Crystal structure of 2-(2,6-diisopropylphenyl)-<i>N</i>,<i>N</i>-diethyl-3,3-dimethyl-2-azaspiro[4.5]decan-1-amine: a diethylamine adduct of a cyclic(alkyl)(amino)carbene (CAAC)
Naumann, Roxanne A.; Ziller, Joseph W.; Liberman-Martin, Allegra L.; Acta Crystallographica Section E 77 (2021) –; doi:10.1107/S2056989021007854

data_2243885
_publ_section_title
;
 Crystal structure of
 2-(2,6-diisopropylphenyl)-<i>N</i>,<i>N</i>-diethyl-3,3-dimethyl-2-azaspiro[4.5]decan-1-amine:
 a diethylamine adduct of a cyclic(alkyl)(amino)carbene (CAAC)
;
_journal_coeditor_code           ZL5021
_journal_issue                   9
_journal_name_full               'Acta Crystallographica Section E'
_journal_page_first
;
;
_journal_paper_doi               10.1107/S2056989021007854
_journal_volume                  77
_journal_year                    2021
_chemical_formula_iupac          'C27 H46 N2'
_chemical_formula_moiety         'C27 H46 N2'
_chemical_formula_sum            'C27 H46 N2'
_chemical_formula_weight         398.66
_chemical_name_systematic
2-(2,6-Diisopropylbenzene)-<i>N</i>,<i>N</i>-diethyl-3,3-dimethyl-2-azaspiro[4.5]decan-1-amine
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2yn'
_space_group_name_H-M_alt        'P 1 21/n 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-2014/7
_cell_angle_alpha                90
_cell_angle_beta                 96.4589(16)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   12.3319(11)
_cell_length_b                   14.4082(13)
_cell_length_c                   13.6155(12)
_cell_measurement_reflns_used    9991
_cell_measurement_temperature    93(2)
_cell_measurement_theta_max      30.48
_cell_measurement_theta_min      2.18
_cell_volume                     2403.9(4)
_computing_cell_refinement
;
SAINT (Bruker, 2014)
;
_computing_data_collection
;
APEX2 (Bruker, 2014)
;
_computing_data_reduction
;
SAINT (Bruker, 2014)
;
_computing_molecular_graphics
;
SHELXTL (Sheldrick, 2008)
;
_computing_publication_material
;
SHELXTL (Sheldrick, 2008)
;
_computing_structure_refinement
;
<i>SHELXL2014/7</i> (Sheldrick, 2015b)
;
_computing_structure_solution
;
<i>SHELXT2014/4</i> (Sheldrick, 2015a)
;
_diffrn_ambient_temperature      93(2)
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 1.000
_diffrn_measurement_device_type  'Bruker SMART APEXII CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0690
_diffrn_reflns_av_unetI/netI     0.0425
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            57200
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         29.575
_diffrn_reflns_theta_min         2.065
_diffrn_source                   'fine-focus sealed tube'
_exptl_absorpt_coefficient_mu    0.063
_exptl_absorpt_correction_T_max  0.8622
_exptl_absorpt_correction_T_min  0.8228
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
(SADABS; Bruker, 2014)
;
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.102
_exptl_crystal_density_method    not_measured
_exptl_crystal_description       irregular
_exptl_crystal_F_000             888
_exptl_crystal_size_max          0.250
_exptl_crystal_size_mid          0.248
_exptl_crystal_size_min          0.191
_refine_diff_density_max         0.381
_refine_diff_density_min         -0.250
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.018
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     270
_refine_ls_number_reflns         6744
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.018
_refine_ls_R_factor_all          0.0721
_refine_ls_R_factor_gt           0.0482
_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^)+(0.0481P)^2^+1.1815P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1058
_refine_ls_wR_factor_ref         0.1207
_reflns_number_gt                5087
_reflns_number_total             6744
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            zl5021sup1.cif
_cod_data_source_block           I
_cod_original_sg_symbol_H-M      'P 21/n'
_cod_database_code               2243885
_shelx_estimated_absorpt_t_min   0.984
_shelx_estimated_absorpt_t_max   0.988
_shelx_hkl_checksum              5672
_shelx_res_checksum              78439
_cod_database_fobs_code 2243885