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_7049052
_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_absolute_configuration ad
_chemical_formula_moiety         'C56 H75 N4 O Ru Zn, C32 H12 B F24'
_chemical_formula_sum            'C88 H87 B F24 N4 O Ru Zn'
_chemical_formula_weight         1849.86
_space_group_crystal_system      orthorhombic
_space_group_IT_number           19
_space_group_name_Hall           'P 2ac 2ab'
_space_group_name_H-M_alt        'P 21 21 21'
_symmetry_space_group_name_Hall  'P 2ac 2ab'
_symmetry_space_group_name_H-M   'P 21 21 21'
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     iterative
_audit_creation_date             2017-07-06
_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                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   16.4346(4)
_cell_length_b                   21.1397(5)
_cell_length_c                   24.5462(5)
_cell_measurement_reflns_used    22592
_cell_measurement_temperature    150.0(2)
_cell_measurement_theta_max      27.3550
_cell_measurement_theta_min      3.8250
_cell_volume                     8527.9(3)
_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      150.0(2)
_diffrn_detector                 'CCD plate'
_diffrn_detector_type            EosS2
_diffrn_measured_fraction_theta_full 0.996
_diffrn_measured_fraction_theta_max 0.991
_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  0.0429
_diffrn_reflns_av_unetI/netI     0.0478
_diffrn_reflns_Laue_measured_fraction_full 0.996
_diffrn_reflns_Laue_measured_fraction_max 0.991
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_h_min       -20
_diffrn_reflns_limit_k_max       27
_diffrn_reflns_limit_k_min       -27
_diffrn_reflns_limit_l_max       31
_diffrn_reflns_limit_l_min       -31
_diffrn_reflns_number            77177
_diffrn_reflns_point_group_measured_fraction_full 0.997
_diffrn_reflns_point_group_measured_fraction_max 0.980
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.484
_diffrn_reflns_theta_min         3.334
_diffrn_source                   'fine-focus sealed X-ray tube'
_diffrn_source_type              'Enhance (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    0.559
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.98496
_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            red
_exptl_crystal_colour_primary    red
_exptl_crystal_density_diffrn    1.441
_exptl_crystal_description       block
_exptl_crystal_F_000             3784
_exptl_crystal_size_max          0.528
_exptl_crystal_size_mid          0.38
_exptl_crystal_size_min          0.378
_refine_diff_density_max         0.830
_refine_diff_density_min         -0.861
_refine_diff_density_rms         0.080
_refine_ls_abs_structure_details
;
 Flack x determined using 6199 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   0.017(4)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.077
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1136
_refine_ls_number_reflns         19171
_refine_ls_number_restraints     67
_refine_ls_restrained_S_all      1.089
_refine_ls_R_factor_all          0.0680
_refine_ls_R_factor_gt           0.0511
_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^)+(0.0462P)^2^+10.8415P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1112
_refine_ls_wR_factor_ref         0.1206
_reflns_Friedel_coverage         0.824
_reflns_Friedel_fraction_full    0.999
_reflns_Friedel_fraction_max     0.966
_reflns_number_gt                16228
_reflns_number_total             19171
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c8dt05023f2.cif
_cod_data_source_block           e17mkw7
_cod_depositor_comments
'Adding full bibliography for 7049052--7049061.cif.'
_cod_database_code               7049052
_shelx_shelxl_version_number     2014/7
_chemical_oxdiff_usercomment     'red 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
 F7A-F8A \\sim F9A-F8A \\sim F7-F9 \\sim F7-F8 \\sim F9-F8
 with sigma of 0.04
 C80-F7A \\sim C80-F9A \\sim C80-F7 \\sim C80-F9 \\sim C80-F8 \\sim C80-F8A
 with sigma of 0.02
 C55-H55A \\sim C55-H55C \\sim C55-H55B
 with sigma of 0.005
 H55A-H55B \\sim H55B-H55C \\sim H55C-H55A
 with sigma of 0.01
3. Uiso/Uaniso restraints and constraints
F7 \\sim F8 \\sim F9 \\sim F7A \\sim F8A \\sim F9A: within 2A with sigma of
0.03 and sigma for terminal atoms of 0.01
4. Others
 Fixed Sof: F7(0.7) F8(0.7) F9(0.7) F7A(0.3) F8A(0.3) F9A(0.3)
5.a Ternary CH refined with riding coordinates:
 C10(H10), C13(H13), C23(H23), C26(H26), C38(H38), C41(H41), C50(H50), C53(H53)
5.b Aromatic/amide H refined with riding coordinates:
 C2(H2), C3(H3), C6(H6), C7(H7), C8(H8), C18(H18), C19(H19), C20(H20),
 C30(H30), C31(H31), C34(H34), C35(H35), C36(H36), C46(H46), C47(H47), C48(H48),
  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.c Idealised Me refined as rotating group:
 C11(H11A,H11B,H11C), C12(H12A,H12B,H12C), C14(H14A,H14B,H14C), C15(H15A,H15B,
 H15C), C24(H24A,H24B,H24C), C25(H25A,H25B,H25C), C27(H27A,H27B,H27C), C28(H28A,
 H28B,H28C), C39(H39A,H39B,H39C), C40(H40A,H40B,H40C), C42(H42A,H42B,H42C),
 C43(H43A,H43B,H43C), C51(H51A,H51B,H51C), C52(H52A,H52B,H52C), C54(H54A,H54B,
 H54C), C57(H57A,H57B,H57C)
;
_olex2_submission_special_instructions 'No special instructions were received'