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_1567187
_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         'C23 H58 Al O3 P Si4'
_chemical_formula_sum            'C23 H58 Al O3 P Si4'
_chemical_formula_weight         553.00
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     dual
_audit_creation_date             2021-04-22
_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                84.6973(8)
_cell_angle_beta                 76.7333(10)
_cell_angle_gamma                75.2570(10)
_cell_formula_units_Z            4
_cell_length_a                   12.51484(16)
_cell_length_b                   16.89311(17)
_cell_length_c                   17.04953(18)
_cell_measurement_reflns_used    86736
_cell_measurement_temperature    100.0(1)
_cell_measurement_theta_max      76.3160
_cell_measurement_theta_min      2.6870
_cell_volume                     3390.60(7)
_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      100.0(1)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 5.3114
_diffrn_detector_type            Atlas
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.989
_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  57.00-180.00   94
  2  \w   -124.00  47.00   1.00    1.00    --  -38.50   0.00  60.00  171
  3  \w    -59.00  33.00   1.00    1.00    --  -38.50  37.00 120.00   92
  4  \w    -59.00  33.00   1.00    1.00    --  -38.50  37.00 -90.00   92
  5  \w     18.00 111.00   1.00    1.00    --   42.70  57.00 150.00   93
  6  \w     11.00  42.00   1.00    1.00    --   42.70  82.00 -70.77   31
  7  \w     15.00 112.00   1.00    1.00    --   42.70  68.00  50.09   97
  8  \w     11.00  42.00   1.00    1.00    --   42.70  82.00-136.85   31
  9  \w     12.00  42.00   1.00    1.00    --   42.70  79.00-158.33   30
 10  \w     18.00 111.00   1.00    1.00    --   42.70  57.00 -30.00   93
 11  \w     12.00  42.00   1.00    1.00    --   42.70  78.00  -1.86   30
 12  \w     22.00 114.00   1.00    1.00    --   42.70  37.00 -90.00   92
 13  \w     11.00  42.00   1.00    1.00    --   42.70  82.00 142.49   31
 14  \w     12.00  42.00   1.00    1.00    --   42.70  79.00  97.27   30
 15  \w     27.00  97.00   1.00    1.00    --   42.70-125.00  30.00   70
 16  \w     87.00 178.00   1.00    1.00    --  111.00  50.00 -94.23   91
 17  \w     85.00 178.00   1.00    1.00    --  111.00  62.00 130.78   93
 18  \w     87.00 178.00   1.00    1.00    --  111.00  53.00  80.66   91
 19  \w     84.00 178.00   1.00    1.00    --  111.00  65.00-104.03   94
 20  \w     85.00 178.00   1.00    1.00    --  111.00  61.00 -55.17   93
 21  \w     89.00 178.00   1.00    1.00    --  111.00  43.00  41.17   89
 22  \w     38.00 109.00   1.00    1.00    --  111.00-111.00  20.64   71
 23  \w     37.00 108.00   1.00    1.00    --  111.00-109.00  50.91   71
 24  \w     85.00 178.00   1.00    1.00    --  111.00  61.00  30.00   93
 25  \w     85.00 178.00   1.00    1.00    --  111.00  61.00 150.00   93
 26  \w     38.00 109.00   1.00    1.00    --  111.00-111.00 173.21   71
 27  \w     41.00 113.00   1.00    1.00    --  111.00-125.00 -30.00   72
 28  \w     31.00 107.00   1.00    1.00    --  111.00 -94.00  90.00   76
 29  \w     37.00 109.00   1.00    1.00    --  111.00-108.00-125.60   72
 30  \w     87.00 178.00   1.00    1.00    --  111.00  54.00 103.67   91
 31  \w     84.00 178.00   1.00    1.00    --  111.00  65.00   3.73   94
 32  \w     86.00 178.00   1.00    1.00    --  111.00  56.00 -79.27   92
 33  \w     85.00 178.00   1.00    1.00    --  111.00  60.00 112.61   93
 34  \w     85.00 178.00   1.00    1.00    --  111.00  61.00-150.00   93
 35  \w     85.00 178.00   1.00    1.00    --  111.00  61.00-120.00   93
 36  \w     84.00 178.00   1.00    1.00    --  111.00  64.00 -44.99   94
 37  \w     43.00 137.00   1.00    1.00    --  111.00 -61.00  60.00   94
 38  \w     85.00 178.00   1.00    1.00    --  111.00  61.00   0.00   93
 39  \w     85.00 178.00   1.00    1.00    --  111.00  61.00 -30.00   93
 40  \w     85.00 178.00   1.00    1.00    --  111.00  61.00 120.00   93
 41  \w     89.00 178.00   1.00    1.00    --  111.00  45.00  60.00   89
 42  \w     85.00 178.00   1.00    1.00    --  111.00  61.00-180.00   93
 43  \w     89.00 178.00   1.00    1.00    --  111.00  45.00-180.00   89
 44  \w     85.00 178.00   1.00    1.00    --  111.00  61.00  60.00   93
 45  \w     85.00 178.00   1.00    1.00    --  111.00  61.00  90.00   93
 46  \w     85.00 178.00   1.00    1.00    --  111.00  62.00-134.16   93
 47  \w     89.00 178.00   1.00    1.00    --  111.00  45.00   0.00   89
 48  \w     43.00 137.00   1.00    1.00    --  111.00 -61.00-150.00   94
 49  \w     82.00 178.00   1.00    1.00    --  111.00  71.00 -81.80   96
 50  \w     86.00 178.00   1.00    1.00    --  111.00  57.00 176.14   92
 51  \w     82.00 178.00   1.00    1.00    --  111.00  71.00-177.85   96
 52  \w     84.00 178.00   1.00    1.00    --  111.00  65.00  76.62   94
