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_4134984
_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_absolute_configuration unk
_chemical_formula_moiety         'Br6 Cu4, C34 H50 Al Br N4 O2 P2, 2(C6 H6)'
_chemical_formula_sum            'C46 H62 Al Br7 Cu4 N4 O2 P2'
_chemical_formula_weight         1605.47
_space_group_crystal_system      monoclinic
_space_group_IT_number           4
_space_group_name_Hall           'P 2yb'
_space_group_name_H-M_alt        'P 1 21 1'
_symmetry_Int_Tables_number      4
_atom_sites_solution_primary     dual
_audit_creation_date             2019-10-07
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_cell_angle_alpha                90
_cell_angle_beta                 91.8940(10)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   12.64470(10)
_cell_length_b                   17.08400(10)
_cell_length_c                   13.26670(10)
_cell_measurement_reflns_used    60943
_cell_measurement_temperature    123.15
_cell_measurement_theta_max      76.9360
_cell_measurement_theta_min      3.4920
_cell_volume                     2864.33(4)
_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 0.9978
_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     29.00  55.00   0.50    1.68    --   49.59  77.00 -90.00   52
  2  \w     38.00  64.00   0.50    1.68    --   60.00  80.00-100.69   52
  3  \w     47.00  79.00   0.50    1.68    --   66.50  77.00-103.03   64
  4  \w     85.00 121.00   0.50    1.68    --   49.59  77.00 -90.00   72
  5  \w     74.00  99.00   0.50    1.68    --   49.59 140.00 -38.00   50
  6  \w     75.00 100.00   0.50    1.68    --   66.50 140.00 -38.00   50
  7  \w    103.00 128.00   0.50    1.68    --   56.00  77.00  23.72   50
  8  \w     71.00  96.00   0.50    1.68    --   49.59 129.00 148.00   50
  9  \w     45.00  71.00   0.50    1.68    --   66.50  79.00 -74.64   52
 10  \w     46.00  73.00   0.50    1.68    --   66.50  77.00 -30.00   54
 11  \w     46.00  95.00   0.50    1.68    --   66.50  77.00   0.00   98
 12  \w     45.00  73.00   0.50    1.68    --   66.50  79.00  70.18   56
 13  \w     47.00  81.00   0.50    1.68    --   66.50  77.00  90.00   68
 14  \w     79.00 104.00   0.50    1.68    --   66.50 129.00 148.00   50
 15  \w     36.00  92.00   0.50    1.68    --   56.00  79.00 167.01  112
 16  \w     36.00  75.00   0.50    1.68    --   56.00  75.00 131.26   78
 17  \w     46.00  72.00   0.50    1.68    --   66.50  77.00 150.00   52
 18  \w     46.00  76.00   0.50    1.68    --   66.50  77.00 120.00   60
 19  \w     46.00  71.00   0.50    1.68    --   66.50  77.00 176.14   50
 20  \w     30.00  62.00   0.50    1.68    --   52.00  81.00  88.28   64
 21  \w     33.00  59.00   0.50    1.68    --   56.00  82.00 136.26   52
 22  \w     11.00  36.00   0.50    1.68    --   40.00  94.00 120.49   50
 23  \w      2.00  27.00   0.50    1.68    --   32.00  96.00  31.04   50
 24  \w     30.00  62.00   0.50    1.68    --   52.00  83.00  46.26   64
 25  \w     48.00  79.00   0.50    1.68    --   66.50  77.00  30.00   62
 26  \w     35.00  61.00   0.50    1.68    --   56.00  77.00  23.72   52
 27  \w     46.00  73.00   0.50    1.68    --   66.50  78.00  45.93   54
 28  \w     33.00  80.00   0.50    1.68    --   56.00  82.00 -22.02   94
 29  \w     47.00  73.00   0.50    1.68    --   66.50  77.00 -60.00   52
 30  \w     47.00  74.00   0.50    1.68    --   66.50  77.00-139.74   54
 31  \w     44.00  70.00   0.50    1.68    --   64.00  75.00-163.81   52
 32  \w     44.00  76.00   0.50    1.68    --   66.50  82.00-168.92   64
 33  \w     19.00  45.00   0.50    1.68    --   44.00  89.00-140.97   52
 34  \w     -4.00  28.00   0.50    1.68    --   24.00  97.00 -51.38   64
 35  \w     17.00  42.00   0.50    1.68    --   44.00  91.00 -47.48   50
 36  \w    -14.00  19.00   0.50    1.68    --   16.00  99.00-139.38   66
 37  \w    -35.00  -7.00   0.50    1.68    --    8.00 120.00-126.64   56
 38  \w    -16.00  10.00   0.50    1.68    --   16.00 102.00   9.68   52
 39  \w    -17.00  15.00   0.50    1.68    --   16.00 102.00 114.52   64
 40  \w    -57.00 -32.00   0.50    1.68    --  -53.09 129.00 148.00   50
