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_4134979
_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         'C41 H37 Al F15 N2 O P, C3 H3'
_chemical_formula_sum            'C44 H40 Al F15 N2 O P'
_chemical_formula_weight         955.75
_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             2019-04-23
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_cell_angle_alpha                90
_cell_angle_beta                 103.5030(10)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   10.47800(10)
_cell_length_b                   19.75960(10)
_cell_length_c                   21.5187(2)
_cell_measurement_reflns_used    34916
_cell_measurement_temperature    123.15
_cell_measurement_theta_max      74.0920
_cell_measurement_theta_min      4.3580
_cell_volume                     4332.10(6)
_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 0.9927
_diffrn_measured_fraction_theta_max 0.9927
_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    -47.00 -16.00   0.50    0.09    --  -42.80  87.00 -94.00   62
  2  \w    -29.00  76.00   0.50    0.09    --   42.80 -87.00 147.00  210
  3  \w     32.00  57.00   0.50    0.37    --   76.50 -87.00 147.00   50
  4  \w    -65.00 -39.00   0.50    0.37    -- -106.00  87.00 -94.00   52
  5  \w   -115.00 -79.00   0.50    0.37    -- -106.00  87.00 -94.00   72
  6  \w   -152.00-126.00   0.50    0.37    -- -106.00 -87.00 147.00   52
  7  \w     79.00 116.00   0.50    0.09    --   42.80 125.00 120.00   74
  8  \w     71.00  96.00   0.50    0.09    --   42.80 125.00 150.00   50
  9  \w     71.00 114.00   0.50    0.09    --   42.80 125.00-180.00   86
 10  \w     71.00 116.00   0.50    0.09    --   42.80 125.00 -60.00   90
 11  \w     73.00 117.00   0.50    0.09    --   42.80 125.00  30.00   88
 12  \w     72.00 117.00   0.50    0.09    --   42.80 125.00   0.00   90
 13  \w     89.00 114.00   0.50    0.37    --   76.50  87.00 -94.00   50
 14  \w   -135.00-109.00   0.50    0.37    -- -106.00 -99.00 -90.00   52
 15  \w   -177.00-140.00   0.50    0.37    -- -106.00 -99.00 -90.00   74
 16  \w   -120.00 -87.00   0.50    0.37    -- -106.00 -57.00-150.00   66
 17  \w   -150.00-124.00   0.50    0.37    -- -106.00  13.00  96.43   52
 18  \w   -118.00 -92.00   0.50    0.37    -- -106.00  63.00 -56.52   52
 19  \w   -127.00 -69.00   0.50    0.37    -- -106.00  57.00  60.00  116
 20  \w    -60.00 -33.00   0.50    0.37    -- -106.00  57.00  60.00   54
 21  \w    -65.00 -36.00   0.50    0.37    -- -106.00 125.00 120.00   58
 22  \w   -114.00 -73.00   0.50    0.37    -- -106.00 125.00 120.00   82
 23  \w   -177.00 -86.00   0.50    0.37    -- -106.00 -57.00-180.00  182
 24  \w    -97.00 -36.00   0.50    0.37    -- -106.00 125.00  30.00  122
 25  \w   -117.00 -91.00   0.50    0.37    -- -106.00  59.00-144.22   52
 26  \w    -87.00 -36.00   0.50    0.37    -- -106.00  57.00-150.00  102
 27  \w   -126.00 -96.00   0.50    0.37    -- -106.00  57.00 -30.00   60
 28  \w    -75.00 -33.00   0.50    0.37    -- -106.00  57.00 -30.00   84
 29  \w    -61.00 -35.00   0.50    0.37    -- -106.00  77.00-180.00   52
 30  \w   -111.00 -74.00   0.50    0.37    -- -106.00  13.00  96.43   74
 31  \w    -67.00 -29.00   0.50    0.37    -- -106.00  13.00  96.43   76
 32  \w   -123.00 -98.00   0.50    0.37    -- -106.00  57.00 150.00   50
 33  \w    -81.00 -33.00   0.50    0.37    -- -106.00  57.00 150.00   96
 34  \w   -106.00 -40.00   0.50    0.37    -- -106.00  92.00 -41.77  132
 35  \w   -125.00 -83.00   0.50    0.37    -- -106.00  57.00   0.00   84
 36  \w    -58.00 -33.00   0.50    0.37    -- -106.00  57.00   0.00   50
 37  \w   -164.00-139.00   0.50    0.37    -- -106.00 -77.00 -30.00   50
 38  \w    -66.00 -41.00   0.50    0.37    -- -106.00  54.00 119.61   50
 39  \w   -121.00 -87.00   0.50    0.37    -- -106.00  54.00 119.61   68
 40  \w   -171.00-146.00   0.50    0.37    -- -106.00 -99.00  90.00   50
 41  \w   -144.00-103.00   0.50    0.37    -- -106.00 -37.00-150.00   82
 42  \w   -134.00 -81.00   0.50    0.37    -- -106.00  19.00 -30.00  106
 43  \w   -111.00 -77.00   0.50    0.37    -- -106.00 -77.00 -30.00   68
 44  \w    -84.00 -58.00   0.50    0.37    -- -106.00 125.00  60.00   52
 45  \w   -141.00-113.00   0.50    0.37    -- -106.00 -57.00 -60.00   56
 46  \w   -145.00-119.00   0.50    0.37    -- -106.00 -99.00  60.00   52
