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_4134973
_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         'C45 H46 Al Cu F15 N2 O2 P'
_chemical_formula_sum            'C45 H46 Al Cu F15 N2 O2 P'
_chemical_formula_weight         1053.36
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_symmetry_Int_Tables_number      2
_atom_sites_solution_primary     iterative
_audit_creation_date             2019-06-26
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_cell_angle_alpha                102.0818(14)
_cell_angle_beta                 99.1286(14)
_cell_angle_gamma                109.5393(16)
_cell_formula_units_Z            2
_cell_length_a                   10.7445(2)
_cell_length_b                   13.4502(2)
_cell_length_c                   21.5779(3)
_cell_measurement_reflns_used    19986
_cell_measurement_temperature    123.15
_cell_measurement_theta_max      74.2010
_cell_measurement_theta_min      3.6140
_cell_volume                     2783.81(9)
_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 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'olex2.refine (Bourhis et al., 2015)'
_computing_structure_solution    'olex2.solve (Bourhis et al., 2015)'
_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 0.9990
_diffrn_measured_fraction_theta_max 0.9990
_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    -70.00 -29.00   0.50    0.05    --  -42.80 104.00-110.00   82
  2  \w     10.00  84.00   0.50    0.05    --   42.80-104.00 147.00  148
  3  \w     82.00 123.00   0.50    0.13    --   76.50 104.00-110.00   82
  4  \w     31.00  57.00   0.50    0.13    --   76.50-104.00 147.00   52
  5  \w   -110.00 -65.00   0.50    0.13    -- -106.00 104.00-110.00   90
  6  \w   -167.00-140.00   0.50    0.13    -- -106.00-104.00 147.00   54
  7  \w   -109.00 -21.00   0.50    0.05    --  -42.80 -57.00 150.00  176
  8  \w    -64.00  31.00   0.50    0.05    --  -42.80  57.00 -60.00  190
  9  \w     71.00 117.00   0.50    0.05    --   42.80 125.00  30.00   92
 10  \w     28.00  88.00   0.50    0.05    --   42.80-125.00  30.00  120
 11  \w     67.00  93.00   0.50    0.05    --   42.80  57.00 -60.00   52
 12  \w     78.00 104.00   0.50    0.05    --   42.80 125.00 150.00   52
 13  \w     79.00 115.00   0.50    0.05    --   42.80 125.00-180.00   72
 14  \w     71.00 111.00   0.50    0.05    --   42.80 125.00-150.00   80
 15  \w   -137.00 -25.00   0.50    0.13    -- -106.00  19.00 -30.00  224
 16  \w   -114.00 -88.00   0.50    0.13    -- -106.00 125.00-180.00   52
 17  \w   -170.00 -71.00   0.50    0.13    -- -106.00-125.00-150.00  198
 18  \w   -174.00 -93.00   0.50    0.13    -- -106.00 -19.00 120.00  162
 19  \w   -117.00 -54.00   0.50    0.13    -- -106.00 125.00  90.00  126
 20  \w   -132.00 -76.00   0.50    0.13    -- -106.00  77.00 -90.00  112
 21  \w   -125.00 -32.00   0.50    0.13    -- -106.00  57.00 120.00  186
 22  \w   -112.00 -32.00   0.50    0.13    -- -106.00  77.00-180.00  160
 23  \w    -63.00 -26.00   0.50    0.13    -- -106.00  19.00-180.00   74
 24  \w   -125.00 -90.00   0.50    0.13    -- -106.00  19.00-180.00   70
 25  \w   -108.00 -38.00   0.50    0.13    -- -106.00 125.00 -90.00  140
 26  \w   -136.00 -86.00   0.50    0.13    -- -106.00 -19.00 -30.00  100
 27  \w   -113.00 -88.00   0.50    0.13    -- -106.00 125.00 -30.00   50
 28  \w   -116.00 -74.00   0.50    0.13    -- -106.00 125.00   0.00   84
 29  \w    -60.00 -32.00   0.50    0.13    -- -106.00  77.00 -90.00   56
 30  \w   -111.00 -28.00   0.50    0.13    -- -106.00  37.00 -60.00  166
