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_7049060
_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         'C40 H59 N4 O6 Ru Zn, C32 H12 B F24'
_chemical_formula_sum            'C72 H71 B F24 N4 O6 Ru Zn'
_chemical_formula_weight         1721.57
_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   geom
_atom_sites_solution_primary     iterative
_audit_creation_date             2017-09-15
_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                94.981(3)
_cell_angle_beta                 91.296(3)
_cell_angle_gamma                97.163(3)
_cell_formula_units_Z            2
_cell_length_a                   12.9608(4)
_cell_length_b                   13.1449(4)
_cell_length_c                   21.6148(7)
_cell_measurement_reflns_used    13920
_cell_measurement_temperature    150.00(11)
_cell_measurement_theta_max      30.0410
_cell_measurement_theta_min      3.5840
_cell_volume                     3637.9(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(11)
_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  0.0262
_diffrn_reflns_av_unetI/netI     0.0439
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       28
_diffrn_reflns_limit_l_min       -27
_diffrn_reflns_number            33375
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.483
_diffrn_reflns_theta_min         3.339
_diffrn_source                   'fine-focus sealed X-ray tube'
_diffrn_source_type              'Enhance (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    0.654
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.92875
_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            orange-yellow
_exptl_crystal_density_diffrn    1.572
_exptl_crystal_description       block
_exptl_crystal_F_000             1748
_exptl_crystal_size_max          0.561
_exptl_crystal_size_mid          0.375
_exptl_crystal_size_min          0.27
_refine_diff_density_max         0.982
_refine_diff_density_min         -0.647
_refine_diff_density_rms         0.077
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.027
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1097
_refine_ls_number_reflns         16641
_refine_ls_number_restraints     264
_refine_ls_restrained_S_all      1.117
_refine_ls_R_factor_all          0.0580
_refine_ls_R_factor_gt           0.0441
_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^)+(0.0405P)^2^+5.5931P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1015
_refine_ls_wR_factor_ref         0.1096
_reflns_Friedel_coverage         0.000
_reflns_number_gt                13744
_reflns_number_total             16641
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c8dt05023f2.cif
_cod_data_source_block           e17mkw39
_cod_depositor_comments
'Adding full bibliography for 7049052--7049061.cif.'
_cod_original_cell_volume        3637.8(2)
_cod_database_code               7049060
_shelx_shelxl_version_number     2014/7
_chemical_oxdiff_usercomment     'yellow-orange block'
_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
 F18-F16 \\sim F18-F17 \\sim F16-F17 \\sim F17A-F16A \\sim F17A-F18A \\sim
F16A-F18A
 with sigma of 0.02
 C72-F18 \\sim C72-F16 \\sim C72-F17 \\sim C72-F17A \\sim C72-F16A \\sim
C72-F18A
 with sigma of 0.01
 F12-F11 \\sim F12-F10 \\sim F11-F10 \\sim F11A-F12A \\sim F11A-F10A \\sim
F12A-F10A
 with sigma of 0.02
 C56-F12 \\sim C56-F11 \\sim C56-F10 \\sim C56-F11A \\sim C56-F12A \\sim
C56-F10A
 with sigma of 0.01
 F4-F6 \\sim F4-F5 \\sim F6-F5 \\sim F5A-F6A \\sim F5A-F4A \\sim F6A-F4A
 with sigma of 0.02
 C63-F4 \\sim C63-F6 \\sim C63-F5 \\sim C63-F5A \\sim C63-F6A \\sim C63-F4A
 with sigma of 0.01
 F22-F23 \\sim F22-F24 \\sim F23-F24 \\sim F22A-F23A \\sim F22A-F24A \\sim
F23A-F24A
 with sigma of 0.04
 C47-F22 \\sim C47-C43 \\sim C47-F23 \\sim C47-F24 \\sim C47-F22A \\sim
C47-F23A \\sim C47-F24A
 with sigma of 0.02
3. Uiso/Uaniso restraints and constraints
F16A \\sim F16 \\sim F17 \\sim F18 \\sim F17A \\sim F18A: within 1.7A with
sigma of 0.02 and sigma for terminal atoms of 0.01
F10 \\sim F11 \\sim F12 \\sim F12A \\sim F10A \\sim F11A: within 1.7A with
sigma of 0.02 and sigma for terminal atoms of 0.01
F4 \\sim F5 \\sim F6 \\sim F4A \\sim F5A \\sim F6A: within 2A with sigma of
0.02 and sigma for terminal atoms of 0.01
F24A \\sim F22 \\sim F23 \\sim F24 \\sim F22A \\sim F23A: within 2A with sigma
of 0.02 and sigma for terminal atoms of 0.01
Uanis(C37) = Uanis(C37A)
Uanis(C38A) = Uanis(C38)
4. Others
 Fixed Sof: H39A(0.55) H39B(0.55) H39C(0.45) H39D(0.45) C37(0.55) H37A(0.55)
 H37B(0.55) C38(0.55) H38A(0.55) H38B(0.55) F16A(0.25) F24A(0.45) F4(0.7)
 F5(0.7) F6(0.7) F10(0.6) F11(0.6) F12(0.6) F16(0.75) F17(0.75) F18(0.75)
 F22(0.55) F23(0.55) F24(0.55) F22A(0.45) F4A(0.3) F12A(0.4) F5A(0.3)
 F17A(0.25) F6A(0.3) F23A(0.45) F10A(0.4) F11A(0.4) F18A(0.25) C37A(0.45)
 H37C(0.45) H37D(0.45) C38A(0.45) H38C(0.45) H38D(0.45)
5.a Secondary CH2 refined with riding coordinates:
 C4(H4A,H4B), C5(H5A,H5B), C7(H7A,H7B), C8(H8A,H8B), C9(H9A,H9B), C10(H10A,
 H10B), C11(H11A,H11B), C13(H13A,H13B), C14(H14A,H14B), C15(H15A,H15B),
 C16(H16A,H16B), C17(H17A,H17B), C21(H21A,H21B), C22(H22A,H22B), C24(H24A,H24B),
  C25(H25A,H25B), C26(H26A,H26B), C27(H27A,H27B), C28(H28A,H28B), C30(H30A,
 H30B), C31(H31A,H31B), C32(H32A,H32B), C33(H33A,H33B), C34(H34A,H34B),
 C36(H36A,H36B), C39(H39A,H39B), C39(H39C,H39D), C37(H37A,H37B), C38(H38A,H38B),
  C37A(H37C,H37D), C38A(H38C,H38D)
5.b Aromatic/amide H refined with riding coordinates:
 C42(H42), C44(H44), C46(H46), C50(H50), C52(H52), C54(H54), C58(H58),
 C60(H60), C62(H62), C66(H66), C68(H68), C70(H70)
5.c Idealised Me refined as rotating group:
 C40(H40A,H40B,H40C)
;
_olex2_submission_special_instructions 'No special instructions were received'