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_4134983
_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         'C33 H34 Al Br Cu F10 N2 O2 P'
_chemical_formula_sum            'C33 H34 Al Br Cu F10 N2 O2 P'
_chemical_formula_weight         882.04
_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     dual
_audit_creation_date             2019-10-07
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_cell_angle_alpha                106.815(2)
_cell_angle_beta                 91.023(2)
_cell_angle_gamma                96.979(2)
_cell_formula_units_Z            2
_cell_length_a                   9.6259(2)
_cell_length_b                   12.1938(3)
_cell_length_c                   16.5765(4)
_cell_measurement_reflns_used    13548
_cell_measurement_temperature    123.15
_cell_measurement_theta_max      73.6700
_cell_measurement_theta_min      3.7750
_cell_volume                     1845.82(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 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'olex2.refine (Bourhis et al., 2015)'
_computing_structure_solution    'ShelXT (Sheldrick, 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 0.9966
_diffrn_measured_fraction_theta_max 0.9966
_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    -22.00   3.00   0.50    0.43    --  -42.80  83.00  22.00   50
  2  \w     11.00 105.00   0.50    0.43    --   42.80  83.00  22.00  188
  3  \w     74.00  99.00   0.50    1.72    --   76.50  83.00  22.00   50
  4  \w     72.00 115.00   0.50    0.43    --   42.80 125.00  60.00   86
  5  \w     32.00  71.00   0.50    1.72    --   76.50 -83.00 -98.00   78
  6  \w     -2.00  23.00   0.50    0.43    --   42.80 -83.00 -98.00   50
  7  \w    -64.00  29.00   0.50    0.43    --  -42.80  57.00-180.00  186
  8  \w    -87.00 -61.00   0.50    1.72    -- -106.00  37.00-120.00   52
  9  \w   -128.00 -92.00   0.50    1.72    -- -106.00 -19.00 -60.00   72
 10  \w   -128.00 -89.00   0.50    1.72    -- -106.00  37.00-120.00   78
 11  \w   -117.00 -92.00   0.50    1.72    -- -106.00 125.00 -90.00   50
 12  \w   -112.00 -43.00   0.50    1.72    -- -106.00 125.00-150.00  138
 13  \w   -136.00 -44.00   0.50    1.72    -- -106.00  83.00  22.00  184
 14  \w    -96.00 -68.00   0.50    1.72    -- -106.00 125.00  60.00   56
 15  \w   -110.00 -46.00   0.50    1.72    -- -106.00 125.00  30.00  128
 16  \w    -95.00 -17.00   0.50    0.43    --  -42.80 125.00  30.00  156
 17  \w    -95.00 -10.00   0.50    0.43    --  -42.80 125.00 150.00  170
 18  \w   -116.00 -33.00   0.50    1.72    -- -106.00 125.00 120.00  166
 19  \w   -116.00 -90.00   0.50    1.72    -- -106.00 125.00  90.00   52
 20  \w   -128.00 -35.00   0.50    1.72    -- -106.00  57.00  30.00  186
 21  \w   -108.00 -83.00   0.50    1.72    -- -106.00 -57.00-150.00   50
 22  \w   -100.00 -75.00   0.50    1.72    -- -106.00 -83.00 -98.00   50
 23  \w   -109.00 -21.00   0.50    0.43    --  -42.80 -83.00 -98.00  176
 24  \w   -132.00 -85.00   0.50    1.72    -- -106.00 -37.00 120.00   94
 25  \w   -170.00 -76.00   0.50    1.72    -- -106.00-125.00  60.00  188
 26  \w   -166.00-113.00   0.50    1.72    -- -106.00 -83.00 -98.00  106
 27  \w   -165.00 -78.00   0.50    1.72    -- -106.00 -77.00-120.00  174
 28  \w   -176.00-125.00   0.50    1.72    -- -106.00 -57.00-150.00  102
 29  \w   -177.00-127.00   0.50    1.72    -- -106.00 -57.00 -60.00  100
 30  \w   -175.00-102.00   0.50    1.72    -- -106.00 -77.00 -30.00  146
 31  \w   -176.00-100.00   0.50    1.72    -- -106.00 -77.00 120.00  152
;
_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      0.0745180000
_diffrn_orient_matrix_UB_12      0.1079962000
_diffrn_orient_matrix_UB_13      0.0668021000
_diffrn_orient_matrix_UB_21      0.1300072000
_diffrn_orient_matrix_UB_22      -0.0039920000
_diffrn_orient_matrix_UB_23      -0.0531247000
_diffrn_orient_matrix_UB_31      -0.0602003000
_diffrn_orient_matrix_UB_32      0.0777871000
_diffrn_orient_matrix_UB_33      -0.0465897000
_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  0.0227
_diffrn_reflns_av_unetI/netI     0.0234
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            19421
_diffrn_reflns_theta_full        68.2451
_diffrn_reflns_theta_max         68.25
_diffrn_reflns_theta_min         3.82
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'PhotonJet (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    3.499
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.87320
_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    1.5869
_exptl_crystal_description       plate
_exptl_crystal_F_000             886.7408
_exptl_crystal_size_max          0.1
_exptl_crystal_size_mid          0.05
_exptl_crystal_size_min          0.05
_refine_diff_density_max         0.3523
_refine_diff_density_min         -0.4307
_refine_diff_density_rms         0.0579
_refine_ls_d_res_high            0.8300
_refine_ls_d_res_low             11.5698
_refine_ls_goodness_of_fit_ref   1.0569
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_constraints    50
_refine_ls_number_parameters     469
_refine_ls_number_reflns         6731
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.0569
_refine_ls_R_factor_all          0.0280
_refine_ls_R_factor_gt           0.0266
_refine_ls_shift/su_max          0.0003
_refine_ls_shift/su_mean         0.0000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0244P)^2^+1.5709P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0678
_refine_ls_wR_factor_ref         0.0685
_reflns_Friedel_coverage         0.0
_reflns_limit_h_max              11
_reflns_limit_h_min              -11
_reflns_limit_k_max              13
_reflns_limit_k_min              -14
_reflns_limit_l_max              19
_reflns_limit_l_min              0
_reflns_number_gt                6344
_reflns_number_total             6731
_reflns_threshold_expression     I>=2u(I)
_cod_data_source_file            ja0c03252_si_002.cif
_cod_data_source_block           9c
_cod_depositor_comments
'Adding full bibliography for 4134972--4134984.cif.'
_cod_database_code               4134983
_chemical_oxdiff_formula         'C66 H70 Al2 Br2 Cu2 F18 N4 O6 P2 '
_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. Restrained distances
3.a Aromatic/amide H refined with riding coordinates:
 C10(H10), C4(H4), C8(H8), C11(H11), C7(H7), C5(H5), C6(H6)
3.b Idealised Me refined as rotating group:
 C16(H16a,H16b,H16c), C21(H21a,H21b,H21c), C17(H17a,H17b,H17c), C22(H22a,H22b,
 H22c), C49(H49a,H49b,H49c), C19(H19a,H19b,H19c), C20(H20a,H20b,H20c), C50(H50a,
 H50b,H50c), C51(H51a,H51b,H51c)
;
_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 1.457
_oxdiff_exptl_absorpt_empirical_full_min 0.769