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_4134981
_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         'C46 H74 Cu N4 O2 P2, C22 H9 Al F15 O'
_chemical_formula_sum            'C68 H83 Al Cu F15 N4 O3 P2'
_chemical_formula_weight         1441.893
_space_group_crystal_system      orthorhombic
_space_group_IT_number           61
_space_group_name_Hall           '-P 2ac 2ab'
_space_group_name_H-M_alt        'P b c a'
_symmetry_Int_Tables_number      61
_atom_sites_solution_primary     dual
_audit_creation_date             2020-02-29
_audit_creation_method
;
Olex2 1.3
(compiled Nov 21 2019 18:26:39 for OlexSys, GUI svn.r6003)
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   19.1617(2)
_cell_length_b                   19.1616(2)
_cell_length_c                   38.3323(4)
_cell_measurement_reflns_used    29665
_cell_measurement_temperature    123.15
_cell_measurement_theta_max      76.8840
_cell_measurement_theta_min      3.9650
_cell_volume                     14074.4(3)
_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 0.9984
_diffrn_measured_fraction_theta_max 0.9982
_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    -15.00  25.28   0.38    1.00    --   49.83 -76.00  10.00  106
  2  \w     11.00  37.22   0.38    3.00    --   66.50 -76.00  10.00   69
  3  \w     30.00  89.66   0.38    1.00    --   49.83  76.00 137.00  157
  4  \w    -37.00  10.12   0.38    1.00    --  -53.08  76.00 137.00  124
  5  \w    -86.00 -44.96   0.38    3.00    -- -105.75  37.00  90.00  108
  6  \w   -106.00 -53.94   0.38    3.00    -- -105.75  37.00  30.00  137
  7  \w   -111.00 -37.28   0.38    3.00    -- -105.75  19.00 -60.00  194
  8  \w    -61.00 -32.88   0.38    3.00    -- -105.75  37.00 -90.00   74
  9  \w   -111.00 -70.34   0.38    3.00    -- -105.75  37.00 -90.00  107
 10  \w   -156.00-131.30   0.38    3.00    -- -105.75 -76.00  10.00   65
 11  \w   -168.00-127.72   0.38    3.00    -- -105.75 -37.00  90.00  106
 12  \w   -177.00-101.00   0.38    3.00    -- -105.75 -37.00 120.00  200
 13  \w   -124.00 -98.92   0.38    1.00    --  -53.08-125.00  60.00   66
 14  \w   -124.00 -76.88   0.38    1.00    --  -53.08-125.00 150.00  124
 15  \w     67.00  92.08   0.38    3.00    --   66.50  76.00 137.00   66
 16  \w     72.00  98.22   0.38    1.00    --   49.83 125.00  90.00   69
 17  \w   -111.00 -45.64   0.38    3.00    -- -105.75  76.00 137.00  172
;
_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      0.0411671000
_diffrn_orient_matrix_UB_12      -0.0664394000
_diffrn_orient_matrix_UB_13      0.0094265000
_diffrn_orient_matrix_UB_21      -0.0472135000
_diffrn_orient_matrix_UB_22      -0.0110354000
_diffrn_orient_matrix_UB_23      0.0320896000
_diffrn_orient_matrix_UB_31      -0.0504467000
_diffrn_orient_matrix_UB_32      -0.0439104000
_diffrn_orient_matrix_UB_33      -0.0222566000
_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  0.0563
_diffrn_reflns_av_unetI/netI     0.0394
_diffrn_reflns_Laue_measured_fraction_full 0.9984
_diffrn_reflns_Laue_measured_fraction_max 0.9982
_diffrn_reflns_limit_h_max       22
_diffrn_reflns_limit_h_min       -23
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_k_min       -23
_diffrn_reflns_limit_l_max       34
_diffrn_reflns_limit_l_min       -46
_diffrn_reflns_number            73504
_diffrn_reflns_point_group_measured_fraction_full 0.9984
_diffrn_reflns_point_group_measured_fraction_max 0.9982
_diffrn_reflns_theta_full        67.6840
_diffrn_reflns_theta_max         68.25
_diffrn_reflns_theta_min         3.46
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'PhotonJet (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    1.744
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.54660
_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    1.361
_exptl_crystal_description       block
_exptl_crystal_F_000             6011.875
_exptl_crystal_size_max          0.1
_exptl_crystal_size_mid          0.1
_exptl_crystal_size_min          0.1
_refine_diff_density_max         0.6951
_refine_diff_density_min         -0.4575
_refine_diff_density_rms         0.0656
_refine_ls_d_res_high            0.8300
_refine_ls_d_res_low             12.7748
_refine_ls_goodness_of_fit_ref   1.0415
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_constraints    120
_refine_ls_number_parameters     870
_refine_ls_number_reflns         12861
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.0415
_refine_ls_R_factor_all          0.0506
_refine_ls_R_factor_gt           0.0410
_refine_ls_shift/su_max          0.0008
_refine_ls_shift/su_mean         0.0000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0465P)^2^+8.9821P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1003
_refine_ls_wR_factor_ref         0.1054
_reflns_Friedel_coverage         0.0
_reflns_limit_h_max              23
_reflns_limit_h_min              0
_reflns_limit_k_max              23
_reflns_limit_k_min              0
_reflns_limit_l_max              46
_reflns_limit_l_min              0
_reflns_number_gt                10910
_reflns_number_total             12861
_reflns_threshold_expression     I>=2u(I)
_cod_data_source_file            ja0c03252_si_002.cif
_cod_data_source_block           8a
_cod_depositor_comments
'Adding full bibliography for 4134972--4134984.cif.'
_cod_database_code               4134981
_chemical_oxdiff_formula         'C544 H688 Al8 Cu8 F104 N32 O40 P16 '
_reflns_odcompleteness_completeness 99.81
_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:
 C50(H50), C23(H23), C26(H26), C53(H53)
3.b Aromatic/amide H refined with riding coordinates:
 C9(H9), C10(H10), C31(H31), C32(H32), C33(H33), C37(H37), C36(H36), C4(H4),
 C6(H6), C5(H5)
3.c Idealised Me refined as rotating group:
 C92(H92a,H92b,H92c), C15(H15a,H15b,H15c), C93(H93a,H93b,H93c), C16(H16a,H16b,
 H16c), C20(H20a,H20b,H20c), C94(H94a,H94b,H94c), C21(H21a,H21b,H21c), C18(H18a,
 H18b,H18c), C19(H19a,H19b,H19c), C25(H25a,H25b,H25c), C55(H55a,H55b,H55c),
 C28(H28a,H28b,H28c), C52(H52a,H52b,H52c), C47(H47a,H47b,H47c), C42(H42a,H42b,
 H42c), C51(H51a,H51b,H51c), C45(H45a,H45b,H45c), C43(H43a,H43b,H43c), C54(H54a,
 H54b,H54c), C27(H27a,H27b,H27c), C46(H46a,H46b,H46c), C48(H48a,H48b,H48c),
 C24(H24a,H24b,H24c)
;
_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 2.520
_oxdiff_exptl_absorpt_empirical_full_min 0.538