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_4134977
_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 H39 Al F15 N2 O P, C7 H8'
_chemical_formula_sum            'C48 H47 Al F15 N2 O P'
_chemical_formula_weight         1010.85
_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             2019-04-03
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_cell_angle_alpha                77.186(2)
_cell_angle_beta                 87.431(2)
_cell_angle_gamma                77.690(2)
_cell_formula_units_Z            2
_cell_length_a                   10.7276(3)
_cell_length_b                   12.1842(3)
_cell_length_c                   18.7183(5)
_cell_measurement_reflns_used    15332
_cell_measurement_temperature    123.15
_cell_measurement_theta_max      31.1060
_cell_measurement_theta_min      2.2210
_cell_volume                     2330.83(11)
_computing_cell_refinement       'CrysAlisPro 1.171.39.46e (Rigaku OD, 2018)'
_computing_data_collection       'CrysAlisPro 1.171.39.46e (Rigaku OD, 2018)'
_computing_data_reduction        'CrysAlisPro 1.171.39.46e (Rigaku OD, 2018)'
_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_type            HyPix
_diffrn_measured_fraction_theta_full 0.9978
_diffrn_measured_fraction_theta_max 0.9978
_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    -34.00  -2.00   0.50   15.69    --   -5.49  96.00  28.00   64
  2  \w    -11.00  32.00   0.50   15.69    --    5.65  96.00  28.00   86
  3  \w    -20.00  66.00   0.50   15.69    --   -5.49  57.00  60.00  172
  4  \w     -7.00  52.00   0.50   15.69    --   -5.49  57.00 -90.00  118
  5  \w    -18.00  58.00   0.50   15.69    --   -5.49  37.00-180.00  152
  6  \w    -17.00   8.00   0.50   15.69    --    5.65 -96.00 -80.00   50
  7  \w    -12.00  14.00   0.50   15.69    --    5.65 -99.00  60.00   52
  8  \w    -26.00  28.00   0.50   15.69    --   -5.49 -99.00 120.00  108
  9  \w      2.00  27.00   0.50   15.69    --    5.65 -99.00 150.00   50
 10  \w    -78.00   4.00   0.50   15.69    --   -5.49 -77.00 -60.00  164
;
_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      -0.0032625000
_diffrn_orient_matrix_UB_12      -0.0416288000
_diffrn_orient_matrix_UB_13      0.0328083000
_diffrn_orient_matrix_UB_21      -0.0475978000
_diffrn_orient_matrix_UB_22      -0.0195264000
_diffrn_orient_matrix_UB_23      -0.0159264000
_diffrn_orient_matrix_UB_31      0.0479970000
_diffrn_orient_matrix_UB_32      -0.0401532000
_diffrn_orient_matrix_UB_33      -0.0134227000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0618
_diffrn_reflns_av_unetI/netI     0.0626
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       26
_diffrn_reflns_limit_l_min       -25
_diffrn_reflns_number            42359
_diffrn_reflns_theta_full        26.3709
_diffrn_reflns_theta_max         26.37
_diffrn_reflns_theta_min         2.23
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'PhotonJet (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    0.177
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.79305
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.39.46e (Rigaku Oxford Diffraction, 2018)
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    1.4402
_exptl_crystal_description       block
_exptl_crystal_F_000             1041.1190
_exptl_crystal_size_max          0.3
_exptl_crystal_size_mid          0.2
_exptl_crystal_size_min          0.2
_refine_diff_density_max         1.2636
_refine_diff_density_min         -0.5416
_refine_diff_density_rms         0.0767
_refine_ls_d_res_high            0.8000
_refine_ls_d_res_low             9.1260
_refine_ls_goodness_of_fit_ref   1.0327
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_constraints    70
_refine_ls_number_parameters     624
_refine_ls_number_reflns         9519
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.0327
_refine_ls_R_factor_all          0.0661
_refine_ls_R_factor_gt           0.0495
_refine_ls_shift/su_max          0.0009
_refine_ls_shift/su_mean         0.0000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0661P)^2^+1.5774P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1292
_refine_ls_wR_factor_ref         0.1393
_reflns_Friedel_coverage         0.0
_reflns_limit_h_max              13
_reflns_limit_h_min              -13
_reflns_limit_k_max              15
_reflns_limit_k_min              -14
_reflns_limit_l_max              23
_reflns_limit_l_min              0
_reflns_number_gt                7446
_reflns_number_total             9519
_reflns_threshold_expression     I>=2u(I)
_cod_data_source_file            ja0c03252_si_002.cif
_cod_data_source_block           3b
_cod_depositor_comments
'Adding full bibliography for 4134972--4134984.cif.'
_cod_database_code               4134977
_chemical_oxdiff_formula         'C41 H39 Al1 F15 N2 O1 P1'
_reflns_odcompleteness_completeness 99.94
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     26.32
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2.a Ternary CH refined with riding coordinates:
 C25(H25), C22(H22)
2.b Secondary CH2 refined with riding coordinates:
 C8(H8a,H8b), C9(H9a,H9b)
2.c Aromatic/amide H refined with riding coordinates:
 C3(H3), C5(H5), C4(H4), C67(H67), C66(H66), C63(H63), C65(H65), C64(H64)
2.d Idealised Me refined as rotating group:
 C19(H19a,H19b,H19c), C17(H17a,H17b,H17c), C14(H14a,H14b,H14c), C18(H18a,H18b,
 H18c), C15(H15a,H15b,H15c), C20(H20a,H20b,H20c), C27(H27a,H27b,H27c), C26(H26a,
 H26b,H26c), C24(H24a,H24b,H24c), C23(H23a,H23b,H23c), C68(H68a,H68b,H68c)
;
_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 3.609
_oxdiff_exptl_absorpt_empirical_full_min 0.324