Rotation-Triggered Transmetalation on a Heterobimetallic Cu/Al <i>N</i>-Phosphine-Oxide-Substituted Imidazolylidene Complex.
Asada, Takahiro; Hoshimoto, Yoichi; Ogoshi, Sensuke; Journal of the American Chemical Society 142 (2020) 9772–9784; doi:10.1021/jacs.0c03252

data_4134982
_publ_section_title
;
 Rotation-Triggered Transmetalation on a Heterobimetallic Cu/Al
 <i>N</i>-Phosphine-Oxide-Substituted Imidazolylidene Complex.
;
_journal_issue                   21
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              9772
_journal_page_last               9784
_journal_paper_doi               10.1021/jacs.0c03252
_journal_volume                  142
_journal_year                    2020
_chemical_formula_moiety         'C43 H33 Al Cu F15 N2 O, C7 H8'
_chemical_formula_sum            'C50 H41 Al Cu F15 N2 O'
_chemical_formula_weight         1061.399
_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'
_symmetry_Int_Tables_number      14
_atom_sites_solution_primary     dual
_audit_creation_date             2020-03-16
_audit_creation_method
;
Olex2 1.3
(compiled 2020.02.04 svn.rd84adfe8 for OlexSys, GUI svn.r6032)
;
_cell_angle_alpha                90
_cell_angle_beta                 115.889(11)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   13.1271(13)
_cell_length_b                   29.4891(16)
_cell_length_c                   13.6529(12)
_cell_measurement_reflns_used    4149
_cell_measurement_temperature    123.15
_cell_measurement_theta_max      72.0350
_cell_measurement_theta_min      4.1640
_cell_volume                     4754.7(8)
_computing_cell_refinement       'CrysAlisPro 1.171.40.43a (Rigaku OD, 2019)'
_computing_data_collection       'CrysAlisPro 1.171.40.43a (Rigaku OD, 2019)'
_computing_data_reduction        'CrysAlisPro 1.171.40.43a (Rigaku OD, 2019)'
_computing_molecular_graphics    'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_structure_refinement  'olex2.refine 1.3 (Bourhis et al., 2015)'
_computing_structure_solution    'SHELXT 2014/5 (Sheldrick, 2014)'
_diffrn_ambient_temperature      123.15
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 10.0000
_diffrn_detector_type            HyPix
_diffrn_measured_fraction_theta_full 0.9993
_diffrn_measured_fraction_theta_max 0.9993
_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     -7.00  18.00   0.50    1.00    --   42.80 -55.00 -71.00   50
  2  \w     26.00  51.00   0.50    3.00    --   76.50 -55.00 -71.00   50
  3  \w     65.00  97.00   0.50    1.00    --   42.80  55.00  70.00   64
  4  \w    103.00 148.00   0.50    3.00    --   76.50  55.00  70.00   90
  5  \w     71.00 113.00   0.50    1.00    --   42.80 125.00   0.00   84
  6  \w     73.00 146.00   0.50    3.00    --   76.50 125.00 -30.00  146
  7  \w     -4.00  23.00   0.50    1.00    --  -42.80  57.00-180.00   54
  8  \w    -59.00 -32.00   0.50    3.00    -- -106.00 125.00 -60.00   54
  9  \w    -70.00 -43.00   0.50    3.00    -- -106.00 125.00-120.00   54
 10  \w    -61.00 -12.00   0.50    1.00    --  -42.80 125.00 -30.00   98
 11  \w    -60.00  31.00   0.50    1.00    --  -42.80  55.00  70.00  182
 12  \w    -94.00 -12.00   0.50    1.00    --  -42.80 125.00  60.00  164
 13  \w    -95.00 -69.00   0.50    1.00    --  -42.80 125.00 -30.00   52
 14  \w   -127.00 -32.00   0.50    3.00    -- -106.00  55.00  70.00  190
 15  \w   -115.00 -32.00   0.50    3.00    -- -106.00  37.00 -90.00  166
 16  \w    -65.00 -30.00   0.50    1.00    --  -42.80  57.00-180.00   70
 17  \w   -116.00 -21.00   0.50    1.00    --  -42.80 -55.00 -71.00  190
 18  \w   -131.00 -34.00   0.50    3.00    -- -106.00  77.00  60.00  194
 19  \w   -116.00 -86.00   0.50    3.00    -- -106.00 125.00 120.00   60
 20  \w   -115.00 -34.00   0.50    3.00    -- -106.00 125.00  90.00  162
 21  \w   -114.00 -42.00   0.50    3.00    -- -106.00 125.00  60.00  144
 22  \w   -119.00 -33.00   0.50    3.00    -- -106.00  57.00 -90.00  172
 23  \w   -116.00 -33.00   0.50    3.00    -- -106.00 125.00-150.00  166
 24  \w   -130.00 -86.00   0.50    3.00    -- -106.00 144.00-160.14   88
 25  \w   -130.00-103.00   0.50    3.00    -- -106.00 144.00 -15.29   54
 26  \w   -177.00 -96.00   0.50    3.00    -- -106.00 -19.00 150.00  162
 27  \w   -174.00-112.00   0.50    3.00    -- -106.00 -99.00   0.00  124
