Activation of H2 over the Ru-Zn Bond in the Transition Metal-Lewis Acid Heterobimetallic Species [Ru(IPr)2(CO)ZnEt](.).
Riddlestone, Ian M.; Rajabi, Nasir A.; Lowe, John P.; Mahon, Mary F.; Macgregor, Stuart A.; Whittlesey, Michael K.; Journal of the American Chemical Society 138 (2016) 11081–11084; doi:10.1021/jacs.6b05243

data_4130618
_publ_section_title
;
 Activation of H2 over the Ru-Zn Bond in the Transition Metal-Lewis Acid
 Heterobimetallic Species [Ru(IPr)2(CO)ZnEt](.).
;
_journal_issue                   35
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              11081
_journal_page_last               11084
_journal_paper_doi               10.1021/jacs.6b05243
_journal_volume                  138
_journal_year                    2016
_chemical_formula_moiety         'C57 H77 N4 O Ru Zn, C32 H12 B F24'
_chemical_formula_sum            'C89 H89 B F24 N4 O Ru Zn'
_chemical_formula_weight         1863.89
_space_group_crystal_system      monoclinic
_space_group_IT_number           7
_space_group_name_Hall           'P -2yac'
_space_group_name_H-M_alt        'P 1 n 1'
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     iterative
_audit_creation_date             2015-09-08
_audit_creation_method
;
Olex2 1.2
(compiled 2015.01.26 svn.r3150 for OlexSys, GUI svn.r4998)
;
_cell_angle_alpha                90
_cell_angle_beta                 102.080(3)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   12.5594(4)
_cell_length_b                   17.4038(5)
_cell_length_c                   20.1905(6)
_cell_measurement_reflns_used    10911
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      26.1300
_cell_measurement_theta_min      3.7240
_cell_volume                     4315.5(2)
_computing_cell_refinement
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.33 (release 27-03-2014 CrysAlis171 .NET)
(compiled Mar 27 2014,17:12:48)
;
_computing_data_collection
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.33 (release 27-03-2014 CrysAlis171 .NET)
(compiled Mar 27 2014,17:12:48)
;
_computing_data_reduction
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.33 (release 27-03-2014 CrysAlis171 .NET)
(compiled Mar 27 2014,17:12:48)
;
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'XH (Sheldrick, 2008)'
_computing_structure_solution    'olex2.solve (Bourhis et al., 2015)'
_diffrn_ambient_temperature      150.15
_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 0.998
_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  0.0367
_diffrn_reflns_av_unetI/netI     0.0621
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       21
_diffrn_reflns_limit_k_min       -21
_diffrn_reflns_limit_l_max       25
_diffrn_reflns_limit_l_min       -24
_diffrn_reflns_number            35480
_diffrn_reflns_point_group_measured_fraction_full 0.944
_diffrn_reflns_point_group_measured_fraction_max 0.936
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         26.371
_diffrn_reflns_theta_min         3.318
_diffrn_source                   'Enhance (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    0.553
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.97615
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.33 (release 27-03-2014 CrysAlis171 .NET)
(compiled Mar 27 2014,17:12:48)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            orange
_exptl_crystal_density_diffrn    1.434
_exptl_crystal_description       block
_exptl_crystal_F_000             1908
_exptl_crystal_size_max          0.2227
_exptl_crystal_size_mid          0.1731
_exptl_crystal_size_min          0.1096
_refine_diff_density_max         0.611
_refine_diff_density_min         -0.407
_refine_diff_density_rms         0.060
_refine_ls_abs_structure_details
;
 Flack x determined using 5631 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   -0.011(6)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.026
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1145
_refine_ls_number_reflns         16525
_refine_ls_number_restraints     56
_refine_ls_restrained_S_all      1.035
_refine_ls_R_factor_all          0.0533
_refine_ls_R_factor_gt           0.0420
_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^)+(0.0277P)^2^+1.0041P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0740
_refine_ls_wR_factor_ref         0.0783
_reflns_Friedel_coverage         0.874
_reflns_Friedel_fraction_full    0.889
_reflns_Friedel_fraction_max     0.874
_reflns_number_gt                14469
_reflns_number_total             16525
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ja6b05243_si_002.cif
_cod_data_source_block           e15mkw5
_cod_database_code               4130618
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Restrained distances
 C65-F4 \\sim C65-F5 \\sim C65-F6 \\sim C65-F4A \\sim C65-F5A \\sim C65-F6A
 with sigma of 0.005
 H27a-C27 \\sim H27b-C27 \\sim H27c-C27
 with sigma of 0.005
3. Uiso/Uaniso restraints and constraints
Uanis(F4) \\sim Ueq, Uanis(F4A) \\sim Ueq, Uanis(F5) \\sim Ueq, Uanis(F5A)
\\sim Ueq, Uanis(F6) \\sim Ueq, Uanis(F6A) \\sim Ueq: with sigma of 0.005 and
sigma for terminal atoms of 0.01
4. Others
 Fixed Sof: F4(0.65) F5(0.65) F6(0.65) F4A(0.35) F5A(0.35) F6A(0.35)
5.a Ternary CH refined with riding coordinates:
 C10(H10), C13(H13), C22(H22), C25(H25), C37(H37), C40(H40), C49(H49), C52(H52)
5.b Secondary CH2 refined with riding coordinates:
 C56(H56a,H56b)
5.c Aromatic/amide H refined with riding coordinates:
 C2(H2), C3(H3), C6(H6), C7(H7), C8(H8), C18(H18), C19(H19), C20(H20),
 C29(H29), C30(H30), C33(H33), C34(H34), C35(H35), C45(H45), C46(H46), C47(H47),
  C59(H59), C61(H61), C63(H63), C67(H67), C69(H69), C71(H71), C75(H75),
 C77(H77), C79(H79), C83(H83), C85(H85), C87(H87)
5.d Idealised Me refined as rotating group:
 C11(H11a,H11b,H11c), C12(H12a,H12b,H12c), C14(H14a,H14b,H14c), C15(H15a,H15b,
 H15c), C23(H23a,H23b,H23c), C24(H24a,H24b,H24c), C26(H26a,H26b,H26c), C38(H38a,
 H38b,H38c), C39(H39a,H39b,H39c), C41(H41a,H41b,H41c), C42(H42a,H42b,H42c),
 C50(H50a,H50b,H50c), C51(H51a,H51b,H51c), C53(H53a,H53b,H53c), C54(H54a,H54b,
 H54c), C57(H57a,H57b,H57c)
;
_shelx_shelxl_version_number     2014/7
_olex2_submission_special_instructions 'No special instructions were received'