 31  \w   -122.00 -28.00   0.50    0.13    -- -106.00  37.00 120.00  188
;
_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      0.0380392000
_diffrn_orient_matrix_UB_12      0.0802327000
_diffrn_orient_matrix_UB_13      0.0687224000
_diffrn_orient_matrix_UB_21      -0.0925601000
_diffrn_orient_matrix_UB_22      -0.0922498000
_diffrn_orient_matrix_UB_23      0.0232391000
_diffrn_orient_matrix_UB_31      0.1210445000
_diffrn_orient_matrix_UB_32      -0.0331639000
_diffrn_orient_matrix_UB_33      0.0204382000
_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  0.0306
_diffrn_reflns_av_unetI/netI     0.0305
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       25
_diffrn_reflns_limit_l_min       -25
_diffrn_reflns_number            29318
_diffrn_reflns_theta_full        68.2513
_diffrn_reflns_theta_max         68.25
_diffrn_reflns_theta_min         3.63
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'PhotonJet (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    1.729
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.70396
_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    1.2565
_exptl_crystal_description       plate
_exptl_crystal_F_000             1077.2736
_exptl_crystal_size_max          0.4
_exptl_crystal_size_mid          0.3
_exptl_crystal_size_min          0.3
_refine_diff_density_max         0.6296
_refine_diff_density_min         -0.4346
_refine_diff_density_rms         0.0667
_refine_ls_d_res_high            0.8300
_refine_ls_d_res_low             12.1613
_refine_ls_goodness_of_fit_ref   1.0344
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_constraints    66
_refine_ls_number_parameters     617
_refine_ls_number_reflns         10169
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.0344
_refine_ls_R_factor_all          0.0437
_refine_ls_R_factor_gt           0.0417
_refine_ls_shift/su_max          0.0005
_refine_ls_shift/su_mean         0.0001
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0663P)^2^+1.8936P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1177
_refine_ls_wR_factor_ref         0.1194
_reflns_Friedel_coverage         0.0
_reflns_limit_h_max              12
_reflns_limit_h_min              -12
_reflns_limit_k_max              15
_reflns_limit_k_min              -16
_reflns_limit_l_max              25
_reflns_limit_l_min              0
_reflns_number_gt                9442
_reflns_number_total             10169
_reflns_threshold_expression     I>=2u(I)
_cod_data_source_file            ja0c03252_si_002.cif
_cod_data_source_block           2a
_cod_depositor_comments
'Adding full bibliography for 4134972--4134984.cif.'
_cod_database_code               4134973
_chemical_oxdiff_formula         'C45 H46 Al1 Cu1 F15 N2 O2 P1'
_reflns_odcompleteness_completeness 99.97
_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. Restrained distances
3.a Ternary CH refined with riding coordinates:
 C1(H1), C0da(H0da)
3.b Aromatic/amide H refined with riding coordinates:
 C7aa(H7aa), C6ba(H6ba), C9aa(H9aa), C6aa(H6aa), C0ba(H0ba)
3.c Idealised Me refined as rotating group:
 C(Ha,Hb,Hc), C12(H12a,H12b,H12c), C1da(H1da,H1db,H1dc), C2da(H2da,H2db,H2dc),
 C3da(H3da,H3db,H3dc), C5da(H5da,H5db,H5dc), C8da(H8da,H8db,H8dc), C9da(H9da,
 H9db,H9dc), C0ea(H0ea,H0eb,H0ec), C1ea(H1ea,H1eb,H1ec), C2ea(H2ea,H2eb,H2ec),
 C3ea(H3ea,H3eb,H3ec), C4ea(H4ea,H4eb,H4ec)
;
_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 1.438
_oxdiff_exptl_absorpt_empirical_full_min 0.663