Reversible CO2 fixation by N-heterocyclic imines forming water-stable zwitterionic nitrogen-base‒CO2 adducts
Wilm, Lukas F. B.; Eder, Tobias; Mück-Lichtenfeld, Christian; Mehlmann, Paul; Wünsche, Marius; Buß, Florenz; Dielmann, Fabian; Green Chemistry 21 (2019) 640–; doi:10.1039/C8GC02952K

data_7232141
_publ_section_title
;
 Reversible CO2 fixation by N-heterocyclic imines forming water-stable
 zwitterionic nitrogen-base--CO2 adducts
;
_journal_issue                   3
_journal_name_full               'Green Chemistry'
_journal_page_first              640
_journal_paper_doi               10.1039/C8GC02952K
_journal_volume                  21
_journal_year                    2019
_chemical_formula_moiety         'C16 H29 N3 O2'
_chemical_formula_sum            'C16 H29 N3 O2'
_chemical_formula_weight         295.42
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2ybc'
_space_group_name_H-M_alt        'P 1 21/c 1'
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/c 1'
_atom_sites_solution_hydrogens   geom
_audit_creation_date             2018-07-23
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_audit_update_record
;
2018-09-05 deposited with the CCDC.
2019-01-10 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 104.5879(6)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   14.3302(2)
_cell_length_b                   9.21940(10)
_cell_length_c                   12.9756(2)
_cell_measurement_reflns_used    9922
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      29.59
_cell_measurement_theta_min      2.65
_cell_volume                     1659.02(4)
_computing_cell_refinement       'Bruker SAINT'
_computing_data_collection       'Bruker APEX2'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_diffrn_ambient_temperature      100.0
_diffrn_measured_fraction_theta_full 0.996
_diffrn_measured_fraction_theta_max 0.997
_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  0.0183
_diffrn_reflns_av_unetI/netI     0.0120
_diffrn_reflns_Laue_measured_fraction_full 0.996
_diffrn_reflns_Laue_measured_fraction_max 0.997
_diffrn_reflns_limit_h_max       19
_diffrn_reflns_limit_h_min       -19
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            27688
_diffrn_reflns_point_group_measured_fraction_full 0.996
_diffrn_reflns_point_group_measured_fraction_max 0.997
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         29.585
_diffrn_reflns_theta_min         2.653
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.079
_exptl_absorpt_correction_T_max  1.0000
_exptl_absorpt_correction_T_min  0.9393
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2012/1 (Bruker,2012) was used for absorption correction.
wR2(int) was 0.1236 before and 0.0274 after correction.
The Ratio of minimum to maximum transmission is 0.9393.
The \l/2 correction factor is Not present.
;
_exptl_crystal_colour            colourless
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.183
_exptl_crystal_description       plate
_exptl_crystal_F_000             648
_exptl_crystal_size_max          0.58
_exptl_crystal_size_mid          0.49
_exptl_crystal_size_min          0.2
_refine_diff_density_max         0.386
_refine_diff_density_min         -0.200
_refine_diff_density_rms         0.044
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.057
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     199
_refine_ls_number_reflns         4642
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.057
_refine_ls_R_factor_all          0.0387
_refine_ls_R_factor_gt           0.0368
_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^)+(0.0514P)^2^+0.6113P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1011
_refine_ls_wR_factor_ref         0.1027
_reflns_Friedel_coverage         0.000
_reflns_number_gt                4346
_reflns_number_total             4642
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c8gc02952k2.cif
_cod_data_source_block           p21c_CCDC1
_cod_depositor_comments
'Adding full bibliography for 7232134--7232146.cif.'
_cod_database_code               7232141
_shelxl_version_number           2013-4
_olex2_refinement_description
;
1. Others
 Fixed Uiso: H5A(0.031) H5B(0.031) H5C(0.031) H6A(0.027) H6B(0.027) H6C(0.027)
 H11(0.017) H13A(0.03) H13B(0.03) H13C(0.03) H12A(0.036) H12B(0.036)
 H12C(0.036) H14(0.015) H15A(0.023) H15B(0.023) H15C(0.023) H16A(0.03)
 H16B(0.03) H16C(0.03) H8A(0.033) H8B(0.033) H8C(0.033) H10A(0.031) H10B(0.031)
 H10C(0.031) H9A(0.036) H9B(0.036) H9C(0.036)
 Fixed X: H5A(0.6949) H5B(0.6466) H5C(0.7614) H6A(0.5829) H6B(0.5631)
 H6C(0.5007) H11(0.8517) H13A(0.7517) H13B(0.8167) H13C(0.7155) H12A(0.9283)
 H12B(0.957) H12C(0.881) H14(0.6445) H15A(0.5186) H15B(0.4758) H15C(0.4692)
 H16A(0.5455) H16B(0.5874) H16C(0.6594) H8A(0.8889) H8B(0.7767) H8C(0.8203)
 H10A(0.8854) H10B(0.8151) H10C(0.928) H9A(0.9625) H9B(1) H9C(0.9347)
 Fixed Y: H5A(1.2494) H5B(1.1329) H5C(1.1393) H6A(0.77) H6B(0.931) H6C(0.8671)
 H11(1.1318) H13A(1.3493) H13B(1.3737) H13C(1.2913) H12A(1.0792) H12B(1.2333)
 H12C(1.2245) H14(0.7172) H15A(0.8835) H15B(0.7225) H15C(0.8269) H16A(0.616)
 H16B(0.5223) H16C(0.5921) H8A(0.6205) H8B(0.6304) H8C(0.7305) H10A(0.808)
 H10B(0.6777) H10C(0.6674) H9A(0.9583) H9B(0.8191) H9C(0.9378)
 Fixed Z: H5A(0.3323) H5B(0.2434) H5C(0.2872) H6A(0.2745) H6B(0.228)
 H6C(0.3039) H11(0.6198) H13A(0.4789) H13B(0.5974) H13C(0.5784) H12A(0.4791)
 H12B(0.5349) H12C(0.4211) H14(0.5962) H15A(0.5807) H15B(0.563) H15C(0.463)
 H16A(0.3916) H16B(0.4969) H16C(0.4342) H8A(0.7809) H8B(0.7215) H8C(0.823)
 H10A(0.538) H10B(0.55) H10C(0.6059) H9A(0.6941) H9B(0.7665) H9C(0.8052)
;
_shelx_res_checksum              54067
_olex2_submission_special_instructions 'No special instructions were received'