Crystal structure of 2-ethyl-1-tert-butyl 3-oxo-2-[phenyl(tert-butoxycarbonylamino)methyl]-1,2-pyrrolidinedicarboxylate, C24H34N2O7
Makhathini, Sifiso. S.; Samipillai, Marivel; Kruger, Hendrik G.; Govender, Thavendran; Naicker, Tricia; Zeitschrift für Kristallographie - New Crystal Structures 231 (2016) 725–727; doi:10.1515/ncrs-2015-0249

data_8106988
_publ_section_title
;
 Crystal structure of 2-ethyl-1-tert-butyl
 3-oxo-2-[phenyl(tert-butoxycarbonylamino)methyl]-1,2-pyrrolidinedicarboxylate,
 C24H34N2O7
;
_journal_issue                   3
_journal_name_full
'Zeitschrift f\"ur Kristallographie - New Crystal Structures'
_journal_page_first              725
_journal_page_last               727
_journal_paper_doi               10.1515/ncrs-2015-0249
_journal_volume                  231
_journal_year                    2016
_chemical_formula_moiety         'C24 H34 N2 O7'
_chemical_formula_sum            'C24 H34 N2 O7'
_chemical_formula_weight         462.53
_chemical_name_systematic
;   
2-ethyl-1-tert-butyl 3-oxo-2-[phenyl(tert-butoxycarbonylamino)methyl]-1,2-pyrrolidinedicarboxylate
;
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_atom_sites_solution_hydrogens   mixed
_cell_angle_alpha                95.143(4)
_cell_angle_beta                 109.970(3)
_cell_angle_gamma                112.229(4)
_cell_formula_units_Z            2
_cell_length_a                   9.9562(8)
_cell_length_b                   10.7465(9)
_cell_length_c                   13.7925(11)
_cell_measurement_reflns_used    9917
_cell_measurement_temperature    173(2)
_cell_measurement_theta_max      28.46
_cell_measurement_theta_min      2.42
_cell_volume                     1242.62(19)
_computing_cell_refinement       'SAINT-plus (Bruker, 2008)'
_computing_data_collection       'APEX2 (Bruker, 2008)'
_computing_data_reduction        'SAINT-Plus and XPREP (Bruker, 2008)'
_computing_molecular_graphics    'ORTEP3 (Farrugia, 2012)'
_computing_publication_material  'Mercury 3.5.1 (2015)'
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_structure_solution    'SHELXL-2013 (Sheldrick, 2013)'
_diffrn_ambient_temperature      173(2)
_diffrn_measured_fraction_theta_full 0.982
_diffrn_measured_fraction_theta_max 0.962
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0421
_diffrn_reflns_av_unetI/netI     0.0326
_diffrn_reflns_Laue_measured_fraction_full 0.982
_diffrn_reflns_Laue_measured_fraction_max 0.962
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            22730
_diffrn_reflns_point_group_measured_fraction_full 0.982
_diffrn_reflns_point_group_measured_fraction_max 0.962
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         28.552
_diffrn_reflns_theta_min         1.623
_diffrn_source                   'sealed tube'
_exptl_absorpt_coefficient_mu    0.091
_exptl_absorpt_correction_T_max  0.984
_exptl_absorpt_correction_T_min  0.972
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   SADABS
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.236
_exptl_crystal_description       block
_exptl_crystal_F_000             496
_exptl_crystal_size_max          0.320
_exptl_crystal_size_mid          0.240
_exptl_crystal_size_min          0.180
_refine_diff_density_max         0.388
_refine_diff_density_min         -0.219
_refine_diff_density_rms         0.047
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.058
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     309
_refine_ls_number_reflns         6107
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.058
_refine_ls_R_factor_all          0.0548
_refine_ls_R_factor_gt           0.0460
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0602P)^2^+0.4413P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1255
_refine_ls_wR_factor_ref         0.1337
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                5104
_reflns_number_total             6107
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            suppl_ncrs-2015-0249_suppl.cif
_cod_data_source_block           1
_cod_original_cell_volume        1242.62(18)
_cod_original_sg_symbol_H-M      P-1
_cod_database_code               8106988
_shelx_estimated_absorpt_t_min   0.972
_shelx_estimated_absorpt_t_max   0.984
_exptl_absorpt_special_details
;
?
;
_shelx_res_checksum              64282
_shelx_hkl_checksum              90380
_publcif_info_exptl_table_max_cols 4
_publcif_info_exptl_table_use_headnotes n