Ruthenium indenylidene complexes bearing N-alkyl/N-mesityl-substituted N-heterocyclic carbene ligands.
Yu, Baoyi; Hamad, Fatma B.; Sels, Bert; Van Hecke, Kristof; Verpoort, Francis; Dalton transactions (Cambridge, England : 2003) 44 (2015) 11835–11842; doi:10.1039/c5dt00967g

data_7035201
_publ_section_title
;
 Ruthenium indenylidene complexes bearing N-alkyl/N-mesityl-substituted
 N-heterocyclic carbene ligands.
;
_journal_issue                   26
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              11835
_journal_page_last               11842
_journal_paper_doi               10.1039/c5dt00967g
_journal_volume                  44
_journal_year                    2015
_chemical_formula_moiety         'C46 H61 Cl2 N2 P Ru'
_chemical_formula_sum            'C46 H61 Cl2 N2 P Ru'
_chemical_formula_weight         844.91
_chemical_name_systematic
;
 ?
;
_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     direct
_audit_creation_date             2014-08-05
_audit_creation_method
;
Olex2 1.2
(compiled 2014.07.22 svn.r2960 for OlexSys, GUI svn.r4862)
;
_audit_update_record
;
2015-02-13 deposited with the CCDC.
2015-05-15 downloaded from the CCDC.
;
_cell_angle_alpha                92.110(3)
_cell_angle_beta                 100.964(4)
_cell_angle_gamma                102.538(4)
_cell_formula_units_Z            2
_cell_length_a                   9.8957(5)
_cell_length_b                   12.6238(6)
_cell_length_c                   17.6587(6)
_cell_measurement_reflns_used    7355
_cell_measurement_temperature    100.0(1)
_cell_measurement_theta_max      75.7880
_cell_measurement_theta_min      4.2510
_cell_volume                     2107.00(17)
_computing_cell_refinement
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.32 (release 02-08-2013 CrysAlis171 .NET)
(compiled Aug  2 2013,16:46:58)
;
_computing_data_collection
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CrysAlisPro, Agilent Technologies,
Version 1.171.36.32 (release 02-08-2013 CrysAlis171 .NET)
(compiled Aug  2 2013,16:46:58)
;
_computing_data_reduction
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CrysAlisPro, Agilent Technologies,
Version 1.171.36.32 (release 02-08-2013 CrysAlis171 .NET)
(compiled Aug  2 2013,16:46:58)
;
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
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_computing_structure_solution    'ShelXS (Sheldrick, 2008)'
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_diffrn_measured_fraction_theta_max 0.974
_diffrn_measurement_details
;
  1 omega  -97.00  -38.00   1.0000    2.4700
omega____ theta____ kappa____ phi______ frames
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  2 omega   52.00   88.00   1.0000    2.4700
omega____ theta____ kappa____ phi______ frames
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  3 omega   74.00   99.00   1.0000    2.4700
omega____ theta____ kappa____ phi______ frames
    -       41.6798  174.0000    8.0000 25

  4 omega -109.00  -83.00   1.0000   11.0000
omega____ theta____ kappa____ phi______ frames
    -      -43.5000 -174.0000   -1.0000 26

  5 omega  -66.00  -41.00   1.0000   11.0000
omega____ theta____ kappa____ phi______ frames
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  6 omega   76.00  110.00   1.0000   11.0000
omega____ theta____ kappa____ phi______ frames
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  7 omega   83.00  108.00   1.0000   11.0000
omega____ theta____ kappa____ phi______ frames
    -      111.0000  174.0000    8.0000 25

  8 omega  117.00  144.00   1.0000   11.0000
omega____ theta____ kappa____ phi______ frames
    -      111.0000  114.0000 -131.0000 27

  9 omega  110.00  138.00   1.0000   11.0000
omega____ theta____ kappa____ phi______ frames
    -      111.0000 -174.0000   -1.0000 28

 10 omega -115.00  -14.00   1.0000    2.4700
omega____ theta____ kappa____ phi______ frames
    -      -41.6798  -57.0000  -90.0000 101

 11 omega   26.00   87.00   1.0000    2.4700
omega____ theta____ kappa____ phi______ frames
    -       41.6798 -125.0000 -150.0000 61

