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_4134980
_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 H35 Al F15 N2 O P'
_chemical_formula_sum            'C39 H35 Al F15 N2 O P'
_chemical_formula_weight         890.65
_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             2019-06-27
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_cell_angle_alpha                70.363(2)
_cell_angle_beta                 79.054(2)
_cell_angle_gamma                89.263(2)
_cell_formula_units_Z            4
_cell_length_a                   11.6018(2)
_cell_length_b                   19.0189(4)
_cell_length_c                   19.6291(4)
_cell_measurement_reflns_used    28203
_cell_measurement_temperature    123.15
_cell_measurement_theta_max      74.0950
_cell_measurement_theta_min      3.8730
_cell_volume                     3999.03(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 0.9986
_diffrn_measured_fraction_theta_max 0.9986
_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   -118.00 -21.00   0.50    0.20    --  -42.80 -45.00 -78.00  194
  2  \w    -61.00  33.00   0.50    0.20    --  -42.80  45.00  71.00  188
  3  \w     41.00  68.00   0.50    0.20    --   42.80  45.00  71.00   54
  4  \w     26.00  51.00   0.50    0.50    --   76.50 -45.00 -78.00   50
  5  \w     79.00 104.00   0.50    0.50    --   76.50  45.00  71.00   50
  6  \w   -172.00-105.00   0.50    0.50    -- -106.00 -45.00 -78.00  134
  7  \w    -72.00 -32.00   0.50    0.50    -- -106.00  45.00  71.00   80
  8  \w   -113.00 -87.00   0.50    0.50    -- -106.00  45.00  71.00   52
  9  \w    -36.00 -11.00   0.50    0.20    --  -42.80 125.00  90.00   50
 10  \w    -93.00 -21.00   0.50    0.20    --  -42.80 125.00-150.00  144
 11  \w    -88.00 -55.00   0.50    0.20    --  -42.80 125.00  90.00   66
 12  \w     71.00 118.00   0.50    0.20    --   42.80  45.00  71.00   94
 13  \w    -32.00  26.00   0.50    0.20    --   42.80 -45.00 -78.00  116
 14  \w     71.00 115.00   0.50    0.20    --   42.80 125.00-180.00   88
 15  \w      2.00  81.00   0.50    0.50    --   76.50 -57.00 120.00  158
 16  \w      2.00 105.00   0.50    0.50    --   76.50 -99.00  60.00  206
 17  \w   -117.00 -57.00   0.50    0.50    -- -106.00 125.00 -60.00  120
 18  \w   -174.00 -75.00   0.50    0.50    -- -106.00 -19.00  60.00  198
 19  \w   -117.00 -45.00   0.50    0.50    -- -106.00 125.00-120.00  144
 20  \w   -103.00 -45.00   0.50    0.50    -- -106.00  57.00-120.00  116
 21  \w   -134.00 -34.00   0.50    0.50    -- -106.00  77.00-120.00  200
 22  \w   -177.00-152.00   0.50    0.50    -- -106.00 -77.00 -30.00   50
 23  \w   -173.00 -76.00   0.50    0.50    -- -106.00 -19.00 150.00  194
 24  \w   -114.00 -40.00   0.50    0.50    -- -106.00 125.00  60.00  148
 25  \w   -120.00 -94.00   0.50    0.50    -- -106.00 -37.00 120.00   52
 26  \w    -97.00 -32.00   0.50    0.50    -- -106.00  77.00  60.00  130
 27  \w   -175.00-110.00   0.50    0.50    -- -106.00-125.00-120.00  130
 28  \w   -174.00-127.00   0.50    0.50    -- -106.00 -37.00 120.00   94
 29  \w    -81.00 -56.00   0.50    0.50    -- -106.00 125.00   0.00   50
 30  \w   -133.00-105.00   0.50    0.50    -- -106.00  77.00  60.00   56
 31  \w   -112.00 -87.00   0.50    0.50    -- -106.00 125.00-150.00   50
 32  \w    -58.00 -32.00   0.50    0.50    -- -106.00 125.00-150.00   52
 33  \w   -117.00 -85.00   0.50    0.50    -- -106.00 125.00  90.00   64
 34  \w   -171.00 -84.00   0.50    0.50    -- -106.00 -99.00-180.00  174
 35  \w   -113.00 -29.00   0.50    0.50    -- -106.00  19.00 -60.00  168
;
_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      0.0954110000
_diffrn_orient_matrix_UB_12      -0.0199220000
_diffrn_orient_matrix_UB_13      0.0472845000
_diffrn_orient_matrix_UB_21      -0.0016331000