 47  \w   -173.00-126.00   0.50    0.37    -- -106.00 -57.00 150.00   94
 48  \w    -67.00 -41.00   0.50    0.37    -- -106.00  57.00-120.00   52
 49  \w   -116.00 -90.00   0.50    0.37    -- -106.00  57.00 -60.00   52
 50  \w   -163.00-138.00   0.50    0.37    -- -106.00 -19.00  90.00   50
 51  \w   -175.00-150.00   0.50    0.37    -- -106.00 -19.00 150.00   50
 52  \w   -114.00 -89.00   0.50    0.37    -- -106.00 -19.00 150.00   50
 53  \w   -172.00 -80.00   0.50    0.37    -- -106.00 -77.00 120.00  184
 54  \w    -95.00 -69.00   0.50    0.37    -- -106.00  77.00-120.00   52
 55  \w   -173.00-145.00   0.50    0.37    -- -106.00 -57.00-150.00   56
;
_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      -0.0344322000
_diffrn_orient_matrix_UB_12      0.0623263000
_diffrn_orient_matrix_UB_13      -0.0437092000
_diffrn_orient_matrix_UB_21      -0.0732613000
_diffrn_orient_matrix_UB_22      0.0313336000
_diffrn_orient_matrix_UB_23      0.0472903000
_diffrn_orient_matrix_UB_31      0.1277455000
_diffrn_orient_matrix_UB_32      0.0347782000
_diffrn_orient_matrix_UB_33      0.0357075000
_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  0.0324
_diffrn_reflns_av_unetI/netI     0.0213
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       24
_diffrn_reflns_limit_k_min       -22
_diffrn_reflns_limit_l_max       26
_diffrn_reflns_limit_l_min       -26
_diffrn_reflns_number            57416
_diffrn_reflns_theta_full        74.2693
_diffrn_reflns_theta_max         74.27
_diffrn_reflns_theta_min         4.23
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'PhotonJet (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    1.680
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.74166
_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    1.4653
_exptl_crystal_description       block
_exptl_crystal_F_000             1966.1892
_exptl_crystal_size_max          0.2
_exptl_crystal_size_mid          0.2
_exptl_crystal_size_min          0.1
_refine_diff_density_max         0.3084
_refine_diff_density_min         -0.3614
_refine_diff_density_rms         0.0464
_refine_ls_d_res_high            0.8009
_refine_ls_d_res_low             10.4619
_refine_ls_goodness_of_fit_ref   1.0385
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_constraints    67
_refine_ls_number_parameters     615
_refine_ls_number_reflns         8754
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.0385
_refine_ls_R_factor_all          0.0324
_refine_ls_R_factor_gt           0.0307
_refine_ls_shift/su_max          0.0001
_refine_ls_shift/su_mean         0.0000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0350P)^2^+1.9609P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0775
_refine_ls_wR_factor_ref         0.0786
_reflns_Friedel_coverage         0.0
_reflns_limit_h_max              10
_reflns_limit_h_min              -13
_reflns_limit_k_max              24
_reflns_limit_k_min              0
_reflns_limit_l_max              26
_reflns_limit_l_min              -9
_reflns_number_gt                8250
_reflns_number_total             8754
_reflns_threshold_expression     I>=2u(I)
_cod_data_source_file            ja0c03252_si_002.cif
_cod_data_source_block           5a
_cod_depositor_comments
'Adding full bibliography for 4134972--4134984.cif.'
_cod_original_sg_symbol_Hall     '-P 2ybc (x-z,y,z)'
_cod_database_code               4134979
_chemical_oxdiff_formula         'C41 H38 Al1 F15 N2 O1 P1'
_reflns_odcompleteness_completeness 98.95
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     74.33
_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. Others
 Sof(C65a)=Sof(C66a)=Sof(C67a)=Sof(H65a)=Sof(H66a)=Sof(H67a)=1-FVAR(1)
 Sof(C65)=Sof(C66)=Sof(C67)=Sof(H65)=Sof(H66)=Sof(H67)=FVAR(1)
4.a Ternary CH refined with riding coordinates:
 C25(H25), C22(H22)
4.b Aromatic/amide H refined with riding coordinates:
 C8(H8), C9(H9), C5(H5), C3(H3), C4(H4), C65(H65), C66(H66), C67(H67),
 C65a(H65a), C66a(H66a), C67a(H67a)
4.c Idealised Me refined as rotating group:
 C14(H14a,H14b,H14c), C19(H19a,H19b,H19c), C15(H15a,H15b,H15c), C20(H20a,H20b,
 H20c), C27(H27a,H27b,H27c), C17(H17a,H17b,H17c), C18(H18a,H18b,H18c), C26(H26a,
 H26b,H26c), C24(H24a,H24b,H24c), C23(H23a,H23b,H23c)
;
_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 1.520
_oxdiff_exptl_absorpt_empirical_full_min 0.732