Coinage metal aluminyl complexes: probing regiochemistry and mechanism in the insertion and reduction of carbon dioxide
Aldridge, Simon; McManus, Caitilín; Hicks, Jamie; Goicoechea, Jose M.; Cui, Xianlu; Zhao, Lili; Frenking, Gernot; Chemical Science  (2021) –; doi:10.1039/D1SC04676D

data_1564717
_publ_section_title
;
 Coinage metal aluminyl complexes: probing regiochemistry and mechanism in
 the insertion and reduction of carbon dioxide
;
_journal_name_full               'Chemical Science'
_journal_paper_doi               10.1039/D1SC04676D
_journal_year                    2021
_chemical_formula_moiety         'C66 H103 Ag Al N4 O2 P'
_chemical_formula_sum            'C66 H103 Ag Al N4 O2 P'
_chemical_formula_weight         1150.34
_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   geom
_atom_sites_solution_primary     dual
_audit_creation_date             2021-02-07
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_audit_update_record
;
2021-05-24 deposited with the CCDC.	2021-09-16 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 102.038(5)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   14.3910(8)
_cell_length_b                   19.5868(6)
_cell_length_c                   26.9617(9)
_cell_measurement_reflns_used    11593
_cell_measurement_temperature    150.01(10)
_cell_measurement_theta_max      75.2330
_cell_measurement_theta_min      4.0020
_cell_volume                     7432.7(6)
_computing_cell_refinement       'CrysAlisPro 1.171.39.46 (Rigaku OD, 2018)'
_computing_data_collection       'CrysAlisPro 1.171.39.46 (Rigaku OD, 2018)'
_computing_data_reduction        'CrysAlisPro 1.171.39.46 (Rigaku OD, 2018)'
_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      150.01(10)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 10.5035
_diffrn_detector_type            Atlas
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.985
_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   -114.00 -28.00   1.00   15.00    --  -41.40 -37.00   0.00   86
  2  \w      2.00  33.00   1.00   15.00    --  -41.40  19.00-180.00   31
  3  \w    -44.00  11.00   1.00   15.00    --  -41.40  57.00 -60.00   55
  4  \w      1.00  36.00   1.00   15.00    --  -41.40  19.00 150.00   35
  5  \w     35.00  89.00   1.00   15.00    --   41.40-125.00-180.00   54
  6  \w     66.00 115.00   1.00   60.00    --  111.00  15.00 -30.00   49
  7  \w     55.00 109.00   1.00   60.00    --  111.00-111.00  90.00   54
  8  \w     40.00  70.00   1.00   60.00    --  111.00 -45.00-150.00   30
  9  \w    111.00 146.00   1.00   60.00    --  111.00 111.00 150.00   35
 10  \w     37.00 109.00   1.00   60.00    --  111.00-111.00-180.00   72
 11  \w     57.00  86.00   1.00   60.00    --  111.00 -61.00  60.00   29
 12  \w     42.00  71.00   1.00   60.00    --  111.00 -45.00-180.00   29
 13  \w     89.00 178.00   1.00   60.00    --  111.00  30.00  30.00   89
 14  \w    148.00 175.00   1.00   60.00    --  111.00  15.00 -30.00   27
 15  \w     39.00  64.00   1.00   60.00    --  111.00 -94.00  90.00   25
 16  \w     36.00  84.00   1.00   60.00    --  111.00 -94.00 -30.00   48
 17  \w     71.00 108.00   1.00   60.00    --  111.00-111.00  60.00   37
 18  \w     74.00 107.00   1.00   60.00    --  111.00 -94.00  90.00   33
 19  \w    129.00 170.00   1.00   60.00    --  111.00  77.00-180.00   41
 20  \w     87.00 170.00   1.00   60.00    --  111.00  45.00 -60.00   83
 21  \w     43.00  71.00   1.00   60.00    --  111.00 -45.00  60.00   28
 22  \w     54.00  91.00   1.00   60.00    --  111.00 -61.00 150.00   37
;
_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      0.1057592000
_diffrn_orient_matrix_UB_12      0.0039380000
_diffrn_orient_matrix_UB_13      -0.0025939000
_diffrn_orient_matrix_UB_21      -0.0280530000
_diffrn_orient_matrix_UB_22      0.0081699000
_diffrn_orient_matrix_UB_23      -0.0580214000
