CO2 capture from ambient air via crystallization with tetraalkylammonium hydroxides
Mishra, Manish Kumar; Smetana, Volodymyr; Hiti, Ethan A.; Wineinger, Hannah B.; Qu, Fengrui; Mudring, Anja-Verena; Rogers, Robin D.; Dalton Transactions  (2022) –; doi:10.1039/D2DT02262A

data_7711720
_publ_section_title
;
 CO2 capture from ambient air via crystallization with tetraalkylammonium
 hydroxides
;
_journal_name_full               'Dalton Transactions'
_journal_paper_doi               10.1039/D2DT02262A
_journal_year                    2022
_chemical_formula_moiety         'C H O3, 0.5(H2 O), C12 H28 N'
_chemical_formula_sum            'C13 H30 N O3.5'
_chemical_formula_weight         256.38
_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'
_atom_sites_solution_hydrogens   mixed
_audit_creation_date             2022-01-13
_audit_creation_method
;
Olex2 1.5-alpha
(compiled 2021.12.21 svn.raa29eb21 for OlexSys, GUI svn.r6440)
;
_audit_update_record
;
2022-05-01 deposited with the CCDC.	2022-10-07 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 103.835(2)
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   15.8432(3)
_cell_length_b                   12.8961(2)
_cell_length_c                   15.5262(3)
_cell_measurement_reflns_used    19816
_cell_measurement_temperature    100.00(10)
_cell_measurement_theta_max      32.5450
_cell_measurement_theta_min      2.0540
_cell_volume                     3080.21(10)
_computing_cell_refinement       'CrysAlisPro 1.171.41.118a (Rigaku OD, 2021)'
_computing_data_collection       'CrysAlisPro 1.171.41.118a (Rigaku OD, 2021)'
_computing_data_reduction        'CrysAlisPro 1.171.41.118a (Rigaku OD, 2021)'
_computing_molecular_graphics    'Olex2 1.5-alpha (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.5-alpha (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2018/3 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT 2014/5 (Sheldrick, 2014)'
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      100.00(10)
_diffrn_detector                 'Hybrid Pixel Array Detector'
_diffrn_detector_area_resol_mean 10.0000
_diffrn_detector_type            HyPix
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.873
_diffrn_measurement_details
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  t~exp~   \w     \q     \k     \f   Frames
  1  \w    -57.00  -9.00   0.50   25.00    --  -12.82 118.00  63.00   96
  2  \w    -80.00 -32.00   0.50   25.00    --  -12.82 159.00-143.00   96
  3  \w    -11.00  84.00   0.50   25.00    --   11.72  77.00-180.00  190
  4  \w     -1.00  85.00   0.50   25.00    --   11.72  37.00-180.00  172
  5  \w     -3.00  74.00   0.50   25.00    --   11.72  57.00 -30.00  154
  6  \w    -85.00 -41.00   0.50   25.00    --  -12.82 178.00 150.00   88
  7  \w     20.00  59.00   0.50   25.00    --  -12.82  37.00   0.00   78
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'XtaLAB Synergy R, DW system, HyPix'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      -0.0124968000
_diffrn_orient_matrix_UB_12      -0.0510932000
_diffrn_orient_matrix_UB_13      -0.0144939000
_diffrn_orient_matrix_UB_21      0.0175957000
_diffrn_orient_matrix_UB_22      -0.0188357000
_diffrn_orient_matrix_UB_23      0.0435332000
_diffrn_orient_matrix_UB_31      -0.0407524000
_diffrn_orient_matrix_UB_32      0.0075595000
_diffrn_orient_matrix_UB_33      0.0104898000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0281
_diffrn_reflns_av_unetI/netI     0.0286
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.873
_diffrn_reflns_limit_h_max       23
_diffrn_reflns_limit_h_min       -21
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_number            48901
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.873
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         33.390
_diffrn_reflns_theta_min         2.061
_diffrn_source                   'Rotating-anode X-ray tube'
_diffrn_source_type              'Rigaku (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    0.078
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.952
_exptl_absorpt_correction_type   gaussian
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.41.118a (Rigaku Oxford Diffraction, 2021)
Numerical absorption correction based on gaussian integration over
a multifaceted crystal model
Empirical absorption correction using spherical harmonics,
implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            'clear colourless'
_exptl_crystal_density_diffrn    1.106
_exptl_crystal_description       irregular
_exptl_crystal_F_000             1144
_exptl_crystal_size_max          0.138
_exptl_crystal_size_mid          0.118
_exptl_crystal_size_min          0.091
_refine_diff_density_max         0.374
_refine_diff_density_min         -0.211
_refine_diff_density_rms         0.040
_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     329
_refine_ls_number_reflns         10451
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.018
_refine_ls_R_factor_all          0.0573
_refine_ls_R_factor_gt           0.0426
_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^)+(0.0503P)^2^+0.6910P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1012
_refine_ls_wR_factor_ref         0.1069
_reflns_Friedel_coverage         0.000
_reflns_number_gt                8473
_reflns_number_total             10451
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d2dt02262a1.cif
_cod_data_source_block           N3333HCO305H2O
_cod_depositor_comments
;

2024-09-24
Z value and formula fixed to values more according to usual
chemical conventions.                 miguel
;
_cod_original_formula_sum            'C26 H60 N2 O7'
_cod_original_formula_weight         512.76
_cod_original_formula_moiety         '2(C H O3), H2 O, 2(C12 H28 N)'
_cod_original_formula_units_Z            4
_cod_database_code               7711720
_shelx_shelxl_version_number     2018/3
_chemical_oxdiff_formula         C26H60N2O7
_shelx_estimated_absorpt_t_max   0.993
_shelx_estimated_absorpt_t_min   0.989
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups, All O(H) groups, All O(H,H) groups
2.a Free rotating group:
 O7(H7C,H7D)
2.b Secondary CH2 refined with riding coordinates:
 C3(H3A,H3B), C4(H4A,H4B), C6(H6A,H6B), C7(H7A,H7B), C9(H9A,H9B), C10(H10A,
 H10B), C12(H12A,H12B), C13(H13A,H13B), C15(H15A,H15B), C16(H16A,H16B),
 C18(H18A,H18B), C19(H19A,H19B), C21(H21A,H21B), C22(H22A,H22B), C24(H24A,H24B),
  C25(H25A,H25B)
2.c Idealised Me refined as rotating group:
 C5(H5A,H5B,H5C), C8(H8A,H8B,H8C), C11(H11A,H11B,H11C), C14(H14A,H14B,H14C),
 C17(H17A,H17B,H17C), C20(H20A,H20B,H20C), C23(H23A,H23B,H23C), C26(H26A,H26B,
 H26C)
2.d Idealised tetrahedral OH refined as rotating group:
 O2(H2), O4(H4)
;
_shelx_res_checksum              97189
_olex2_submission_special_instructions 'No special instructions were received'
_oxdiff_exptl_absorpt_empirical_details
;
Empirical correction (ABSPACK) includes:
- Absorption correction using spherical harmonics
- Frame scaling
;
_oxdiff_exptl_absorpt_empirical_full_max 1.240
_oxdiff_exptl_absorpt_empirical_full_min 0.774