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_4134975
_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         'C39 H34 Al Cu F15 N2 O2 P'
_chemical_formula_sum            'C39 H34 Al Cu F15 N2 O2 P'
_chemical_formula_weight         969.19
_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             2019-09-24
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_cell_angle_alpha                90
_cell_angle_beta                 104.524(2)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   12.4894(2)
_cell_length_b                   19.8533(3)
_cell_length_c                   19.8687(4)
_cell_measurement_reflns_used    15839
_cell_measurement_temperature    123.15
_cell_measurement_theta_max      74.1810
_cell_measurement_theta_min      3.8200
_cell_volume                     4769.12(15)
_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 0.9909
_diffrn_measured_fraction_theta_max 0.9909
_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    -71.00  15.00   0.50    0.05    --  -42.80  75.00 -69.00  172
  2  \w    -24.00  21.00   0.50    0.05    --   42.80 -75.00 162.00   90
  3  \w      3.00  50.00   0.50    0.16    --   76.50 -75.00 162.00   94
  4  \w   -118.00 -84.00   0.50    0.16    -- -106.00 -75.00 162.00   68
  5  \w   -129.00 -32.00   0.50    0.16    -- -106.00  75.00 -69.00  194
  6  \w   -159.00-127.00   0.50    0.16    -- -106.00 -75.00 162.00   64
  7  \w   -112.00 -14.00   0.50    0.05    --  -42.80 -77.00 120.00  196
  8  \w     58.00 101.00   0.50    0.05    --   42.80  75.00 -69.00   86
  9  \w     71.00 116.00   0.50    0.05    --   42.80 125.00 150.00   90
 10  \w   -115.00 -32.00   0.50    0.16    -- -106.00 125.00 -60.00  166
 11  \w   -110.00 -84.00   0.50    0.16    -- -106.00  19.00   0.00   52
 12  \w   -176.00 -82.00   0.50    0.16    -- -106.00 -77.00-180.00  188
 13  \w   -142.00 -76.00   0.50    0.16    -- -106.00 -19.00   0.00  132
 14  \w   -117.00 -84.00   0.50    0.16    -- -106.00 -99.00  90.00   66
 15  \w   -153.00-127.00   0.50    0.16    -- -106.00 -99.00  90.00   52
 16  \w   -156.00-126.00   0.50    0.16    -- -106.00 -37.00   0.00   60
 17  \w   -113.00 -85.00   0.50    0.16    -- -106.00 -37.00   0.00   56
 18  \w   -116.00 -91.00   0.50    0.16    -- -106.00 125.00-150.00   50
 19  \w    -60.00 -35.00   0.50    0.16    -- -106.00 125.00-150.00   50
 20  \w   -173.00 -83.00   0.50    0.16    -- -106.00 -99.00-120.00  180
;
_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      -0.1049809000
_diffrn_orient_matrix_UB_12      -0.0439480000
_diffrn_orient_matrix_UB_13      -0.0187013000
_diffrn_orient_matrix_UB_21      0.0551533000
_diffrn_orient_matrix_UB_22      -0.0463879000
_diffrn_orient_matrix_UB_23      -0.0435171000
_diffrn_orient_matrix_UB_31      0.0465991000
_diffrn_orient_matrix_UB_32      -0.0440419000
_diffrn_orient_matrix_UB_33      0.0646206000
_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  0.0539
_diffrn_reflns_av_unetI/netI     0.0449
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       23
_diffrn_reflns_limit_k_min       -23
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            27496
_diffrn_reflns_theta_full        68.2508
_diffrn_reflns_theta_max         68.25
_diffrn_reflns_theta_min         3.80
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'PhotonJet (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    1.973
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.86766
_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            yellow
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    1.3497
_exptl_crystal_description       block
_exptl_crystal_F_000             1962.1091
_exptl_crystal_size_max          0.3
_exptl_crystal_size_mid          0.2
_exptl_crystal_size_min          0.2
_refine_diff_density_max         0.4615
_refine_diff_density_min         -0.5667
_refine_diff_density_rms         0.0773
_refine_ls_d_res_high            0.8300
_refine_ls_d_res_low             11.6347
_refine_ls_goodness_of_fit_ref   1.0194
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_constraints    50
_refine_ls_number_parameters     559
_refine_ls_number_reflns         8643
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.0194
_refine_ls_R_factor_all          0.0513
_refine_ls_R_factor_gt           0.0463
_refine_ls_shift/su_max          0.0002
_refine_ls_shift/su_mean         0.0000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0816P)^2^+2.2792P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1293
_refine_ls_wR_factor_ref         0.1347
_reflns_Friedel_coverage         0.0
_reflns_limit_h_max              11
_reflns_limit_h_min              -15
_reflns_limit_k_max              23
_reflns_limit_k_min              0
_reflns_limit_l_max              23
_reflns_limit_l_min              -10
_reflns_number_gt                7562
_reflns_number_total             8643
_reflns_threshold_expression     I>=2u(I)
_cod_data_source_file            ja0c03252_si_002.cif
_cod_data_source_block           2c
_cod_depositor_comments
'Adding full bibliography for 4134972--4134984.cif.'
_cod_original_sg_symbol_Hall     '-P 2ybc (x-z,y,z)'
_cod_database_code               4134975
_chemical_oxdiff_formula         'C39 H34 Al1 Cu1 F15 N2 O2 P1'
_reflns_odcompleteness_completeness 99.09
_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 Aromatic/amide H refined with riding coordinates:
 C3(H3), C7(H7), C9(H9), C8(H8), C4(H4), C6(H6), C5(H5)
3.b Idealised Me refined as rotating group:
 C20(H20a,H20b,H20c), C18(H18a,H18b,H18c), C15(H15a,H15b,H15c), C16(H16a,H16b,
 H16c), C19(H19a,H19b,H19c), C21(H21a,H21b,H21c), C59(H59a,H59b,H59c), C60(H60a,
 H60b,H60c), C61(H61a,H61b,H61c)
;
_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 3.312
_oxdiff_exptl_absorpt_empirical_full_min 0.707