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_7232144
_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         'C8 H13 N3 O2'
_chemical_formula_sum            'C8 H13 N3 O2'
_chemical_formula_weight         183.21
_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   mixed
_atom_sites_solution_primary     iterative
_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                 104.1304(18)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   6.6679(3)
_cell_length_b                   14.6889(5)
_cell_length_c                   9.6025(4)
_cell_measurement_reflns_used    9981
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      30.507
_cell_measurement_theta_min      3.442
_cell_volume                     912.05(6)
_computing_cell_refinement       'SAINT v8.37A (Bruker, 2015)'
_computing_data_collection       'Bruker APEX2'
_computing_data_reduction        'SAINT v8.37A (Bruker, 2015)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_computing_structure_solution
;
Superflip (Palatinus & Chapuis, 2007;Palatinus & van der Lee, 2008;
Palatinus et al., 2012)
;
_diffrn_ambient_temperature      100.01
_diffrn_measured_fraction_theta_full 0.995
_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  0.0247
_diffrn_reflns_av_unetI/netI     0.0139
_diffrn_reflns_Laue_measured_fraction_full 0.995
_diffrn_reflns_Laue_measured_fraction_max 0.997
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_h_min       -8
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_l_max       13
_diffrn_reflns_limit_l_min       -13
_diffrn_reflns_number            20261
_diffrn_reflns_point_group_measured_fraction_full 0.995
_diffrn_reflns_point_group_measured_fraction_max 0.997
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         30.514
_diffrn_reflns_theta_min         3.533
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.098
_exptl_absorpt_correction_T_max  1.0000
_exptl_absorpt_correction_T_min  0.9156
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2016/2 (Bruker,2016/2) was used for absorption correction.
wR2(int) was 0.0709 before and 0.0385 after correction.
The Ratio of minimum to maximum transmission is 0.9156.
The \l/2 correction factor is 0.00150.
;
_exptl_crystal_colour            colourless
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.334
_exptl_crystal_description       block
_exptl_crystal_F_000             392
_exptl_crystal_size_max          0.12
_exptl_crystal_size_mid          0.11
_exptl_crystal_size_min          0.08
_refine_diff_density_max         0.406
_refine_diff_density_min         -0.345
_refine_diff_density_rms         0.055
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.052
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     126
_refine_ls_number_reflns         2785
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.052
_refine_ls_R_factor_all          0.0416
_refine_ls_R_factor_gt           0.0391
_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^)+(0.0589P)^2^+0.3913P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1085
_refine_ls_wR_factor_ref         0.1110
_reflns_Friedel_coverage         0.000
_reflns_number_gt                2583
_reflns_number_total             2785
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c8gc02952k2.cif
_cod_data_source_block           p21c_CCDC2
_cod_depositor_comments
'Adding full bibliography for 7232134--7232146.cif.'
_cod_database_code               7232144
_shelxl_version_number           2013-4
_olex2_refinement_description
;
1. Others
 Fixed Uiso: H5A(0.021) H5B(0.021) H5C(0.021) H6A(0.027) H6B(0.027) H6C(0.027)
 H7A(0.027) H7B(0.027) H7C(0.027) H8A(0.029) H8B(0.029) H8C(0.029)
 Fixed X: H5A(0.5068) H5B(0.557) H5C(0.4444) H6A(0.1304) H6B(-0.0418)
 H6C(0.1981) H7A(-0.2911) H7B(-0.3027) H7C(-0.3793) H8A(-0.1728) H8B(-0.0065)
 H8C(-0.2052)
 Fixed Y: H5A(0.4742) H5B(0.369) H5C(0.3995) H6A(0.5211) H6B(0.5692)
 H6C(0.5825) H7A(0.4728) H7B(0.5148) H7C(0.4128) H8A(0.2396) H8B(0.2567)
 H8C(0.3211)
 Fixed Z: H5A(0.3526) H5B(0.3339) H5C(0.4558) H6A(0.4382) H6B(0.3146)
 H6C(0.3197) H7A(-0.0319) H7B(0.1197) H7C(0.079) H8A(0.0169) H8B(-0.0756) H8C(-
 0.0969)
;
_shelx_res_checksum              6083
_olex2_submission_special_instructions 'No special instructions were received'