Heterobimetallic ruthenium-zinc complexes with bulky N-heterocyclic carbenes: syntheses, structures and reactivity.
Espinal-Viguri, Maialen; Varela-Izquierdo, Victor; Miloserdov, Fedor M.; Riddlestone, Ian M.; Mahon, Mary F.; Whittlesey, Michael K.; Dalton transactions (Cambridge, England : 2003) 48 (2019) 4176–4189; doi:10.1039/c8dt05023f

data_7049056
_publ_section_title
;
 Heterobimetallic ruthenium-zinc complexes with bulky N-heterocyclic
 carbenes: syntheses, structures and reactivity.
;
_journal_issue                   13
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              4176
_journal_page_last               4189
_journal_paper_doi               10.1039/c8dt05023f
_journal_volume                  48
_journal_year                    2019
_chemical_formula_moiety         'C56 H79 N4 O Ru Zn, C32 H12 B F24'
_chemical_formula_sum            'C88 H91 B F24 N4 O Ru Zn'
_chemical_formula_weight         1853.89
_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_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     iterative
_audit_creation_date             2018-07-12
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_audit_update_record
;
2018-11-30 deposited with the CCDC.    2019-02-19 downloaded from the CCDC.
;
_cell_angle_alpha                84.0630(10)
_cell_angle_beta                 88.7670(10)
_cell_angle_gamma                85.4020(10)
_cell_formula_units_Z            2
_cell_length_a                   12.7837(2)
_cell_length_b                   17.1267(3)
_cell_length_c                   20.4172(3)
_cell_measurement_reflns_used    44335
_cell_measurement_temperature    150.01(10)
_cell_measurement_theta_max      30.3960
_cell_measurement_theta_min      2.9260
_cell_volume                     4431.51(12)
_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      150.01(10)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 8.1150
_diffrn_detector_type            EosS2
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.986
_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           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0629
_diffrn_reflns_av_unetI/netI     0.0430
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.986
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_h_min       -18
_diffrn_reflns_limit_k_max       24
_diffrn_reflns_limit_k_min       -24
_diffrn_reflns_limit_l_max       28
_diffrn_reflns_limit_l_min       -29
_diffrn_reflns_number            159961
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.986
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         30.508
_diffrn_reflns_theta_min         2.582
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    0.538
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.63416
_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            colourless
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.389
_exptl_crystal_description       block
_exptl_crystal_F_000             1900
_exptl_crystal_size_max          0.317
_exptl_crystal_size_mid          0.132
_exptl_crystal_size_min          0.103
_refine_diff_density_max         0.755
_refine_diff_density_min         -1.176
_refine_diff_density_rms         0.091
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.042
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1267
_refine_ls_number_reflns         26703
_refine_ls_number_restraints     157
_refine_ls_restrained_S_all      1.065
_refine_ls_R_factor_all          0.0694
_refine_ls_R_factor_gt           0.0503
_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^)+(0.0550P)^2^+3.8737P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1188
_refine_ls_wR_factor_ref         0.1298
_reflns_Friedel_coverage         0.000
_reflns_number_gt                21382
_reflns_number_total             26703
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c8dt05023f2.cif
_cod_data_source_block           s18mkw11
_cod_depositor_comments
'Adding full bibliography for 7049052--7049061.cif.'
_cod_database_code               7049056
_shelx_shelxl_version_number     2014/7
_chemical_oxdiff_usercomment     'colorless block'
_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
 H1-H2
 0.75 with sigma of 0.01
 F10-C64 \\sim F10A-C64
 with sigma of 0.02
 F11-C64 \\sim F11A-C64
 with sigma of 0.02
 F12-C64 \\sim F12A-C64
 with sigma of 0.02
 F13-C71 \\sim F13A-C71A
 with sigma of 0.02
 F14-C71 \\sim F14A-C71A
 with sigma of 0.02
 F15-C71 \\sim F15A-C71A
 with sigma of 0.02
 C67-C71 \\sim C67-C71A
 with sigma of 0.02
 F13-F14 \\sim F13A-F14A
 with sigma of 0.04
 F13-F15 \\sim F13A-F15A
 with sigma of 0.04
 F13-C67 \\sim F13A-C67
 with sigma of 0.04
 F14-F15 \\sim F14A-F15A
 with sigma of 0.04
 F14-C67 \\sim F14A-C67
 with sigma of 0.04
 F15-C67 \\sim F15A-C67
 with sigma of 0.04
 F19-C80 \\sim F19A-C80A
 with sigma of 0.02
 F20-C80 \\sim F20A-C80A
 with sigma of 0.02
 F21-C80 \\sim F21A-C80A
 with sigma of 0.02
 C77-C80 \\sim C77-C80A
 with sigma of 0.02
 F19-F20 \\sim F19A-F20A
 with sigma of 0.04
 F19-F21 \\sim F19A-F21A
 with sigma of 0.04
 F19-C77 \\sim F19A-C77
 with sigma of 0.04
 F20-F21 \\sim F20A-F21A
 with sigma of 0.04
 F20-C77 \\sim F20A-C77
 with sigma of 0.04
 F21-C77 \\sim F21A-C77
 with sigma of 0.04
 F2-C88 \\sim F1A-C88 \\sim F1-C88 \\sim F3A-C88 \\sim F2A-C88 \\sim F3-C88
 with sigma of 0.005
 F7-C63 \\sim F7A-C63
 with sigma of 0.02
 F8-C63 \\sim F8A-C63
 with sigma of 0.02
 F9-C63 \\sim F9A-C63
 with sigma of 0.02
 Ru1-H2 \\sim Ru1-H1
 with sigma of 0.02
3. Uiso/Uaniso restraints and constraints
F19 \\sim F20 \\sim F21 \\sim C80: within 2A with sigma of 0.02 and sigma for
terminal atoms of 0.01
F19A \\sim F21A \\sim C80A \\sim F20A: within 2A with sigma of 0.02 and sigma
for terminal atoms of 0.01
F1 \\sim F3A \\sim F3 \\sim F2A \\sim F2 \\sim F1A: within 2A with sigma of
0.02 and sigma for terminal atoms of 0.01
F11A \\sim F11 \\sim F12A \\sim F12 \\sim F10A \\sim F10: within 2A with sigma
of 0.02 and sigma for terminal atoms of 0.01
4. Others
 Fixed Sof: F1(0.75) F2(0.75) F3(0.75) F7(0.5) F8(0.5) F9(0.5) F10(0.5)
 F11(0.5) F12(0.5) F13(0.7) F14(0.7) F15(0.7) F19(0.55) F20(0.55) F21(0.55)
 C71(0.7) C80(0.55) F11A(0.5) F12A(0.5) F10A(0.5) F14A(0.3) C71A(0.3) F13A(0.3)
 F15A(0.3) F19A(0.45) F21A(0.45) C80A(0.45) F20A(0.45) F2A(0.25) F3A(0.25)
 F1A(0.25) F9A(0.5) F7A(0.5) F8A(0.5)
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 Aromatic/amide H refined with riding coordinates:
 C2(H0AA), C3(H1AA), 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),
  C58(H58), C60(H60), C62(H62), C66(H66), C68(H68), C70(H70), C74(H74),
 C76(H76), C78(H78), C82(H82), C84(H84), C86(H86)
5.c 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), C27(H27A,
 H27B,H27C), 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), C56(H56A,H56B,H56C)
;
_olex2_submission_special_instructions 'No special instructions were received'