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_4134974
_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         'C45 H48 Al Cu F15 N2 O2 P'
_chemical_formula_sum            'C45 H48 Al Cu F15 N2 O2 P'
_chemical_formula_weight         1055.37
_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             2019-06-12
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_cell_angle_alpha                102.2940(10)
_cell_angle_beta                 98.9510(10)
_cell_angle_gamma                108.8730(10)
_cell_formula_units_Z            2
_cell_length_a                   10.73790(10)
_cell_length_b                   13.4792(2)
_cell_length_c                   21.5394(2)
_cell_measurement_reflns_used    18867
_cell_measurement_temperature    123.15
_cell_measurement_theta_max      73.6600
_cell_measurement_theta_min      3.6190
_cell_volume                     2796.08(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 0.9975
_diffrn_measured_fraction_theta_max 0.9975
_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    -66.00  25.00   0.50    0.06    --  -42.80  99.00  70.00  182
  2  \w     32.00  59.00   0.50    0.06    --   42.80 -99.00 -36.00   54
  3  \w     92.00 118.00   0.50    0.24    --   76.50  99.00  70.00   52
  4  \w     31.00  56.00   0.50    0.24    --   76.50 -99.00 -36.00   50
  5  \w    -70.00 -37.00   0.50    0.24    -- -106.00  99.00  70.00   66
  6  \w   -127.00 -92.00   0.50    0.24    -- -106.00 -99.00 -36.00   70
  7  \w   -116.00 -85.00   0.50    0.06    --  -42.80-125.00-150.00   62
  8  \w    -94.00 -11.00   0.50    0.06    --  -42.80 125.00  90.00  166
  9  \w     71.00  99.00   0.50    0.06    --   42.80 125.00 -90.00   56
 10  \w    -34.00  61.00   0.50    0.06    --   42.80 -37.00   0.00  190
 11  \w    -28.00  65.00   0.50    0.06    --   42.80 -57.00 -90.00  186
 12  \w     72.00 117.00   0.50    0.06    --   42.80 125.00  90.00   90
 13  \w     82.00 108.00   0.50    0.06    --   42.80 125.00  30.00   52
 14  \w     71.00 123.00   0.50    0.24    --   76.50 125.00   0.00  104
 15  \w   -166.00 -78.00   0.50    0.24    -- -106.00 -77.00 120.00  176
 16  \w    -82.00 -33.00   0.50    0.24    -- -106.00 125.00 -30.00   98
 17  \w   -143.00-101.00   0.50    0.24    -- -106.00 -57.00-120.00   84
 18  \w   -117.00 -57.00   0.50    0.24    -- -106.00 125.00 120.00  120
 19  \w   -123.00 -85.00   0.50    0.24    -- -106.00 -37.00-180.00   76
 20  \w   -116.00 -71.00   0.50    0.24    -- -106.00 125.00-180.00   90
 21  \w   -177.00-102.00   0.50    0.24    -- -106.00-125.00-150.00  150
 22  \w   -143.00 -83.00   0.50    0.24    -- -106.00 -99.00-180.00  120
 23  \w   -116.00 -90.00   0.50    0.24    -- -106.00 -37.00   0.00   52
 24  \w   -175.00-144.00   0.50    0.24    -- -106.00 -37.00   0.00   62
 25  \w   -109.00 -32.00   0.50    0.24    -- -106.00 125.00  30.00  154
 26  \w   -116.00 -49.00   0.50    0.24    -- -106.00 125.00 -90.00  134
 27  \w   -176.00-132.00   0.50    0.24    -- -106.00 -99.00 150.00   88
 28  \w   -112.00 -87.00   0.50    0.24    -- -106.00 -99.00 150.00   50
 29  \w    -82.00 -33.00   0.50    0.24    -- -106.00  77.00-150.00   98
 30  \w   -117.00 -33.00   0.50    0.24    -- -106.00 125.00   0.00  168
 31  \w    -59.00 -33.00   0.50    0.24    -- -106.00 125.00-180.00   52
 32  \w   -135.00 -91.00   0.50    0.24    -- -106.00  77.00-150.00   88
 33  \w    -97.00 -71.00   0.50    0.24    -- -106.00-125.00-150.00   52
 34  \w   -134.00 -32.00   0.50    0.24    -- -106.00  77.00 -90.00  204