 12 omega -126.00  -98.00   1.0000   11.0000
omega____ theta____ kappa____ phi______ frames
    -      -43.5000  -94.0000   60.0000 28

 13 omega -125.00  -98.00   1.0000   11.0000
omega____ theta____ kappa____ phi______ frames
    -      -43.5000  -94.0000 -150.0000 27

 14 omega  -55.00   30.00   1.0000   11.0000
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 15 omega -124.00  -82.00   1.0000   11.0000
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 16 omega   39.00   98.00   1.0000   11.0000
omega____ theta____ kappa____ phi______ frames
    -      111.0000  -45.0000   90.0000 59

 17 omega   55.00   95.00   1.0000   11.0000
omega____ theta____ kappa____ phi______ frames
    -      111.0000  -94.0000    0.0000 40

 18 omega   64.00   91.00   1.0000   11.0000
omega____ theta____ kappa____ phi______ frames
    -      111.0000  -30.0000  150.0000 27

 19 omega   94.00  150.00   1.0000   11.0000
omega____ theta____ kappa____ phi______ frames
    -      111.0000  125.0000  -30.0000 56

 20 omega   59.00  100.00   1.0000   11.0000
omega____ theta____ kappa____ phi______ frames
    -      111.0000  -77.0000 -180.0000 41

 21 omega   30.00   87.00   1.0000   11.0000
omega____ theta____ kappa____ phi______ frames
    -      111.0000  -15.0000   60.0000 57

 22 omega   46.00   98.00   1.0000   11.0000
omega____ theta____ kappa____ phi______ frames
    -      111.0000  -45.0000   30.0000 52

 23 omega   41.00   92.00   1.0000   11.0000
omega____ theta____ kappa____ phi______ frames
    -      111.0000  -45.0000 -150.0000 51

 24 omega   39.00   95.00   1.0000   11.0000
omega____ theta____ kappa____ phi______ frames
    -      111.0000  -45.0000  150.0000 56

 25 omega   72.00   98.00   1.0000   11.0000
omega____ theta____ kappa____ phi______ frames
    -      111.0000  -45.0000  -30.0000 26

 26 omega   59.00  109.00   1.0000   11.0000
omega____ theta____ kappa____ phi______ frames
    -      111.0000  -94.0000  150.0000 50

 27 omega   39.00  101.00   1.0000   11.0000
omega____ theta____ kappa____ phi______ frames
    -      111.0000 -125.0000    0.0000 62

 28 omega  135.00  171.00   1.0000   11.0000
omega____ theta____ kappa____ phi______ frames
    -      111.0000   30.0000   90.0000 36

 29 omega   99.00  158.00   1.0000   11.0000
omega____ theta____ kappa____ phi______ frames
    -      111.0000  125.0000 -180.0000 59

 30 omega   57.00   90.00   1.0000   11.0000
omega____ theta____ kappa____ phi______ frames
    -      111.0000  -30.0000 -150.0000 33

 31 omega   66.00  109.00   1.0000   11.0000
omega____ theta____ kappa____ phi______ frames
    -      111.0000 -125.0000   90.0000 43

 32 omega   72.00  106.00   1.0000   11.0000
omega____ theta____ kappa____ phi______ frames
    -      111.0000 -125.0000  -60.0000 34

 33 omega  117.00  142.00   1.0000   11.0000
omega____ theta____ kappa____ phi______ frames
    -      111.0000  -77.0000 -180.0000 25

 34 omega   84.00  128.00   1.0000   11.0000
omega____ theta____ kappa____ phi______ frames
    -      111.0000   30.0000   90.0000 44

 35 omega  102.00  178.00   1.0000   11.0000
omega____ theta____ kappa____ phi______ frames
    -      111.0000  125.0000   90.0000 76

 36 omega   96.00  123.00   1.0000   11.0000
omega____ theta____ kappa____ phi______ frames
    -      111.0000  -15.0000   60.0000 27

 37 omega  139.00  164.00   1.0000   11.0000
omega____ theta____ kappa____ phi______ frames
    -      111.0000  -15.0000   60.0000 25

 38 omega   95.00  178.00   1.0000   11.0000
omega____ theta____ kappa____ phi______ frames
    -      111.0000  125.0000 -150.0000 83

