Carbon dioxide reduction by an Al-O-P frustrated Lewis pair.
Wickemeyer, Lucas; Aders, Niklas; Mix, Andreas; Neumann, Beate; Stammler, Hans-Georg; Cabrera-Trujillo, Jorge J; Fernández, Israel; Mitzel, Norbert W.; Chemical science 13 (2022) 8088–8094; doi:10.1039/d2sc01870e

data_1567186
_publ_section_title
;
 Carbon dioxide reduction by an Al-O-P frustrated Lewis pair.
;
_journal_issue                   27
_journal_name_full               'Chemical science'
_journal_page_first              8088
_journal_page_last               8094
_journal_paper_doi               10.1039/d2sc01870e
_journal_volume                  13
_journal_year                    2022
_chemical_formula_moiety         'C30 H78 Al2 O4 Si8'
_chemical_formula_sum            'C30 H78 Al2 O4 Si8'
_chemical_formula_weight         781.60
_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     dual
_audit_creation_date             2021-05-06
_audit_creation_method
;
Olex2 1.3-ac4
(compiled 2019.04.23 svn.r3594 for Rigaku Oxford Diffraction, GUI svn.r5739)
;
_audit_update_record
;
2022-02-14 deposited with the CCDC.	2022-06-02 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 104.662(3)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   14.9120(3)
_cell_length_b                   9.33098(17)
_cell_length_c                   17.8266(5)
_cell_measurement_reflns_used    32985
_cell_measurement_temperature    100.01(10)
_cell_measurement_theta_max      76.4670
_cell_measurement_theta_min      4.9970
_cell_volume                     2399.68(10)
_computing_cell_refinement       'CrysAlisPro 1.171.41.104a (Rigaku OD, 2021)'
_computing_data_collection       'CrysAlisPro 1.171.41.104a (Rigaku OD, 2021)'
_computing_data_reduction        'CrysAlisPro 1.171.41.104a (Rigaku OD, 2021)'
_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    'ShelXT (Sheldrick, 2015)'
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      100.01(10)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 5.3114
_diffrn_detector_type            Atlas
_diffrn_measured_fraction_theta_full 0.995
_diffrn_measured_fraction_theta_max 0.981
_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    -64.00  30.00   1.00    1.00    --  -38.50  57.00  90.00   94
  2  \w    -59.00  33.00   1.00    1.00    --  -38.50  37.00   0.00   92
  3  \w    -72.00  39.00   1.00    1.00    --  -38.50  19.00 -90.00  111
  4  \w    -59.00  33.00   1.00    1.00    --  -38.50  37.00 150.00   92
  5  \w     13.00  42.00   1.00    1.00    --   42.70  77.00-100.96   29
  6  \w     18.00 111.00   1.00    1.00    --   42.70  57.00 120.00   93
  7  \w     22.00 114.00   1.00    1.00    --   42.70  37.00 -30.00   92
  8  \w     12.00  42.00   1.00    1.00    --   42.70  79.00  32.60   30
  9  \w     18.00 111.00   1.00    1.00    --   42.70  57.00   0.00   93
 10  \w     11.00  42.00   1.00    1.00    --   42.70  82.00 171.10   31
 11  \w     12.00  42.00   1.00    1.00    --   42.70  78.00 -44.90   30
 12  \w     15.00 112.00   1.00    1.00    --   42.70  67.00-139.83   97
 13  \w     18.00 111.00   1.00    1.00    --   42.70  57.00-180.00   93
 14  \w     12.00  42.00   1.00    1.00    --   42.70  79.00  89.74   30
 15  \w     27.00  97.00   1.00    1.00    --   42.70-125.00 -90.00   70
 16  \w     12.00  42.00   1.00    1.00    --   42.70  79.00  60.98   30
 17  \w     84.00 178.00   1.00    3.50    --  111.00  66.00  58.89   94
 18  \w     84.00 178.00   1.00    3.50    --  111.00  66.00   4.60   94
 19  \w     87.00 178.00   1.00    3.50    --  111.00  50.00 154.23   91
 20  \w     87.00 178.00   1.00    3.50    --  111.00  54.00 -73.06   91
 21  \w     37.00 109.00   1.00    3.50    --  111.00-110.00  89.07   72
 22  \w     89.00 178.00   1.00    3.50    --  111.00  45.00 150.00   89
 23  \w     85.00 178.00   1.00    3.50    --  111.00  61.00 150.00   93
 24  \w     31.00 107.00   1.00    3.50    --  111.00 -94.00-150.00   76
 25  \w     43.00 137.00   1.00    3.50    --  111.00 -61.00 -30.00   94
 26  \w     84.00 178.00   1.00    3.50    --  111.00  63.00 109.41   94
 27  \w     50.00 110.00   1.00    3.50    --  111.00-117.00   2.17   60
 28  \w    122.00 176.00   1.00    3.50    --  111.00  68.00  83.82   54
 29  \w     83.00 178.00   1.00    3.50    --  111.00  67.00 -48.85   95
 30  \w     83.00 119.00   1.00    3.50    --  111.00  68.00  83.82   36
 31  \w    123.00 176.00   1.00    3.50    --  111.00  45.00   0.00   53
 32  \w    113.00 178.00   1.00    3.50    --  111.00  59.00 164.62   65
 33  \w     87.00 119.00   1.00    3.50    --  111.00  54.00  50.36   32
 34  \w     85.00 178.00   1.00    3.50    --  111.00  61.00  18.09   93
 35  \w     89.00 118.00   1.00    3.50    --  111.00  45.00   0.00   29
 36  \w     85.00 112.00   1.00    3.50    --  111.00  61.00 120.00   27
 37  \w    126.00 176.00   1.00    3.50    --  111.00  61.00 120.00   50
 38  \w     43.00 136.00   1.00    3.50    --  111.00 -61.00 120.00   93
 39  \w     85.00 111.00   1.00    3.50    --  111.00  61.00   0.00   26
