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_1564719
_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         'C59 H89 Ag Ga N2 O P, 2(C7 H8)'
_chemical_formula_sum            'C73 H105 Ag Ga N2 O P'
_chemical_formula_weight         1235.14
_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   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                82.027(3)
_cell_angle_beta                 72.271(3)
_cell_angle_gamma                70.022(4)
_cell_formula_units_Z            2
_cell_length_a                   12.8040(6)
_cell_length_b                   14.3764(5)
_cell_length_c                   20.7258(7)
_cell_measurement_reflns_used    14921
_cell_measurement_temperature    150.03(13)
_cell_measurement_theta_max      30.2760
_cell_measurement_theta_min      3.3530
_cell_volume                     3412.7(3)
_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      150.03(13)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 10.4102
_diffrn_detector_type            Atlas
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.859
_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    -24.00  19.00   1.00   37.50    --  -12.38  77.00 150.00   43
  2  \w    -83.00  13.00   1.00   37.50    --  -12.38 -57.00   0.00   96
  3  \w     23.00  56.00   1.00   37.50    --  -12.38  57.00 150.00   33
  4  \w    -13.00  19.00   1.00   37.50    --  -12.38 -77.00-150.00   32
  5  \w    -36.00  -1.00   1.00   37.50    --  -12.38  57.00 150.00   35
  6  \w    -14.00  83.00   1.00   37.50    --   12.85  57.00 -60.00   97
;
_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      0.0519261000
_diffrn_orient_matrix_UB_12      -0.0198658000
_diffrn_orient_matrix_UB_13      0.0099208000
_diffrn_orient_matrix_UB_21      0.0188440000
_diffrn_orient_matrix_UB_22      0.0398644000
_diffrn_orient_matrix_UB_23      -0.0176561000
_diffrn_orient_matrix_UB_31      -0.0266450000
_diffrn_orient_matrix_UB_32      0.0278609000
_diffrn_orient_matrix_UB_33      0.0297104000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0248
_diffrn_reflns_av_unetI/netI     0.0443
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.859
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_h_min       -18
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -29
_diffrn_reflns_number            33574
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.859
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         30.409
_diffrn_reflns_theta_min         2.972
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    0.747
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.70392
_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    1.202
_exptl_crystal_description       plate
_exptl_crystal_F_000             1316
_exptl_crystal_size_max          0.4
_exptl_crystal_size_mid          0.3
_exptl_crystal_size_min          0.01
_refine_diff_density_max         0.895
_refine_diff_density_min         -0.653
_refine_diff_density_rms         0.068
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.023
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     715
_refine_ls_number_reflns         17762
_refine_ls_number_restraints     214
_refine_ls_restrained_S_all      1.044
_refine_ls_R_factor_all          0.0586
_refine_ls_R_factor_gt           0.0407
_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^)+(0.0341P)^2^+2.8890P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0904
_refine_ls_wR_factor_ref         0.1005
_reflns_Friedel_coverage         0.000
_reflns_number_gt                13962
_reflns_number_total             17762
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d1sc04676d2.cif
_cod_data_source_block           3'-Ag
_cod_database_code               1564719
_publcif_datablock.id            {2208f5be-8aa8-438c-a22c-741e74185c61}
_shelx_shelxl_version_number     2018/3
_chemical_oxdiff_formula         'C50 H60 Ga1 N2 O1 P1 Ag1'
_shelx_estimated_absorpt_t_max   0.993
_shelx_estimated_absorpt_t_min   0.754
_reflns_odcompleteness_completeness 99.88
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     27.42
_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. Restrained distances
 C301-C306 \\sim C306-C305 \\sim C305-C304 \\sim C304-C303 \\sim C303-C302
\\sim C302-C301
 with sigma of 0.02
 C301-C303 \\sim C301-C305 \\sim C302-C304 \\sim C306-C302 \\sim C305-C303
\\sim C306-C304
 with sigma of 0.04
 C300-C302 \\sim C300-C306
 with sigma of 0.04
 C203-C204 \\sim C204-C205 \\sim C205-C200 \\sim C200-C201 \\sim C201-C202
\\sim C202-C203
 with sigma of 0.02
 C203-C201 \\sim C203-C205 \\sim C202-C200 \\sim C204-C202 \\sim C205-C201
\\sim C204-C200
 with sigma of 0.04
 C206-C202 \\sim C206-C204
 with sigma of 0.04
3. Restrained planarity
 C300, C301, C306, C305, C304, C303, C302
 with sigma of 0.1
 C206, C203, C204, C205, C200, C201, C202
 with sigma of 0.1
4. Uiso/Uaniso restraints and constraints
C300 \\sim C301 \\sim C306 \\sim C305 \\sim C304 \\sim C303 \\sim C302: within
2A with sigma of 0.04 and sigma for terminal atoms of 0.08
C300 \\sim C301 \\sim C306 \\sim C302 \\sim C305 \\sim C303 \\sim C304: within
2A with sigma of 0.005 and sigma for terminal atoms of 0.01
C300 \\sim C301: within 2A with sigma of 0.005 and sigma for terminal atoms of
0.01
C30 \\sim C32 \\sim C31: within 2A with sigma of 0.005 and sigma for terminal
atoms of 0.01
5. Rigid body (RIGU) restrains
 C300, C301, C306, C305, C304, C303, C302
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 C206, C203, C204, C205, C200, C201, C202
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
6.a Ternary CH refined with riding coordinates:
 C45(H45), C42(H42), C33(H33), C30(H30)
6.b Aromatic/amide H refined with riding coordinates:
 C3(H3), C11(H11), C5(H5), C9(H9), C26(H26), C40(H40), C39(H39), C38(H38),
 C28(H28), C27(H27), C201(H201), C200(H200), C205(H205), C204(H204), C202(H202),
  C306(H306), C305(H305), C304(H304), C303(H303), C302(H302)
6.c Fitted hexagon refined as free rotating group:
 C201(C200,C205,C204,C203,C202), C301(C306,C305,C304,C303,C302)
6.d Idealised Me refined as rotating group:
 C18(H18a,H18b,H18c), C19(H19a,H19b,H19c), C59(H59a,H59b,H59c), C15(H15a,H15b,
 H15c), C46(H46a,H46b,H46c), C21(H21a,H21b,H21c), C17(H17a,H17b,H17c), C23(H23a,
 H23b,H23c), C16(H16a,H16b,H16c), C50(H50a,H50b,H50c), C54(H54a,H54b,H54c),
 C53(H53a,H53b,H53c), C51(H51a,H51b,H51c), C58(H58a,H58b,H58c), C49(H49a,H49b,
 H49c), C44(H44a,H44b,H44c), C47(H47a,H47b,H47c), C57(H57a,H57b,H57c), C35(H35a,
 H35b,H35c), C43(H43a,H43b,H43c), C22(H22a,H22b,H22c), C31(H31a,H31b,H31c),
 C34(H34a,H34b,H34c), C55(H55a,H55b,H55c), C32(H32a,H32b,H32c), C206(H20a,H20b,
 H20c), C300(H30a,H30b,H30c)
;
_shelx_res_checksum              62695
_shelx_hkl_checksum              12623
_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 1.489
_oxdiff_exptl_absorpt_empirical_full_min 0.644
_publcif_funding_html
;
;