 39 omega   59.00   90.00   1.0000   11.0000
omega____ theta____ kappa____ phi______ frames
    -      111.0000  -61.0000  -30.0000 31

 40 omega  113.00  164.00   1.0000   11.0000
omega____ theta____ kappa____ phi______ frames
    -      111.0000   61.0000  150.0000 51

 41 omega   64.00   91.00   1.0000   11.0000
omega____ theta____ kappa____ phi______ frames
    -      111.0000   15.0000  -30.0000 27

 42 omega  118.00  166.00   1.0000   11.0000
omega____ theta____ kappa____ phi______ frames
    -      111.0000   15.0000  -30.0000 48

 43 omega   39.00   91.00   1.0000   11.0000
omega____ theta____ kappa____ phi______ frames
    -      111.0000  -30.0000  -60.0000 52

 44 omega   83.00  108.00   1.0000   11.0000
omega____ theta____ kappa____ phi______ frames
    -      111.0000   61.0000  150.0000 25
;
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at zero, Atlas'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_UB_11      -0.0384776000
_diffrn_orient_matrix_UB_12      0.0105235000
_diffrn_orient_matrix_UB_13      -0.0876907000
_diffrn_orient_matrix_UB_21      0.1572060000
_diffrn_orient_matrix_UB_22      0.0178385000
_diffrn_orient_matrix_UB_23      -0.0044999000
_diffrn_orient_matrix_UB_31      -0.0183263000
_diffrn_orient_matrix_UB_32      -0.1237129000
_diffrn_orient_matrix_UB_33      -0.0154764000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0630
_diffrn_reflns_av_unetI/netI     0.0657
_diffrn_reflns_laue_measured_fraction_full 0.994
_diffrn_reflns_laue_measured_fraction_max 0.974
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            24516
_diffrn_reflns_point_group_measured_fraction_full 0.994
_diffrn_reflns_point_group_measured_fraction_max 0.974
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         76.456
_diffrn_reflns_theta_min         3.599
_diffrn_source                   'SuperNova (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    4.782
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.73072
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.32 (release 02-08-2013 CrysAlis171 .NET)
(compiled Aug  2 2013,16:46:58)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            'clear light red'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   light
_exptl_crystal_colour_primary    red
_exptl_crystal_density_diffrn    1.332
_exptl_crystal_description       plate
_exptl_crystal_F_000             888
_exptl_crystal_size_max          0.2854
_exptl_crystal_size_mid          0.1437
_exptl_crystal_size_min          0.0598
_refine_diff_density_max         0.668
_refine_diff_density_min         -1.088
_refine_diff_density_rms         0.085
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.030
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     519
_refine_ls_number_reflns         8618
_refine_ls_number_restraints     57
_refine_ls_restrained_S_all      1.032
_refine_ls_R_factor_all          0.0710
_refine_ls_R_factor_gt           0.0533
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0764P)^2^+1.2529P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1366
_refine_ls_wR_factor_ref         0.1531
_reflns_Friedel_coverage         0.000
