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_4134453
_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         'C56 H50 P3 Ru Zn2, C32 H12 B F24'
_chemical_formula_sum            'C88 H62 B F24 P3 Ru Zn2'
_chemical_formula_weight         1910.90
_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   geom
_atom_sites_solution_primary     iterative
_audit_creation_date             2018-08-20
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_cell_angle_alpha                90.385(2)
_cell_angle_beta                 99.080(3)
_cell_angle_gamma                104.878(2)
_cell_formula_units_Z            2
_cell_length_a                   13.4442(4)
_cell_length_b                   17.6572(5)
_cell_length_c                   18.2564(5)
_cell_measurement_reflns_used    13064
_cell_measurement_temperature    150.00(10)
_cell_measurement_theta_max      29.2160
_cell_measurement_theta_min      3.7000
_cell_volume                     4131.0(2)
_computing_cell_refinement       'CrysAlisPro 1.171.39.46 (Rigaku OD, 2018)'
_computing_data_collection       'CrysAlisPro 1.171.39.46 (Rigaku OD, 2018)'
_computing_data_reduction        'CrysAlisPro 1.171.39.46 (Rigaku OD, 2018)'
_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      150.00(10)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 16.1468
_diffrn_detector_type            EosS2
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.845
_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  0.0267
_diffrn_reflns_av_unetI/netI     0.0483
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.845
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       24
_diffrn_reflns_limit_k_min       -23
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_number            41802
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.845
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         29.451
_diffrn_reflns_theta_min         3.372
_diffrn_source                   'fine-focus sealed X-ray tube'
_diffrn_source_type              'Enhance (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    0.914
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.97186
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.39.46 (Rigaku Oxford Diffraction, 2018)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            'dark orange'
_exptl_crystal_colour_modifier   dark
_exptl_crystal_colour_primary    orange
_exptl_crystal_density_diffrn    1.536
_exptl_crystal_description       block
_exptl_crystal_F_000             1920
_exptl_crystal_size_max          0.575
_exptl_crystal_size_mid          0.306
_exptl_crystal_size_min          0.202
_refine_diff_density_max         0.820
_refine_diff_density_min         -0.642
_refine_diff_density_rms         0.074
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.025
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1155
_refine_ls_number_reflns         19367
_refine_ls_number_restraints     153
_refine_ls_restrained_S_all      1.066
_refine_ls_R_factor_all          0.0627
_refine_ls_R_factor_gt           0.0395
_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^)+(0.0360P)^2^+3.1182P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0837
_refine_ls_wR_factor_ref         0.0947
_reflns_Friedel_coverage         0.000
_reflns_number_gt                14710
_reflns_number_total             19367
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ja0c01062_si_002.cif
_cod_data_source_block           e18mkw8
_cod_depositor_comments
'Adding full bibliography for 4134447--4134453.cif.'
_cod_database_code               4134453
_shelxl_version_number           2014-3
_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
 F4-C82 \\sim F6A-C82 \\sim F6-C82 \\sim F5A-C82 \\sim F5-C82 \\sim F4A-C82
 with sigma of 0.005
 F16-F17 \\sim F16-F18 \\sim F17-F18
 with sigma of 0.02
 C86-F16 \\sim C86-F17 \\sim C86-F18 \\sim C86-C73
 with sigma of 0.02
 F16-C86 \\sim F16A-C86
 with sigma of 0.02
 F17-C86 \\sim F17A-C86
 with sigma of 0.02
 F18-C86 \\sim F18A-C86
 with sigma of 0.02
 F16-C86 \\sim F17B-C86
 with sigma of 0.02
 F17-C86 \\sim F18B-C86
 with sigma of 0.02
 F18-C86 \\sim F16B-C86
 with sigma of 0.02
3. Rigid body (RIGU) restrains
 C82, F4A, F6A, F5A
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 C82, F4, F5, F6
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 F16B, F17B, F18B, C86, F17A, F18, F16A, F16, F18A, F17
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
4. Others
 Fixed Sof: F16B(0.3) F17B(0.3) F18B(0.3) F4A(0.4) F17A(0.2) F6A(0.4) F4(0.6)
 F18(0.5) F5(0.6) F5A(0.4) F6(0.6) F16A(0.2) F16(0.5) F18A(0.2) F17(0.5)
5.a Aromatic/amide H refined with riding coordinates:
 C4(H4), C5(H5), C6(H6), C7(H7), C10(H10), C11(H11), C12(H12), C13(H13),
 C14(H14), C16(H16), C17(H17), C18(H18), C19(H19), C20(H20), C22(H22), C23(H23),
  C24(H24), C25(H25), C26(H26), C28(H28), C29(H29), C30(H30), C31(H31),
 C32(H32), C34(H34), C35(H35), C36(H36), C37(H37), C38(H38), C40(H40), C41(H41),
  C42(H42), C43(H43), C44(H44), C46(H46), C47(H47), C48(H48), C49(H49),
 C50(H50), C52(H52), C53(H53), C54(H54), C55(H55), C56(H56), C58(H58), C60(H60),
  C62(H62), C64(H64), C66(H66), C68(H68), C70(H70), C72(H72), C74(H74),
 C76(H76), C78(H78), C80(H80)
5.b Idealised Me refined as rotating group:
 C1(H1A,H1B,H1C), C2(H2A,H2B,H2C)
;