_exptl_crystal_size_mid          0.12
_exptl_crystal_size_min          0.06
_refine_diff_density_max         0.28
_refine_diff_density_min         -0.17
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.03
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     176
_refine_ls_number_reflns         3253
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.03
_refine_ls_R_factor_all          0.085
_refine_ls_R_factor_gt           0.055
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_max_lt       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^)+(0.0866P)^2^+0.0739P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.143
_refine_ls_wR_factor_ref         0.162
_reflns_number_gt                2157
_reflns_number_total             3253
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            rz2303.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        1474.8(6)
_cod_original_sg_symbol_H-M      'P 21/c'
_cod_database_code               2221485
_cod_database_fobs_code          2221485