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_4134449
_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         'C63 H63 Mg O2 P3 Ru'
_chemical_formula_sum            'C63 H63 Mg O2 P3 Ru'
_chemical_formula_weight         1070.42
_space_group_crystal_system      monoclinic
_space_group_IT_number           15
_space_group_name_Hall           '-C 2yc'
_space_group_name_H-M_alt        'C 1 2/c 1'
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     iterative
_audit_creation_date             2018-10-13
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_cell_angle_alpha                90
_cell_angle_beta                 99.0450(10)
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   41.0356(5)
_cell_length_b                   13.7554(2)
_cell_length_c                   19.4148(2)
_cell_measurement_reflns_used    27291
_cell_measurement_temperature    200.00(10)
_cell_measurement_theta_max      73.0190
_cell_measurement_theta_min      4.2010
_cell_volume                     10822.6(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      200.00(10)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 8.1150
_diffrn_detector_type            EosS2
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.993
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at home/near, EosS2'
_diffrn_measurement_method       '\w scans'
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0630
_diffrn_reflns_av_unetI/netI     0.0362
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.993
_diffrn_reflns_limit_h_max       50
_diffrn_reflns_limit_h_min       -50
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_number            81094
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.993
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         73.538
_diffrn_reflns_theta_min         3.393
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    3.627
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.65439
_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            'light yellow'
_exptl_crystal_colour_modifier   light
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    1.314
_exptl_crystal_description       block
_exptl_crystal_F_000             4464
_exptl_crystal_size_max          0.193
_exptl_crystal_size_mid          0.118
_exptl_crystal_size_min          0.058
_refine_diff_density_max         0.588
_refine_diff_density_min         -0.557
_refine_diff_density_rms         0.052
_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     663
_refine_ls_number_reflns         10832
_refine_ls_number_restraints     7
_refine_ls_restrained_S_all      1.028
_refine_ls_R_factor_all          0.0414
_refine_ls_R_factor_gt           0.0316
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0345P)^2^+5.3043P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0715
_refine_ls_wR_factor_ref         0.0756
_reflns_Friedel_coverage         0.000
_reflns_number_gt                9152
_reflns_number_total             10832
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ja0c01062_si_002.cif
_cod_data_source_block           s18mkw32
_cod_depositor_comments
'Adding full bibliography for 4134447--4134453.cif.'
_cod_database_code               4134449
_shelxl_version_number           2014-3
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups, All C(H,H,H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Restrained distances
 O2-C62 \\sim O2-C62A
 with sigma of 0.02
 C59-C60 \\sim C59-C60A
 with sigma of 0.02
 C62-C61 \\sim C62A-C61A
 with sigma of 0.02
 C60-C61 \\sim C60A-C61A
 with sigma of 0.02
 O2-C61 \\sim O2-C61A
 with sigma of 0.02
 C59-C61 \\sim C59-C61A
 with sigma of 0.02
 C62-C60 \\sim C62A-C60A
 with sigma of 0.02
3. Others
 Fixed Sof: H59C(0.4) H59D(0.4) H59A(0.6) H59B(0.6) C60(0.6) H60A(0.6)
 H60B(0.6) C61(0.6) H61A(0.6) H61B(0.6) C62(0.6) H62A(0.6) H62B(0.6) C60A(0.4)
 H60C(0.4) H60D(0.4) C61A(0.4) H61C(0.4) H61D(0.4) C62A(0.4) H62C(0.4) H62D(0.4)
4.a Secondary CH2 refined with riding coordinates:
 C55(H55A,H55B), C56(H56A,H56B), C57(H57A,H57B), C58(H58A,H58B), C59(H59C,
 H59D), C59(H59A,H59B), C60(H60A,H60B), C61(H61A,H61B), C62(H62A,H62B),
 C60A(H60C,H60D), C61A(H61C,H61D), C62A(H62C,H62D)
4.b Aromatic/amide H refined with riding coordinates:
 C2(H2), C3(H3), C4(H4), C5(H5), C8(H8), C9(H9), C10(H10), C11(H11), C12(H12),
 C14(H14), C15(H15), C16(H16), C17(H17), C18(H18), C21(H21), C22(H22), C23(H23),
  C24(H24), C26(H26), C27(H27), C28(H28), C29(H29), C30(H30), C32(H32),
 C33(H33), C34(H34), C35(H35), C36(H36), C38(H38), C39(H39), C40(H40), C41(H41),
  C42(H42), C44(H44), C45(H45), C46(H46), C47(H47), C48(H48), C50(H50),
 C51(H51), C52(H52), C53(H53), C54(H54)
4.c Idealised Me refined as rotating group:
 C63(H63A,H63B,H63C)
;