 28  \w   -177.00 -85.00   0.50    3.00    -- -106.00 -55.00 -71.00  184
 29  \w   -175.00 -99.00   0.50    3.00    -- -106.00 -37.00  30.00  152
 30  \w   -158.00 -71.00   0.50    3.00    -- -106.00-125.00 150.00  174
 31  \w   -171.00 -92.00   0.50    3.00    -- -106.00 -37.00   0.00  158
 32  \w   -172.00-104.00   0.50    3.00    -- -106.00 -57.00 -90.00  136
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type
'XtaLAB Synergy, Single source at offset/far, HyPix'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      0.0375666000
_diffrn_orient_matrix_UB_12      0.0348430000
_diffrn_orient_matrix_UB_13      -0.0617678000
_diffrn_orient_matrix_UB_21      0.1208457000
_diffrn_orient_matrix_UB_22      -0.0005169000
_diffrn_orient_matrix_UB_23      0.0934050000
_diffrn_orient_matrix_UB_31      0.0321857000
_diffrn_orient_matrix_UB_32      -0.0389024000
_diffrn_orient_matrix_UB_33      -0.0563512000
_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  0.1039
_diffrn_reflns_av_unetI/netI     0.0524
_diffrn_reflns_Laue_measured_fraction_full 0.9993
_diffrn_reflns_Laue_measured_fraction_max 0.9993
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       32
_diffrn_reflns_limit_k_min       -35
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_number            53720
_diffrn_reflns_point_group_measured_fraction_full 0.9993
_diffrn_reflns_point_group_measured_fraction_max 0.9993
_diffrn_reflns_theta_full        67.6840
_diffrn_reflns_theta_max         68.25
_diffrn_reflns_theta_min         3.90
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'PhotonJet (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    1.710
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.51274
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.40.43a (Rigaku Oxford Diffraction, 2019)
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    1.483
_exptl_crystal_description       plate
_exptl_crystal_F_000             2161.517
_exptl_crystal_size_max          0.3
_exptl_crystal_size_mid          0.1
_exptl_crystal_size_min          0.1
_refine_diff_density_max         0.9946
_refine_diff_density_min         -0.6495
_refine_diff_density_rms         0.1145
_refine_ls_d_res_high            0.8300
_refine_ls_d_res_low             11.3385
_refine_ls_goodness_of_fit_ref   1.0900
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_constraints    62
_refine_ls_number_parameters     641
_refine_ls_number_reflns         8716
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.0900
_refine_ls_R_factor_all          0.1029
_refine_ls_R_factor_gt           0.0768
_refine_ls_shift/su_max          0.0010
_refine_ls_shift/su_mean         0.0000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0765P)^2^+6.8927P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1737
_refine_ls_wR_factor_ref         0.1888
_reflns_Friedel_coverage         0.0
_reflns_limit_h_max              8
_reflns_limit_h_min              -15
_reflns_limit_k_max              35
_reflns_limit_k_min              0
_reflns_limit_l_max              16
_reflns_limit_l_min              -8
_reflns_number_gt                6584
_reflns_number_total             8716
_reflns_threshold_expression     I>=2u(I)
_cod_data_source_file            ja0c03252_si_002.cif
_cod_data_source_block           IMesCuOtBuAl(C6F5)3
_cod_depositor_comments
'Adding full bibliography for 4134972--4134984.cif.'
_cod_original_sg_symbol_Hall     '-P 2ybc (x-z,y,z)'
_cod_database_code               4134982
_chemical_oxdiff_formula         'C208 H172 Al4 Cu4 F52 N4 O8 '
_reflns_odcompleteness_completeness 99.96
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     68.13
_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 Aromatic/amide H refined with riding coordinates:
 C45(H45), C56(H56), C54(H54), C43(H43), C48(H48), C49(H49), C68(H68),
 C69(H69), C67(H67), C65(H65), C66(H66)
2.b Idealised Me refined as rotating group:
 C38(H38a,H38b,H38c), C39(H39a,H39b,H39c), C40(H40a,H40b,H40c), C62(H62a,H62b,
 H62c), C58(H58a,H58b,H58c), C60(H60a,H60b,H60c), C59(H59a,H59b,H59c), C61(H61a,
 H61b,H61c), C63(H63a,H63b,H63c), C70(H70a,H70b,H70c)
;
_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 2.091
_oxdiff_exptl_absorpt_empirical_full_min 0.380