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_7049055
_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 H77 N4 O Ru Zn, C H2 Cl2, C32 H12 B F24'
_chemical_formula_sum            'C89 H91 B Cl2 F24 N4 O Ru Zn'
_chemical_formula_weight         1936.80
_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             2017-07-01
_audit_creation_method
;
Olex2 1.2
(compiled 2017.03.28 svn.r3405 for OlexSys, GUI svn.r5337)
;
_audit_update_record
;
2018-11-30 deposited with the CCDC.    2019-02-19 downloaded from the CCDC.
;
_cell_angle_alpha                95.885(2)
_cell_angle_beta                 94.337(2)
_cell_angle_gamma                98.208(2)
_cell_formula_units_Z            2
_cell_length_a                   13.1638(4)
_cell_length_b                   17.7078(6)
_cell_length_c                   19.6253(6)
_cell_measurement_reflns_used    14279
_cell_measurement_temperature    150.00(10)
_cell_measurement_theta_max      28.3710
_cell_measurement_theta_min      3.6910
_cell_volume                     4485.0(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 8.0734
_diffrn_detector_type            EosS2
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.962
_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  0.0362
_diffrn_reflns_av_unetI/netI     0.0594
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.962
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       -22
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -24
_diffrn_reflns_number            40172
_diffrn_reflns_point_group_measured_fraction_full 0.997
_diffrn_reflns_point_group_measured_fraction_max 0.962
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.484
_diffrn_reflns_theta_min         3.397
_diffrn_source                   'fine-focus sealed X-ray tube'
_diffrn_source_type              'Enhance (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    0.593
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.94537
_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            'pale yellow'
_exptl_crystal_density_diffrn    1.434
_exptl_crystal_description       block
_exptl_crystal_F_000             1980
_exptl_crystal_size_max          0.577
_exptl_crystal_size_mid          0.493
_exptl_crystal_size_min          0.41
_refine_diff_density_max         0.876
_refine_diff_density_min         -0.566
_refine_diff_density_rms         0.073
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.037
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1246
_refine_ls_number_reflns         19792
_refine_ls_number_restraints     240
_refine_ls_restrained_S_all      1.059
_refine_ls_R_factor_all          0.0675
_refine_ls_R_factor_gt           0.0467
_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^)+(0.0431P)^2^+2.8838P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1017
_refine_ls_wR_factor_ref         0.1136
_reflns_Friedel_coverage         0.000
_reflns_number_gt                15414
_reflns_number_total             19792
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c8dt05023f2.cif
_cod_data_source_block           e17mkw19
_cod_depositor_comments
'Adding full bibliography for 7049052--7049061.cif.'
_cod_database_code               7049055
_shelxl_version_number           2014-3
_chemical_oxdiff_usercomment     'Yellow block'
_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
 C26-H26A = C26-H26B = C26-H26C
 0.98 with sigma of 0.005
 F1-F2 \\sim F1-F3 \\sim F2-F3 \\sim F2A-F3A \\sim F2A-F1A \\sim F3A-F1A
 with sigma of 0.02
 C79-F13 \\sim C79-F14 \\sim C79-F15 \\sim C79-F13A \\sim C79-F15A \\sim
C79-F14A
 with sigma of 0.01
 Cl00-C89 \\sim Cl-C89A \\sim Cl1A-C89A \\sim Cl1-C89
 with sigma of 0.005
 C79-F14B \\sim C79-F13 \\sim C79-F15A \\sim C79-F13B \\sim C79-F14A \\sim
C79-F14 \\sim C79-F15 \\sim C79-
 F13A \\sim C79-F15B
 with sigma of 0.01
 F13-F14 \\sim F14-F15 \\sim F15-F13 \\sim F13A-F14A \\sim F14A-F15A \\sim
F15A-F13A \\sim F13B-F14B ~
 F14B-F15B \\sim F15B-F13B
 with sigma of 0.02
3. Uiso/Uaniso restraints and constraints
F1 \\sim F1 \\sim F2 \\sim F2 \\sim F3 \\sim F3 \\sim F1A \\sim F1A \\sim F2A
\\sim F2A \\sim F3A \\sim F3A: within 2A with sigma of 0.02 and sigma for
terminal atoms of 0.01
F13 \\sim F14 \\sim F15 \\sim F13A \\sim F14A \\sim F15A \\sim F13B \\sim F14B
\\sim F15B: within 2A with sigma of 0.02 and sigma for terminal atoms of 0.01
Uanis(C89A) = Uanis(C89)
4. Others
 Fixed Sof: Cl(0.45) Cl1A(0.45) C89A(0.45) H89C(0.45) H89D(0.45) Cl00(0.55)
 Cl1(0.55) C89(0.55) H89A(0.55) H89B(0.55) F1(0.75) F2(0.75) F3(0.75) F13(0.5)
 F14(0.5) F15(0.5) F1A(0.25) F2A(0.25) F3A(0.25) F13A(0.4) F14A(0.4) F15A(0.4)
 F13B(0.1) F14B(0.1) F15B(0.1)
5.a Ternary CH refined with riding coordinates:
 C12(H12), C15(H15), C24(H24), C27(H27), C39(H39), C42(H42), C51(H51), C54(H54)
5.b Secondary CH2 refined with riding coordinates:
 C89A(H89C,H89D), C89(H89A,H89B)
5.c Aromatic/amide H refined with riding coordinates:
 C4(H4), C5(H5), C8(H8), C9(H9), C10(H10), C20(H20), C21(H21), C22(H22),
 C31(H31), C32(H32), C35(H35), C36(H36), C37(H37), C47(H47), C48(H48), C49(H49),
  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.d Idealised Me refined as rotating group:
 C2(H2A,H2B,H2C), C13(H13A,H13B,H13C), C14(H14A,H14B,H14C), C16(H16A,H16B,
 H16C), C17(H17A,H17B,H17C), C25(H25A,H25B,H25C), C28(H28A,H28B,H28C), C29(H29A,
 H29B,H29C), C40(H40A,H40B,H40C), C41(H41A,H41B,H41C), C43(H43A,H43B,H43C),
 C44(H44A,H44B,H44C), C52(H52A,H52B,H52C), C53(H53A,H53B,H53C), C55(H55A,H55B,
 H55C), C56(H56A,H56B,H56C)
;
_olex2_submission_special_instructions 'No special instructions were received'