 41  \w   -112.00 -35.00   0.50    1.68    -- -105.75 125.00 120.00  154
 42  \w    -81.00 -54.00   0.50    1.68    --  -53.09 140.00 -38.00   54
 43  \w   -106.00 -61.00   0.50    1.68    -- -105.75 125.00  30.00   90
 44  \w    -83.00 -35.00   0.50    1.68    -- -105.75 125.00 -30.00   96
 45  \w   -104.00 -34.00   0.50    1.68    -- -105.75  37.00-150.00  140
 46  \w    -82.00 -56.00   0.50    1.68    --  -76.00 -75.00-172.84   52
 47  \w    -83.00 -57.00   0.50    1.68    --  -80.00 -82.00-119.35   52
 48  \w    -85.00 -58.00   0.50    1.68    --  -80.00 -82.00 -85.28   54
 49  \w    -80.00 -54.00   0.50    1.68    --  -76.00 -82.00 -44.57   52
 50  \w    -89.00 -54.00   0.50    1.68    --  -76.00 -79.00-108.40   70
 51  \w    -90.00 -57.00   0.50    1.68    --  -80.00 -83.00 -55.19   66
 52  \w    -87.00 -61.00   0.50    1.68    --  -84.00 -82.00   1.17   52
 53  \w   -101.00 -75.00   0.50    1.68    --  -53.09-129.00  75.00   52
 54  \w   -100.00 -57.00   0.50    1.68    --  -80.00 -82.00 100.78   86
 55  \w    -87.00 -53.00   0.50    1.68    --  -76.00 -83.00 176.84   68
 56  \w    -91.00 -64.00   0.50    1.68    --  -84.00 -74.00 141.70   54
 57  \w    -95.00 -69.00   0.50    1.68    --  -92.00 -83.00 148.36   52
 58  \w    -90.00 -64.00   0.50    1.68    --  -84.00 -74.00  70.91   52
 59  \w    -94.00 -65.00   0.50    1.68    --  -84.00 -72.00  32.02   58
 60  \w    -94.00 -68.00   0.50    1.68    --  -88.00 -74.00  65.57   52
 61  \w   -107.00 -68.00   0.50    1.68    --  -88.00 -75.00   9.08   78
 62  \w    -90.00 -64.00   0.50    1.68    --  -84.00 -74.00 -75.79   52
 63  \w    -99.00 -69.00   0.50    1.68    --  -88.00 -72.00 -95.24   60
 64  \w   -101.00 -75.00   0.50    1.68    --  -92.00 -73.00-105.34   52
 65  \w   -104.00 -75.00   0.50    1.68    --  -96.00 -77.00 -44.96   58
 66  \w   -105.00 -79.00   0.50    1.68    --  -96.00 -67.00 -37.57   52
 67  \w   -100.00 -72.00   0.50    1.68    --  -92.00 -74.00  37.13   56
 68  \w   -107.00 -76.00   0.50    1.68    --  -92.00 -66.00 107.05   62
 69  \w   -104.00 -73.00   0.50    1.68    --  -92.00 -72.00 167.85   62
 70  \w   -123.00 -84.00   0.50    1.68    -- -105.75-129.00  75.00   78
 71  \w   -104.00 -72.00   0.50    1.68    --  -92.00 -74.00  61.74   64
 72  \w   -115.00 -77.00   0.50    1.68    --  -92.00 -63.00  78.02   76
 73  \w   -118.00 -76.00   0.50    1.68    --  -96.00 -75.00  59.36   84
 74  \w   -146.00-120.00   0.50    1.68    --  -92.00 -66.00 107.05   52
 75  \w   -137.00 -76.00   0.50    1.68    --  -92.00 -66.00 155.12  122
 76  \w   -159.00 -68.00   0.50    1.68    --  -88.00 -74.00  20.72  182
 77  \w   -100.00 -74.00   0.50    1.68    --  -53.09-140.00 -97.00   52
 78  \w   -108.00 -77.00   0.50    1.68    -- -105.75-140.00 -97.00   62
 79  \w   -135.00 -75.00   0.50    1.68    --  -92.00 -68.00-127.05  120
 80  \w   -158.00-114.00   0.50    1.68    --  -88.00 -72.00 -95.24   88
 81  \w   -159.00 -65.00   0.50    1.68    --  -88.00 -82.00-156.17  188
 82  \w   -163.00 -72.00   0.50    1.68    --  -92.00 -74.00-170.61  182
 83  \w   -163.00 -72.00   0.50    1.68    --  -92.00 -74.00-133.25  182
 84  \w   -163.00 -72.00   0.50    1.68    --  -92.00 -76.00  -0.77  182
 85  \w   -152.00 -73.00   0.50    1.68    --  -92.00 -72.00 153.63  158
 86  \w   -160.00-107.00   0.50    1.68    --  -88.00 -74.00  65.57  106
 87  \w   -162.00-120.00   0.50    1.68    --  -92.00 -83.00 148.36   84
 88  \w   -162.00-131.00   0.50    1.68    --  -92.00 -63.00  78.02   62
 89  \w   -158.00 -75.00   0.50    1.68    --  -96.00 -77.00 137.31  166
 90  \w   -165.00 -79.00   0.50    1.68    --  -96.00 -67.00 102.12  172
 91  \w   -168.00 -80.00   0.50    1.68    --  -96.00 -66.00 -20.56  176
 92  \w   -167.00-124.00   0.50    1.68    --  -96.00 -75.00  59.36   86
 93  \w   -176.00-116.00   0.50    1.68    -- -105.75 -99.00  90.00  120
 94  \w   -171.00 -83.00   0.50    1.68    -- -105.75 -81.00 -56.65  176
 95  \w   -174.00 -85.00   0.50    1.68    -- -105.75 -76.00 -77.99  178
 96  \w   -108.00 -47.00   0.50    1.68    -- -105.75  57.00-180.00  122
 97  \w   -126.00 -62.00   0.50    1.68    -- -105.75 140.00 -38.00  128
