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_7049054
_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
'C39 H57 N4 O6 Ru, 2(C3 H2.5 F0.5), C32 H12 B F24'
_chemical_formula_sum            'C77 H74 B F25 N4 O6 Ru'
_chemical_formula_weight         1738.28
_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             2017-09-09
_audit_creation_method
;
Olex2 1.2
(compiled 2017.08.10 svn.r3458 for OlexSys, GUI svn.r5381)
;
_audit_update_record
;
2018-11-30 deposited with the CCDC.    2019-02-19 downloaded from the CCDC.
;
_cell_angle_alpha                87.261(3)
_cell_angle_beta                 80.381(2)
_cell_angle_gamma                75.276(2)
_cell_formula_units_Z            2
_cell_length_a                   14.9600(4)
_cell_length_b                   15.8674(5)
_cell_length_c                   16.5741(5)
_cell_measurement_reflns_used    12562
_cell_measurement_temperature    150.00(10)
_cell_measurement_theta_max      28.2120
_cell_measurement_theta_min      3.7750
_cell_volume                     3751.5(2)
_computing_cell_refinement       'CrysAlisPro 1.171.38.46 (Rigaku OD, 2015)'
_computing_data_collection       'CrysAlisPro 1.171.38.46 (Rigaku OD, 2015)'
_computing_data_reduction        'CrysAlisPro 1.171.38.46 (Rigaku OD, 2015)'
_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 0.997
_diffrn_measured_fraction_theta_max 0.975
_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  0.0392
_diffrn_reflns_av_unetI/netI     0.0566
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.975
_diffrn_reflns_limit_h_max       19
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            46082
_diffrn_reflns_point_group_measured_fraction_full 0.997
_diffrn_reflns_point_group_measured_fraction_max 0.975
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.484
_diffrn_reflns_theta_min         3.435
_diffrn_source                   'fine-focus sealed X-ray tube'
_diffrn_source_type              'Enhance (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    0.327
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.91123
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.38.46 (Rigaku Oxford Diffraction, 2015)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            yellow-orange
_exptl_crystal_density_diffrn    1.539
_exptl_crystal_description       block
_exptl_crystal_F_000             1772
_exptl_crystal_size_max          0.56
_exptl_crystal_size_mid          0.542
_exptl_crystal_size_min          0.434
_refine_diff_density_max         2.798
_refine_diff_density_min         -0.678
_refine_diff_density_rms         0.090
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.063
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1188
_refine_ls_number_reflns         16803
_refine_ls_number_restraints     334
_refine_ls_restrained_S_all      1.123
_refine_ls_R_factor_all          0.0813
_refine_ls_R_factor_gt           0.0617
_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^)+(0.0503P)^2^+9.5828P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1407
_refine_ls_wR_factor_ref         0.1516
_reflns_Friedel_coverage         0.000
_reflns_number_gt                13369
_reflns_number_total             16803
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c8dt05023f2.cif
_cod_data_source_block           e17mkw36
_cod_depositor_comments
'Adding full bibliography for 7049052--7049061.cif.'