_diffrn_orient_matrix_UB_31      -0.0023523000
_diffrn_orient_matrix_UB_32      0.0781712000
_diffrn_orient_matrix_UB_33      0.0062179000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0510
_diffrn_reflns_av_unetI/netI     0.0508
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.985
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       24
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       32
_diffrn_reflns_limit_l_min       -33
_diffrn_reflns_number            44027
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.985
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         76.146
_diffrn_reflns_theta_min         3.867
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    2.777
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.70561
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.39.46 (Rigaku Oxford Diffraction, 2018)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            colourless
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.028
_exptl_crystal_description       plate
_exptl_crystal_F_000             2472
_exptl_crystal_size_max          0.2
_exptl_crystal_size_mid          0.1
_exptl_crystal_size_min          0.05
_refine_diff_density_max         0.868
_refine_diff_density_min         -2.430
_refine_diff_density_rms         0.103
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.028
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     705
_refine_ls_number_reflns         15310
_refine_ls_number_restraints     18
_refine_ls_restrained_S_all      1.030
_refine_ls_R_factor_all          0.1053
_refine_ls_R_factor_gt           0.0920
_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^)+(0.1557P)^2^+15.7728P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2628
_refine_ls_wR_factor_ref         0.2760
_reflns_Friedel_coverage         0.000
_reflns_number_gt                12164
_reflns_number_total             15310
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d1sc04676d2.cif
_cod_data_source_block           7-Ag
_cod_original_cell_volume        7432.7(5)
_cod_database_code               1564717
_publcif_datablock.id            {7ebd7094-9205-45bf-ae11-f6ffff973fb5}
_shelx_shelxl_version_number     2018/3
_chemical_oxdiff_formula         'C50 H60 Al1 Ag1 P1 N4 O2'
_shelx_estimated_absorpt_t_max   0.874
_shelx_estimated_absorpt_t_min   0.607
_reflns_odcompleteness_completeness 99.59
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     74.33
_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. Uiso/Uaniso restraints and constraints
C19 \\sim C18 \\sim C16 \\sim C17: within 2A with sigma of 0.005 and sigma for
terminal atoms of 0.01
3.a Ternary CH refined with riding coordinates:
 C45(H45), C52(H52), C49(H49), C30(H30), C33(H33), C42(H42)
3.b Aromatic/amide H refined with riding coordinates:
 C5(H5), C39(H39), C3(H3), C13(H13), C11(H11), C41(H41), C40(H40), C28(H28),
 C27(H27), C26(H26)
3.c Idealised Me refined as rotating group:
 C50(H50A,H50B,H50C), C9(H9A,H9B,H9C), C8(H8A,H8B,H8C), C48(H48A,H48B,H48C),
 C21(H21A,H21B,H21C), C46(H46A,H46B,H46C), C54(H54A,H54B,H54C), C31(H31A,H31B,
 H31C), C66(H66A,H66B,H66C), C47(H47A,H47B,H47C), C53(H53A,H53B,H53C), C32(H32A,
 H32B,H32C), C62(H62A,H62B,H62C), C58(H58A,H58B,H58C), C57(H57A,H57B,H57C),
 C60(H60A,H60B,H60C), C64(H64A,H64B,H64C), C61(H61A,H61B,H61C), C22(H22A,H22B,
 H22C), C65(H65A,H65B,H65C), C23(H23A,H23B,H23C), C35(H35A,H35B,H35C), C34(H34A,
 H34B,H34C), C56(H56A,H56B,H56C), C44(H44A,H44B,H44C), C43(H43A,H43B,H43C),
 C17(H17A,H17B,H17C), C19(H19A,H19B,H19C), C18(H18A,H18B,H18C)
;
_shelx_res_checksum              35277
_shelx_hkl_checksum              93343
_shelx_fab_checksum              99421
_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 1.690
_oxdiff_exptl_absorpt_empirical_full_min 0.660
_publcif_funding_html
;
;