 98  \w   -125.00 -43.00   0.50    1.68    -- -105.75  77.00   0.00  164
 99  \w   -117.00 -46.00   0.50    1.68    -- -105.75  57.00   0.00  142
100  \w   -119.00 -56.00   0.50    1.68    -- -105.75 129.00 148.00  126
101  \w     24.00  93.00   0.50    1.68    --   49.59-129.00  75.00  138
102  \w     39.00  64.00   0.50    1.68    --   66.50-129.00  75.00   50
103  \w     37.00  62.00   0.50    1.68    --   49.59-140.00 -97.00   50
104  \w     59.00 113.00   0.50    1.68    --   66.50-140.00 -97.00  108
;
_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      0.1127643000
_diffrn_orient_matrix_UB_12      -0.0331365000
_diffrn_orient_matrix_UB_13      0.0148144000
_diffrn_orient_matrix_UB_21      0.0440546000
_diffrn_orient_matrix_UB_22      0.0838069000
_diffrn_orient_matrix_UB_23      0.0102482000
_diffrn_orient_matrix_UB_31      -0.0144778000
_diffrn_orient_matrix_UB_32      -0.0031603000
_diffrn_orient_matrix_UB_33      0.1147540000
_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  0.0369
_diffrn_reflns_av_unetI/netI     0.0147
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_number            92905
_diffrn_reflns_theta_full        68.2503
_diffrn_reflns_theta_max         68.25
_diffrn_reflns_theta_min         3.50
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'PhotonJet (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    8.374
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.57440
_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            orange
_exptl_crystal_colour_primary    orange
_exptl_crystal_density_diffrn    1.8613
_exptl_crystal_description       block
_exptl_crystal_F_000             1550.5747
_exptl_crystal_size_max          0.1
_exptl_crystal_size_mid          0.1
_exptl_crystal_size_min          0.1
_refine_diff_density_max         0.3604
_refine_diff_density_min         -0.8349
_refine_diff_density_rms         0.0631
_refine_ls_abs_structure_details
'Flack, H. D. (1983). Acta Cryst. A39, 876-881.'
_refine_ls_abs_structure_Flack   0.016(10)
_refine_ls_d_res_high            0.8300
_refine_ls_d_res_low             12.6378
_refine_ls_goodness_of_fit_ref   1.0429
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_constraints    100
_refine_ls_number_parameters     607
_refine_ls_number_reflns         10450
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.0429
_refine_ls_R_factor_all          0.0240
_refine_ls_R_factor_gt           0.0235
_refine_ls_shift/su_max          0.0010
_refine_ls_shift/su_mean         0.0000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0449P)^2^+1.4409P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0627
_refine_ls_wR_factor_ref         0.0635
_reflns_Friedel_coverage         0.998
_reflns_limit_h_max              15
_reflns_limit_h_min              -15
_reflns_limit_k_max              20
_reflns_limit_k_min              -20
_reflns_limit_l_max              15
_reflns_limit_l_min              -15
_reflns_number_gt                10285
_reflns_number_total             10450
_reflns_threshold_expression     I>=2u(I)
_cod_data_source_file            ja0c03252_si_002.cif
_cod_data_source_block           15c
_cod_depositor_comments
'Adding full bibliography for 4134972--4134984.cif.'
_cod_original_sg_symbol_Hall     ' P 2yb'
_cod_database_code               4134984
_chemical_oxdiff_formula         'C21 H34 Cu1 Br3 P1 O2 Al1 N2'
_reflns_odcompleteness_completeness 99.96
_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:
 C11(H11), C10(H10), C18(H18), C23(H23), C55(H55), C17(H17), C26(H26),
 C38(H38), C41(H41), C25(H25), C24(H24), C58(H58), C56(H56), C27(H27), C42(H42),
  C59(H59), C57(H57), C39(H39), C40(H40), C61(H61), C60(H60), C63(H63),
 C64(H64), C62(H62), C65(H65), C66(H66)
3.b Idealised Me refined as rotating group:
 C44(H44a,H44b,H44c), C48(H48a,H48b,H48c), C49(H49a,H49b,H49c), C46(H46a,H46b,
 H46c), C35(H35a,H35b,H35c), C30(H30a,H30b,H30c), C32(H32a,H32b,H32c), C45(H45a,
 H45b,H45c), C31(H31a,H31b,H31c), C50(H50a,H50b,H50c), C36(H36a,H36b,H36c),
 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 2.005
_oxdiff_exptl_absorpt_empirical_full_min 0.656