_cod_database_code               7049054
_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
2. Restrained distances
 Ru1-H1 = Ru1-H1A
 1.6 with sigma of 0.005
 O4-C22A \\sim O4-C22
 with sigma of 0.005
 C23-C22A \\sim C23-C22
 with sigma of 0.005
 F14-F13 \\sim F14-F15 \\sim F13-F15 \\sim F15A-F13A \\sim F15A-F14A \\sim
F13A-F14A
 with sigma of 0.04
 C70-F14 \\sim C70-F13 \\sim C70-F15 \\sim C70-F15A \\sim C70-F13A \\sim
C70-F14A
 with sigma of 0.02
 F11-F10 \\sim F11-F12 \\sim F10-F12 \\sim F11A-F12A \\sim F11A-F10A \\sim
F12A-F10A
 with sigma of 0.04
 C55-F11 \\sim C55-F10 \\sim C55-F12 \\sim C55-F11A \\sim C55-F12A \\sim
C55-F10A
 with sigma of 0.01
 F7-F9 \\sim F7-F8 \\sim F9-F8 \\sim F8A-F9A \\sim F8A-F7A \\sim F9A-F7A
 with sigma of 0.04
 C54-F7 \\sim C54-F9 \\sim C54-F8 \\sim C54-F8A \\sim C54-F9A \\sim C54-F7A
 with sigma of 0.01
 F19-F21 \\sim F19-F20 \\sim F21-F20 \\sim F20A-F19A \\sim F20A-F21A \\sim
F19A-F21A
 with sigma of 0.04
 C63-F19 \\sim C63-F21 \\sim C63-F20 \\sim C63-F20A \\sim C63-F19A \\sim
C63-F21A
 with sigma of 0.01
 F1-F2 \\sim F1-F3 \\sim F2-F3 \\sim F1A-F2A \\sim F1A-F3A \\sim F2A-F3A
 with sigma of 0.04
 C46-F1 \\sim C46-F2 \\sim C46-F1A \\sim C46-F3 \\sim C46-F2A \\sim C46-F3A
 with sigma of 0.01
3. Uiso/Uaniso restraints and constraints
F13 \\sim F14 \\sim F15 \\sim F13A \\sim F14A \\sim F15A: within 2A with sigma
of 0.02 and sigma for terminal atoms of 0.01
F10 \\sim F11 \\sim F12 \\sim F10A \\sim F11A \\sim F12A: within 2A with sigma
of 0.02 and sigma for terminal atoms of 0.01
F19 \\sim F20 \\sim F21 \\sim F19A \\sim F20A \\sim F21A: within 2A with sigma
of 0.02 and sigma for terminal atoms of 0.01
F1 \\sim F2 \\sim F3 \\sim F1A \\sim F2A \\sim F3A: within 2A with sigma of
0.02 and sigma for terminal atoms of 0.01
F7 \\sim F8 \\sim F9 \\sim F7A \\sim F8A \\sim F9A: within 2A with sigma of
0.02 and sigma for terminal atoms of 0.01
4. Others
 Fixed Sof: H1(0.5) H1A(0.5) C22(0.75) H22A(0.75) H22B(0.75) C22A(0.25)
 H22C(0.25) H22D(0.25) F25(0.5) H76(0.5) F1(0.65) F2(0.65) F3(0.65) F7(0.55)
 F8(0.55) F9(0.55) F10(0.5) F11(0.5) F12(0.5) F13(0.75) F14(0.75) F15(0.75)
 F19(0.75) F20(0.75) F21(0.75) F1A(0.35) F2A(0.35) F3A(0.35) F7A(0.45)
 F8A(0.45) F9A(0.45) F10A(0.5) F11A(0.5) F12A(0.5) F13A(0.25) F14A(0.25)
 F15A(0.25) F19A(0.25) F20A(0.25) F21A(0.25) F26(0.5) H74(0.5)
5.a Secondary CH2 refined with riding coordinates:
 C5(H5A,H5B), C7(H7A,H7B), C8(H8A,H8B), C9(H9A,H9B), C10(H10A,H10B), C11(H11A,
 H11B), C12(H12A,H12B), C14(H14A,H14B), C15(H15A,H15B), C16(H16A,H16B),
 C17(H17A,H17B), C18(H18A,H18B), C24(H24A,H24B), C25(H25A,H25B), C26(H26A,H26B),
  C27(H27A,H27B), C28(H28A,H28B), C29(H29A,H29B), C31(H31A,H31B), C32(H32A,
 H32B), C33(H33A,H33B), C34(H34A,H34B), C35(H35A,H35B), C36(H36A,H36B),
 C37(H37A,H37B), C38(H38A,H38B), C39(H39A,H39B), C22(H22A,H22B), C22A(H22C,H22D)
5.b Aromatic/amide H refined with riding coordinates:
 C75(H75), C76(H76), C77(H77), C41(H41), C43(H43), C45(H45), C49(H49),
 C51(H51), C53(H53), C57(H57), C59(H59), C61(H61), C65(H65), C67(H67), C69(H69),
  C72(H72), C73(H73), C74(H74)
;
_olex2_submission_special_instructions 'No special instructions were received'