Zn-Promoted C-H Reductive Elimination and H<sub>2</sub> Activation via a Dual Unsaturated Heterobimetallic Ru-Zn Intermediate.
Miloserdov, Fedor M.; Rajabi, Nasir A.; Lowe, John P.; Mahon, Mary F.; Macgregor, Stuart A.; Whittlesey, Michael K.; Journal of the American Chemical Society 142 (2020) 6340–6349; doi:10.1021/jacs.0c01062

data_4134452
_publ_section_title
;
 Zn-Promoted C-H Reductive Elimination and H<sub>2</sub> Activation via a
 Dual Unsaturated Heterobimetallic Ru-Zn Intermediate.
;
_journal_issue                   13
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              6340
_journal_page_last               6349
_journal_paper_doi               10.1021/jacs.0c01062
_journal_volume                  142
_journal_year                    2020
_chemical_formula_moiety         'C55 H47 P3 Ru Zn'
_chemical_formula_sum            'C55 H47 P3 Ru Zn'
_chemical_formula_weight         967.27
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     iterative
_audit_creation_date             2019-06-28
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_cell_angle_alpha                85.312(3)
_cell_angle_beta                 73.891(3)
_cell_angle_gamma                72.861(3)
_cell_formula_units_Z            2
_cell_length_a                   11.2221(3)
_cell_length_b                   13.0503(4)
_cell_length_c                   16.6725(5)
_cell_measurement_reflns_used    9898
_cell_measurement_temperature    150.00(10)
_cell_measurement_theta_max      30.0140
_cell_measurement_theta_min      3.5880
_cell_volume                     2241.67(12)
_computing_cell_refinement       'CrysAlisPro 1.171.40.57a (Rigaku OD, 2019)'
_computing_data_collection       'CrysAlisPro 1.171.40.57a (Rigaku OD, 2019)'
_computing_data_reduction        'CrysAlisPro 1.171.40.57a (Rigaku OD, 2019)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_computing_structure_solution    'olex2.solve (Bourhis et al., 2015)'
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      150.01(10)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 8.0734
_diffrn_detector_type            EosS2
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.851
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'New Xcalibur, EosS2'
_diffrn_measurement_method       '\w scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0244
_diffrn_reflns_av_unetI/netI     0.0467
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.851
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            21853
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.851
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         30.279
_diffrn_reflns_theta_min         3.367
_diffrn_source                   'fine-focus sealed X-ray tube'
_diffrn_source_type              'Enhance (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    1.016
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.93150
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.40.57a (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    1.433
_exptl_crystal_description       block
_exptl_crystal_F_000             992
_exptl_crystal_size_max          0.643
_exptl_crystal_size_mid          0.389
_exptl_crystal_size_min          0.231
_refine_diff_density_max         0.484
_refine_diff_density_min         -0.454
_refine_diff_density_rms         0.077
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.025
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     576
_refine_ls_number_reflns         11418
_refine_ls_number_restraints     25
_refine_ls_restrained_S_all      1.024
_refine_ls_R_factor_all          0.0456
_refine_ls_R_factor_gt           0.0330
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0244P)^2^+1.1468P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0676
_refine_ls_wR_factor_ref         0.0727
_reflns_Friedel_coverage         0.000
_reflns_number_gt                9487
_reflns_number_total             11418
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ja0c01062_si_002.cif
_cod_data_source_block           e19mkw30
_cod_depositor_comments
'Adding full bibliography for 4134447--4134453.cif.'
_cod_database_code               4134452
_shelx_shelxl_version_number     2014/7
_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
 P3-C50A \\sim P3-C50B
 with sigma of 0.02
3. Rigid bond restraints
 C50A, C51A, C52A, C53A, C54A, C55A
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
 C50B, C51B, C52B, C53B, C54B, C55B
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
4. Others
 Fixed Sof: C50A(0.55) C51A(0.55) H51A(0.55) C52A(0.55) H52A(0.55) C53A(0.55)
 H53A(0.55) C54A(0.55) H54A(0.55) C55A(0.55) H55A(0.55) C50B(0.45) C51B(0.45)
 H51B(0.45) C52B(0.45) H52B(0.45) C53B(0.45) H53B(0.45) C54B(0.45) H54B(0.45)
 C55B(0.45) H55B(0.45)
5.a Aromatic/amide H refined with riding coordinates:
 C4(H4), C5(H5), C6(H6), C7(H7), C9(H9), C10(H10), C11(H11), C12(H12),
 C13(H13), C15(H15), C16(H16), C17(H17), C18(H18), C19(H19), C21(H21), C22(H22),
  C23(H23), C24(H24), C27(H27), C28(H28), C29(H29), C30(H30), C31(H31),
 C33(H33), C34(H34), C35(H35), C36(H36), C37(H37), C39(H39), C40(H40), C41(H41),
  C42(H42), C43(H43), C45(H45), C46(H46), C47(H47), C48(H48), C49(H49),
 C51A(H51A), C52A(H52A), C53A(H53A), C54A(H54A), C55A(H55A), C51B(H51B),
 C52B(H52B), C53B(H53B), C54B(H54B), C55B(H55B)
5.b Fitted hexagon refined as free rotating group:
 C50A(C51A,C52A,C53A,C54A,C55A), C50B(C51B,C52B,C53B,C54B,C55B)
5.c Idealised Me refined as rotating group:
 C1(H1A,H1B,H1C)
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