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_4134972
_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         'C8 H5 Al0.33 F5 O0.33 P0.33'
_chemical_formula_sum            'C8 H5 Al0.333 F5 O0.333 P0.333'
_chemical_formula_weight         220.77
_space_group_crystal_system      trigonal
_space_group_IT_number           148
_space_group_name_Hall           '-R 3'
_space_group_name_H-M_alt        'R -3 :H'
_symmetry_Int_Tables_number      148
_atom_sites_solution_primary     dual
_audit_creation_date             2019-06-13
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_cell_angle_alpha                90
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_cell_angle_gamma                120
_cell_formula_units_Z            18
_cell_length_a                   12.8696(2)
_cell_length_b                   12.8696(2)
_cell_length_c                   27.1408(6)
_cell_measurement_reflns_used    10212
_cell_measurement_temperature    123.15
_cell_measurement_theta_max      73.2040
_cell_measurement_theta_min      4.2500
_cell_volume                     3892.99(12)
_computing_cell_refinement       'CrysAlisPro 1.171.40.43a (Rigaku OD, 2019)'
_computing_data_collection       'CrysAlisPro 1.171.40.43a (Rigaku OD, 2019)'
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_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 0.9932
_diffrn_measured_fraction_theta_max 0.9915
_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    -90.00 -20.00   0.50    0.16    --  -42.80 119.00  16.00  140
  2  \w    -94.00 -69.00   0.50    0.16    --  -42.80 155.00 173.00   50
  3  \w   -104.00 -76.00   0.50    0.16    --  -42.80-155.00 135.00   56
  4  \w     59.00  84.00   0.50    0.16    --   42.80 155.00 173.00   50
  5  \w     42.00  93.00   0.50    0.16    --   42.80-119.00 -67.00  102
  6  \w     47.00  74.00   0.50    0.16    --   42.80-155.00 135.00   54
  7  \w     76.00 101.00   0.50    0.66    --   76.50 155.00 173.00   50
  8  \w     35.00  60.00   0.50    0.66    --   76.50-119.00 -67.00   50
  9  \w    105.00 130.00   0.50    0.66    --   76.50 119.00  16.00   50
 10  \w     81.00 106.00   0.50    0.66    --   76.50-155.00 135.00   50
 11  \w   -109.00 -84.00   0.50    0.66    -- -106.00 155.00 173.00   50
 12  \w    -83.00 -57.00   0.50    0.66    -- -106.00 119.00  16.00   52
 13  \w   -150.00-125.00   0.50    0.66    -- -106.00-119.00 -67.00   50
 14  \w    -57.00 -32.00   0.50    0.66    -- -106.00 155.00 173.00   50
 15  \w   -116.00 -17.00   0.50    0.16    --  -42.80 -77.00 -60.00  198
 16  \w     71.00 117.00   0.50    0.16    --   42.80 125.00-120.00   92
 17  \w     86.00 117.00   0.50    0.16    --   42.80 125.00 -60.00   62
 18  \w     77.00 102.00   0.50    0.16    --   42.80 125.00 -90.00   50
 19  \w     24.00 115.00   0.50    0.16    --   42.80  57.00-120.00  182
 20  \w     54.00 150.00   0.50    0.66    --   76.50  57.00-180.00  192
 21  \w   -177.00 -84.00   0.50    0.66    -- -106.00 -37.00 -60.00  186
 22  \w   -173.00 -86.00   0.50    0.66    -- -106.00 -19.00-120.00  174
 23  \w   -126.00 -33.00   0.50    0.66    -- -106.00  57.00-120.00  186
 24  \w    -94.00 -30.00   0.50    0.66    -- -106.00  37.00-120.00  128
 25  \w   -100.00 -37.00   0.50    0.66    -- -106.00 125.00-180.00  126
 26  \w   -113.00 -48.00   0.50    0.66    -- -106.00 125.00-120.00  130
 27  \w   -154.00-122.00   0.50    0.66    -- -106.00 -37.00-180.00   64
 28  \w   -133.00 -33.00   0.50    0.66    -- -106.00  77.00 120.00  200
 29  \w    -68.00 -28.00   0.50    0.66    -- -106.00  37.00  60.00   80
 30  \w   -115.00 -90.00   0.50    0.66    -- -106.00 125.00  90.00   50
 31  \w   -116.00 -88.00   0.50    0.66    -- -106.00 125.00 150.00   56