 53  \w   -110.00 -18.00   1.00    1.00    --  -38.50 -37.00 120.00   92
 54  \w     18.00 111.00   1.00    1.00    --   42.70  57.00 -60.00   93
 55  \w     27.00  97.00   1.00    1.00    --   42.70-125.00 -60.00   70
 56  \w     12.00  42.00   1.00    1.00    --   42.70  78.00 -30.51   30
 57  \w      9.00 120.00   1.00    1.00    --   42.70  19.00-150.00  111
 58  \w     18.00 111.00   1.00    1.00    --   42.70  57.00-120.00   93
 59  \w     22.00 114.00   1.00    1.00    --   42.70  37.00  30.00   92
 60  \w     22.00 114.00   1.00    1.00    --   42.70  37.00  60.00   92
 61  \w     15.00 112.00   1.00    1.00    --   42.70  67.00 168.77   97
 62  \w     22.00 114.00   1.00    1.00    --   42.70  37.00-180.00   92
 63  \w     22.00 114.00   1.00    1.00    --   42.70  37.00 -60.00   92
 64  \w     22.00 114.00   1.00    1.00    --   42.70  37.00 -30.00   92
 65  \w     12.00  42.00   1.00    1.00    --   42.70  80.00  33.45   30
 66  \w     15.00 112.00   1.00    1.00    --   42.70  67.00  66.03   97
 67  \w    -43.00 128.00   1.00    1.00    --   42.70   0.00-180.00  171
 68  \w     22.00 114.00   1.00    1.00    --   42.70  37.00-150.00   92
 69  \w     85.00 178.00   1.00    1.00    --  111.00  61.00 -60.00   93
;
_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      0.0294392000
_diffrn_orient_matrix_UB_12      0.0628287000
_diffrn_orient_matrix_UB_13      -0.0677414000
_diffrn_orient_matrix_UB_21      -0.0542156000
_diffrn_orient_matrix_UB_22      0.0698362000
_diffrn_orient_matrix_UB_23      0.0593229000
_diffrn_orient_matrix_UB_31      0.1147756000
_diffrn_orient_matrix_UB_32      -0.0089133000
_diffrn_orient_matrix_UB_33      0.0228388000
_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  0.0287
_diffrn_reflns_av_unetI/netI     0.0137
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.989
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       21
_diffrn_reflns_limit_k_min       -21
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            124304
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.989
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         76.486
_diffrn_reflns_theta_min         2.664
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    2.477
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.611
_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    1.083
_exptl_crystal_description       block
_exptl_crystal_F_000             1216
_exptl_crystal_size_max          0.265
_exptl_crystal_size_mid          0.209
_exptl_crystal_size_min          0.166
_refine_diff_density_max         0.359
_refine_diff_density_min         -0.314
_refine_diff_density_rms         0.039
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.033
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     631
_refine_ls_number_reflns         14100
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.033
_refine_ls_R_factor_all          0.0269
_refine_ls_R_factor_gt           0.0255
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0357P)^2^+1.2654P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0686
_refine_ls_wR_factor_ref         0.0696
_reflns_Friedel_coverage         0.000
_reflns_number_gt                13368
_reflns_number_total             14100
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d2sc01870e2.cif
_cod_data_source_block           compound6
_cod_depositor_comments
'Adding full bibliography for 1567184--1567187.cif.'
_cod_database_code               1567187
_shelx_shelxl_version_number     2018/3
_chemical_oxdiff_formula         C23H58AlO3PSi4
_reflns_odcompleteness_completeness 99.81
_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. Others
 Sof(C24)=Sof(H24)=1-FVAR(1)
 Sof(C24B)=Sof(H24B)=FVAR(1)
3.a Ternary CH refined with riding coordinates:
 C2(H2A), C3(H3), C25(H25), C26(H26)
3.b Aromatic/amide H refined with riding coordinates:
 C1(H1A), C24(H24), C24B(H24B)
3.c Idealised Me refined as rotating group:
 C4(H4A,H4B,H4C), C5(H5A,H5B,H5C), C6(H6A,H6B,H6C), C7(H7A,H7B,H7C), C8(H8A,
 H8B,H8C), C9(H9A,H9B,H9C), C10(H10A,H10B,H10C), C11(H11A,H11B,H11C), C12(H12A,
 H12B,H12C), C13(H13A,H13B,H13C), C14(H14A,H14B,H14C), C15(H15A,H15B,H15C),
 C17(H17A,H17B,H17C), C18(H18A,H18B,H18C), C19(H19A,H19B,H19C), C21(H21A,H21B,
 H21C), C22(H22A,H22B,H22C), C23(H23A,H23B,H23C), C27(H27A,H27B,H27C), C28(H28A,
 H28B,H28C), C29(H29A,H29B,H29C), C30(H30A,H30B,H30C), C31(H31A,H31B,H31C),
 C32(H32A,H32B,H32C), C33(H33A,H33B,H33C), C34(H34A,H34B,H34C), C35(H35A,H35B,
 H35C), C36(H36A,H36B,H36C), C37(H37A,H37B,H37C), C38(H38A,H38B,H38C), C40(H40A,
 H40B,H40C), C41(H41A,H41B,H41C), C42(H42A,H42B,H42C), C44(H44A,H44B,H44C),
 C45(H45A,H45B,H45C), C46(H46A,H46B,H46C)
;
_shelx_res_checksum              68958
_shelx_hkl_checksum              52206
_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 1.153
_oxdiff_exptl_absorpt_empirical_full_min 0.883