_diffrn_orient_matrix_UB_22      -0.0799515000
_diffrn_orient_matrix_UB_23      -0.0028197000
_diffrn_orient_matrix_UB_31      0.0961331000
_diffrn_orient_matrix_UB_32      0.0251001000
_diffrn_orient_matrix_UB_33      -0.0705734000
_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  0.0276
_diffrn_reflns_av_unetI/netI     0.0270
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       23
_diffrn_reflns_limit_k_min       -23
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_limit_l_min       -24
_diffrn_reflns_number            50106
_diffrn_reflns_theta_full        68.2450
_diffrn_reflns_theta_max         68.24
_diffrn_reflns_theta_min         3.89
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'PhotonJet (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    1.775
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.86812
_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    1.4792
_exptl_crystal_description       block
_exptl_crystal_F_000             1825.8225
_exptl_crystal_size_max          0.3
_exptl_crystal_size_mid          0.3
_exptl_crystal_size_min          0.2
_refine_diff_density_max         0.4541
_refine_diff_density_min         -0.4924
_refine_diff_density_rms         0.0470
_refine_ls_d_res_high            0.8300
_refine_ls_d_res_low             11.3734
_refine_ls_goodness_of_fit_ref   1.0450
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_constraints    100
_refine_ls_number_parameters     1083
_refine_ls_number_reflns         14593
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.0450
_refine_ls_R_factor_all          0.0374
_refine_ls_R_factor_gt           0.0334
_refine_ls_shift/su_max          0.0000
_refine_ls_shift/su_mean         0.0000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0398P)^2^+1.7863P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0870
_refine_ls_wR_factor_ref         0.0894
_reflns_Friedel_coverage         0.0
_reflns_limit_h_max              13
_reflns_limit_h_min              -13
_reflns_limit_k_max              22
_reflns_limit_k_min              -21
_reflns_limit_l_max              23
_reflns_limit_l_min              0
_reflns_number_gt                13097
_reflns_number_total             14593
_reflns_threshold_expression     I>=2u(I)
_cod_data_source_file            ja0c03252_si_002.cif
_cod_data_source_block           5b
_cod_depositor_comments
;
Adding full bibliography for 4134972--4134984.cif.

2025-07-29
Z value and formula fixed to values more according to usual
chemical conventions.                 miguel
;
_cod_original_formula_sum            'C78 H70 Al2 F30 N4 O2 P2'
_cod_original_formula_weight         1781.31
_cod_original_formula_moiety         '2(C39 H35 Al F15 N2 O P)'
_cod_original_formula_units_Z            2
_cod_database_code               4134980
_chemical_oxdiff_formula         'C156 H144 Al4 F60 N8 O4 P4 '
_reflns_odcompleteness_completeness 99.94
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     66.97
_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.a Ternary CH refined with riding coordinates:
 C48(H48), C45(H45), C20(H20), C23(H23)
2.b Aromatic/amide H refined with riding coordinates:
 C30(H30), C28(H28), C29(H29), C5(H5), C3(H3), C4(H4)
2.c Idealised Me refined as rotating group:
 C17(H17a,H17b,H17c), C42(H42a,H42b,H42c), C18(H18a,H18b,H18c), C13(H13a,H13b,
 H13c), C12(H12a,H12b,H12c), C50(H50a,H50b,H50c), C15(H15a,H15b,H15c), C43(H43a,
 H43b,H43c), C40(H40a,H40b,H40c), C16(H16a,H16b,H16c), C41(H41a,H41b,H41c),
 C38(H38a,H38b,H38c), C49(H49a,H49b,H49c), C37(H37a,H37b,H37c), C47(H47a,H47b,
 H47c), C46(H46a,H46b,H46c), C25(H25a,H25b,H25c), C24(H24a,H24b,H24c), C22(H22a,
 H22b,H22c), C21(H21a,H21b,H21c)
;
_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 1.272
_oxdiff_exptl_absorpt_empirical_full_min 0.774