 35  \w   -128.00-103.00   0.50    0.24    -- -106.00  37.00  60.00   50
 36  \w    -67.00 -41.00   0.50    0.24    -- -106.00  37.00  60.00   52
 37  \w   -176.00 -91.00   0.50    0.24    -- -106.00 -37.00  30.00  170
;
_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      0.0021248000
_diffrn_orient_matrix_UB_12      -0.0627489000
_diffrn_orient_matrix_UB_13      -0.0683025000
_diffrn_orient_matrix_UB_21      0.0351964000
_diffrn_orient_matrix_UB_22      0.1064528000
_diffrn_orient_matrix_UB_23      -0.0206626000
_diffrn_orient_matrix_UB_31      0.1522682000
_diffrn_orient_matrix_UB_32      0.0240089000
_diffrn_orient_matrix_UB_33      0.0245348000
_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  0.0416
_diffrn_reflns_av_unetI/netI     0.0415
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       25
_diffrn_reflns_limit_l_min       -25
_diffrn_reflns_number            31944
_diffrn_reflns_theta_full        68.2494
_diffrn_reflns_theta_max         68.25
_diffrn_reflns_theta_min         3.65
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'PhotonJet (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    1.722
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.86417
_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    1.2534
_exptl_crystal_description       block
_exptl_crystal_F_000             1081.2734
_exptl_crystal_size_max          0.3
_exptl_crystal_size_mid          0.2
_exptl_crystal_size_min          0.1
_refine_diff_density_max         0.6995
_refine_diff_density_min         -0.4367
_refine_diff_density_rms         0.0642
_refine_ls_d_res_high            0.8300
_refine_ls_d_res_low             12.1077
_refine_ls_goodness_of_fit_ref   1.0271
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_constraints    68
_refine_ls_number_parameters     617
_refine_ls_number_reflns         10211
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.0271
_refine_ls_R_factor_all          0.0456
_refine_ls_R_factor_gt           0.0426
_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^)+(0.0743P)^2^+1.1343P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1218
_refine_ls_wR_factor_ref         0.1247
_reflns_Friedel_coverage         0.0
_reflns_limit_h_max              12
_reflns_limit_h_min              -12
_reflns_limit_k_max              15
_reflns_limit_k_min              -16
_reflns_limit_l_max              25
_reflns_limit_l_min              0
_reflns_number_gt                9170
_reflns_number_total             10211
_reflns_threshold_expression     I>=2u(I)
_cod_data_source_file            ja0c03252_si_002.cif
_cod_data_source_block           2b
_cod_depositor_comments
'Adding full bibliography for 4134972--4134984.cif.'
_cod_database_code               4134974
_chemical_oxdiff_formula         'C45 H49 Al1 Cu1 F15 N2 O2 P1'
_reflns_odcompleteness_completeness 99.94
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     68.13
_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:
 C23(H23), C26(H26)
2.b Secondary CH2 refined with riding coordinates:
 C9(H9a,H9b), C10(H10a,H10b)
2.c Aromatic/amide H refined with riding coordinates:
 C4(H4), C6(H6), C5(H5)
2.d Idealised Me refined as rotating group:
 C15(H15a,H15b,H15c), C25(H25a,H25b,H25c), C24(H24a,H24b,H24c), C20(H20a,H20b,
 H20c), C18(H18a,H18b,H18c), C19(H19a,H19b,H19c), C16(H16a,H16b,H16c), C65(H65a,
 H65b,H65c), C21(H21a,H21b,H21c), C66(H66a,H66b,H66c), C67(H67a,H67b,H67c),
 C28(H28a,H28b,H28c), C27(H27a,H27b,H27c)
;
_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 1.668
_oxdiff_exptl_absorpt_empirical_full_min 0.605