 40  \w     85.00 112.00   1.00    3.50    --  111.00  61.00-120.00   27
 41  \w     85.00 114.00   1.00    3.50    --  111.00  61.00 -30.00   29
 42  \w     89.00 171.00   1.00    3.50    --  111.00  45.00-120.00   82
 43  \w     85.00 177.00   1.00    3.50    --  111.00  61.00 -90.00   92
 44  \w     85.00 111.00   1.00    3.50    --  111.00  61.00-180.00   26
 45  \w     85.00 120.00   1.00    3.50    --  111.00  61.00-150.00   35
 46  \w     85.00 112.00   1.00    3.50    --  111.00  59.00 164.62   27
 47  \w    116.00 141.00   1.00    3.50    --  111.00 -77.00 -90.00   25
 48  \w     85.00 112.00   1.00    3.50    --  111.00  61.00 -60.00   27
 49  \w     37.00  68.00   1.00    3.50    --  111.00 -94.00 -90.00   31
 50  \w     70.00 107.00   1.00    3.50    --  111.00 -94.00 -90.00   37
 51  \w     89.00 117.00   1.00    3.50    --  111.00  45.00  90.00   28
 52  \w     84.00 111.00   1.00    3.50    --  111.00  64.00 -68.27   27
 53  \w    130.00 173.00   1.00    3.50    --  111.00  59.00-161.29   43
 54  \w     86.00 113.00   1.00    3.50    --  111.00  61.00  30.00   27
 55  \w     48.00  84.00   1.00    3.50    --  111.00 -77.00 -90.00   36
 56  \w     84.00 110.00   1.00    3.50    --  111.00  63.00  51.81   26
 57  \w     31.00 107.00   1.00    3.50    --  111.00 -94.00 120.00   76
 58  \w     85.00 123.00   1.00    3.50    --  111.00  59.00-161.29   38
 59  \w     85.00 112.00   1.00    3.50    --  111.00  59.00-100.96   27
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at home/near, Atlas'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      0.0141606000
_diffrn_orient_matrix_UB_12      -0.1624223000
_diffrn_orient_matrix_UB_13      0.0136872000
_diffrn_orient_matrix_UB_21      0.0959333000
_diffrn_orient_matrix_UB_22      0.0113523000
_diffrn_orient_matrix_UB_23      -0.0171990000
_diffrn_orient_matrix_UB_31      0.0445132000
_diffrn_orient_matrix_UB_32      0.0279244000
_diffrn_orient_matrix_UB_33      0.0865570000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Cu K\a'
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0477
_diffrn_reflns_av_unetI/netI     0.0264
_diffrn_reflns_Laue_measured_fraction_full 0.995
_diffrn_reflns_Laue_measured_fraction_max 0.981
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_h_min       -18
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            29223
_diffrn_reflns_point_group_measured_fraction_full 0.995
_diffrn_reflns_point_group_measured_fraction_max 0.981
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         76.809
_diffrn_reflns_theta_min         5.873
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    2.681
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.443
_exptl_absorpt_correction_type   gaussian
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.41.104a (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_colour_lustre     clear
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.082
_exptl_crystal_description       plate
_exptl_crystal_F_000             856
_exptl_crystal_size_max          0.395
_exptl_crystal_size_mid          0.215
_exptl_crystal_size_min          0.069
_refine_diff_density_max         0.380
_refine_diff_density_min         -0.389
_refine_diff_density_rms         0.063
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.058
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     211
_refine_ls_number_reflns         4967
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.058
_refine_ls_R_factor_all          0.0346
_refine_ls_R_factor_gt           0.0337
_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^)+(0.0581P)^2^+0.8601P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0915
_refine_ls_wR_factor_ref         0.0940
_reflns_Friedel_coverage         0.000
_reflns_number_gt                4818
_reflns_number_total             4967
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d2sc01870e2.cif
_cod_data_source_block           compound7d
_cod_depositor_comments
'Adding full bibliography for 1567184--1567187.cif.'
_cod_original_cell_volume        2399.69(10)
_cod_database_code               1567186
_shelx_shelxl_version_number     2018/3
_chemical_oxdiff_formula         'C30 H78 Al2 O4 Si8'
_reflns_odcompleteness_completeness 99.48
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     71.98
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2.a Ternary CH refined with riding coordinates:
 C1(H1), C8(H8)
2.b Aromatic/amide H refined with riding coordinates:
 C15(H15)
2.c Idealised Me refined as rotating group:
 C2(H2A,H2B,H2C), C3(H3A,H3B,H3C), C4(H4A,H4B,H4C), C5(H5A,H5B,H5C), C6(H6A,
 H6B,H6C), C7(H7A,H7B,H7C), C9(H9A,H9B,H9C), C10(H10A,H10B,H10C), C11(H11A,H11B,
 H11C), C12(H12A,H12B,H12C), C13(H13A,H13B,H13C), C14(H14A,H14B,H14C)
;
_shelx_res_checksum              21571
_shelx_hkl_checksum              18186
_olex2_date_sample_data_collection 2021-05-06
_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
- Detector area scaling
;
_oxdiff_exptl_absorpt_empirical_full_max 1.429
_oxdiff_exptl_absorpt_empirical_full_min 0.750