 32  \w    -99.00 -46.00   0.50    0.66    -- -106.00  77.00  90.00  106
 33  \w   -168.00-112.00   0.50    0.66    -- -106.00 -77.00 -90.00  112
 34  \w   -116.00 -65.00   0.50    0.66    -- -106.00 125.00 -90.00  102
 35  \w   -135.00-110.00   0.50    0.66    -- -106.00  77.00  90.00   50
 36  \w   -127.00 -84.00   0.50    0.66    -- -106.00  37.00  60.00   86
 37  \w   -177.00 -92.00   0.50    0.66    -- -106.00 -57.00   0.00  170
 38  \w   -123.00 -97.00   0.50    0.66    -- -106.00-155.00 135.00   52
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type
'XtaLAB Synergy, Single source at offset/far, HyPix'
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_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      0.0305882000
_diffrn_orient_matrix_UB_12      -0.0310633000
_diffrn_orient_matrix_UB_13      -0.0508324000
_diffrn_orient_matrix_UB_21      0.0925152000
_diffrn_orient_matrix_UB_22      -0.0264948000
_diffrn_orient_matrix_UB_23      0.0242314000
_diffrn_orient_matrix_UB_31      -0.0980529000
_diffrn_orient_matrix_UB_32      -0.1320415000
_diffrn_orient_matrix_UB_33      0.0070317000
_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  0.0250
_diffrn_reflns_av_unetI/netI     0.0099
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       33
_diffrn_reflns_limit_l_min       -33
_diffrn_reflns_number            15031
_diffrn_reflns_theta_full        74.2825
_diffrn_reflns_theta_max         74.28
_diffrn_reflns_theta_min         4.29
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'PhotonJet (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    2.472
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.60022
_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    1.6949
_exptl_crystal_description       cube
_exptl_crystal_F_000             1992.7604
_exptl_crystal_size_max          0.3
_exptl_crystal_size_mid          0.3
_exptl_crystal_size_min          0.3
_refine_diff_density_max         0.1885
_refine_diff_density_min         -0.2842
_refine_diff_density_rms         0.0437
_refine_ls_d_res_high            0.8009
_refine_ls_d_res_low             10.3099
_refine_ls_goodness_of_fit_ref   1.0423
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_constraints    7
_refine_ls_number_parameters     128
_refine_ls_number_reflns         1757
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.0423
_refine_ls_R_factor_all          0.0309
_refine_ls_R_factor_gt           0.0301
_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^)+(0.0375P)^2^+5.1951P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0778
_refine_ls_wR_factor_ref         0.0783
_reflns_Friedel_coverage         0.0
_reflns_limit_h_max              13
_reflns_limit_h_min              0
_reflns_limit_k_max              13
_reflns_limit_k_min              0
_reflns_limit_l_max              33
_reflns_limit_l_min              -33
_reflns_number_gt                1691
_reflns_number_total             1757
_reflns_threshold_expression     I>=2u(I)
_cod_data_source_file            ja0c03252_si_002.cif
_cod_data_source_block           Et3POAl(C6F5)3
_cod_depositor_comments
'Adding full bibliography for 4134972--4134984.cif.'
_cod_original_sg_symbol_H-M      'R -3'
_cod_database_code               4134972
_chemical_oxdiff_formula         'C24 H15 Al1 F15 O1 P1'
_reflns_odcompleteness_completeness 100.00
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     68.13
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2.a Secondary CH2 refined with riding coordinates:
 C3(H3a,H3b)
2.b Idealised Me refined as rotating group:
 C4(H4a,H4b,H4c)
;
_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 1.700
_oxdiff_exptl_absorpt_empirical_full_min 0.638