Crystal structure of <i>tert</i>-butyl 4-[4-(4-fluorophenyl)-2-methylbut-3-yn-2-yl]piperazine-1-carboxylate
Gumireddy, Ashwini; DeBoyace, Kevin; Rupprecht, Alexander; Gupta, Mohit; Patel, Saloni; Flaherty, Patrick T.; Wildfong, Peter L. D.; Acta Crystallographica Section E 77 (2021) 360–365; doi:10.1107/S2056989021002346

data_2243773
_publ_section_title
;
 Crystal structure of <i>tert</i>-butyl
 4-[4-(4-fluorophenyl)-2-methylbut-3-yn-2-yl]piperazine-1-carboxylate
;
_journal_coeditor_code           ZL5007
_journal_issue                   4
_journal_name_full               'Acta Crystallographica Section E'
_journal_page_first              360
_journal_page_last               365
_journal_paper_doi               10.1107/S2056989021002346
_journal_volume                  77
_journal_year                    2021
_chemical_absolute_configuration rm
_chemical_formula_iupac          'C20 H27 F N2 O2'
_chemical_formula_moiety         'C20 H27 F N2 O2'
_chemical_formula_sum            'C20 H27 F N2 O2'
_chemical_formula_weight         346.43
_chemical_name_systematic
;
<i>tert</i>-Butyl
4-[4-(4-fluorophenyl)-2-methylbut-3-yn-2-yl]piperazine-1-carboxylate
;
_space_group_crystal_system      monoclinic
_space_group_IT_number           4
_space_group_name_Hall           'P 2yb'
_space_group_name_H-M_alt        'P 1 21 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-2018/3
_cell_angle_alpha                90
_cell_angle_beta                 104.691(2)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   10.2576(11)
_cell_length_b                   9.5127(10)
_cell_length_c                   10.5318(11)
_cell_measurement_reflns_used    3739
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      23.907
_cell_measurement_theta_min      2.929
_cell_volume                     994.07(18)
_computing_cell_refinement
;
SMART and SAINT (Bruker, 1998)
;
_computing_data_collection
;
SMART and SAINT (Bruker, 1998)
;
_computing_data_reduction
;
SMART and SAINT (Bruker, 1998)
;
_computing_molecular_graphics
;
CrystalMaker (Palmer, 2014)
;
_computing_publication_material
;
<i>SHELXL2018/3</i> (Sheldrick, 2015)
;
_computing_structure_refinement
;
<i>SHELXL2018/3</i> (Sheldrick, 2015)
;
_computing_structure_solution
;
SHELXS97 (Sheldrick, 2008)
;
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device_type  'Bruker SMART APEXII'
_diffrn_measurement_method       '\f and \w Scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0171
_diffrn_reflns_av_unetI/netI     0.0246
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       14
_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_number            10640
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         28.688
_diffrn_reflns_theta_min         1.999
_exptl_absorpt_coefficient_mu    0.081
_exptl_absorpt_correction_T_max  0.7457
_exptl_absorpt_correction_T_min  0.7041
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
(SADABS; Sheldrick, 2002)
;
_exptl_crystal_colour            Colorless
_exptl_crystal_density_diffrn    1.157
_exptl_crystal_description       Plate
_exptl_crystal_F_000             372
_exptl_crystal_size_max          0.650
_exptl_crystal_size_mid          0.500
_exptl_crystal_size_min          0.165
_refine_diff_density_max         0.117
_refine_diff_density_min         -0.113
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.040
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     231
_refine_ls_number_reflns         5058
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.040
_refine_ls_R_factor_all          0.0577
_refine_ls_R_factor_gt           0.0395
_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^)+(0.0543P)^2^+0.0286P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0975
_refine_ls_wR_factor_ref         0.1088
_reflns_number_gt                3662
_reflns_number_total             5058
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            zl5007sup1.cif
_cod_data_source_block           I
_cod_original_sg_symbol_H-M      'P 21'
_cod_database_code               2243773
_cod_database_fobs_code          2243773
_shelx_estimated_absorpt_t_min   0.949
_shelx_estimated_absorpt_t_max   0.987
_shelx_hkl_checksum              96633
_shelx_res_checksum              14960