_reflns_number_gt                6723
_reflns_number_total             8618
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c5dt00967g2.cif
_cod_data_source_block           fv075
_cod_depositor_comments
'Adding full bibliography for 7035200--7035203.cif.'
_cod_database_code               7035201
_shelxl_version_number           2013-4
_chemical_oxdiff_formula         'Ru2 C40 H80 Cl4 P2 N4 '
_reflns_odcompleteness_completeness 99.21
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     74.33
_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
 C10A-C11A = C11A-C12A = C12A-C13A = C13A-C14A = C14A-C15A = C15A-C10A
 1.39 with sigma of 0.01
 C10B-C11B = C11B-C12B = C12B-C13B = C13B-C14B = C14B-C15B = C15B-C10B
 1.39 with sigma of 0.01
 C3B-C10B
 1.48 with sigma of 0.01
 C1A-C2A
 1.43 with sigma of 0.01
 C2A-C3A
 1.43 with sigma of 0.01
 C3A-C4A
 1.44 with sigma of 0.01
 C4A-C9A
 1.44 with sigma of 0.01
 C9A-C1A
 1.44 with sigma of 0.01
 C1B-C2B
 1.43 with sigma of 0.01
 C2B-C3B
 1.43 with sigma of 0.01
 C3B-C4B
 1.44 with sigma of 0.01
 C4B-C9B
 1.44 with sigma of 0.01
 C9B-C1B
 1.44 with sigma of 0.01
 C4A-C5A
 1.42 with sigma of 0.01
 C5A-C6A
 1.37 with sigma of 0.01
 C6A-C7A
 1.42 with sigma of 0.01
 C7A-C8A
 1.36 with sigma of 0.01
 C8A-C9A
 1.42 with sigma of 0.01
 C4B-C5B
 1.42 with sigma of 0.01
 C5B-C6B
 1.37 with sigma of 0.01
 C6B-C7B
 1.42 with sigma of 0.01
 C7B-C8B
 1.36 with sigma of 0.01
 C8B-C9B
 1.42 with sigma of 0.01
 C4B-C6B
 2.4 with sigma of 0.02
 C5B-C7B
 2.43 with sigma of 0.02
 C6B-C8B
 2.42 with sigma of 0.02
 C7B-C9B
 2.4 with sigma of 0.02
 C8B-C4B
 2.47 with sigma of 0.02
 C9B-C5B
 2.47 with sigma of 0.02
3. Restrained planarity
 C10A, C11A, C12A, C13A, C14A, C15A
 with sigma of 0.01
 C10B, C11B, C12B, C13B, C14B, C15B
 with sigma of 0.01
 C1A, C2A, C3A, C4A, C9A, C5A, C6A, C7A, C8A
 with sigma of 0.01
 C1B, C2B, C3B, C4B, C9B, C5B, C6B, C7B, C8B
 with sigma of 0.01
4. Uiso/Uaniso restraints and constraints
Uanis(C1A) = Uanis(C1B)
Uanis(C2A) = Uanis(C2B)
Uanis(C3A) = Uanis(C3B)
Uanis(C4A) = Uanis(C4B)
Uanis(C5A) = Uanis(C5B)
Uanis(C6A) = Uanis(C6B)
Uanis(C7A) = Uanis(C7B)
Uanis(C8A) = Uanis(C8B)
Uanis(C9A) = Uanis(C9B)
Uanis(C10A) = Uanis(C10B)
Uanis(C11A) = Uanis(C11B)
Uanis(C12A) = Uanis(C12B)
Uanis(C13A) = Uanis(C13B)
Uanis(C14A) = Uanis(C14B)
Uanis(C15A) = Uanis(C15B)
5. Others
 Sof(C1B)=Sof(C2B)=Sof(H2B)=Sof(C3B)=Sof(C4B)=Sof(C5B)=Sof(H5B)=Sof(C6B)=
 Sof(H6B)=Sof(C8B)=Sof(H8B)=Sof(C7B)=Sof(H7B)=Sof(C9B)=Sof(C10B)=Sof(C11B)=
 Sof(H11B)=Sof(C12B)=Sof(H12B)=Sof(C13B)=Sof(H13B)=Sof(C14B)=Sof(H14B)=
 Sof(C15B)=Sof(H15B)=1-FVAR(1)
 Sof(C1A)=Sof(C2A)=Sof(H2A)=Sof(C3A)=Sof(C4A)=Sof(C5A)=Sof(H5A)=Sof(C6A)=
 Sof(H6A)=Sof(C7A)=Sof(H7A)=Sof(C8A)=Sof(H8A)=Sof(C9A)=Sof(C10A)=Sof(C11A)=
 Sof(H11A)=Sof(C12A)=Sof(H12A)=Sof(C13A)=Sof(H13A)=Sof(C14A)=Sof(H14A)=
 Sof(C15A)=Sof(H15A)=FVAR(1)
6.a Ternary CH refined with riding coordinates:
 C35(H35), C41(H41), C29(H29)
6.b Secondary CH2 refined with riding coordinates:
 C33(H33A,H33B), C34(H34A,H34B), C42(H42A,H42B), C17(H17A,H17B), C46(H46A,
 H46B), C45(H45A,H45B), C30(H30A,H30B), C44(H44A,H44B), C18(H18A,H18B),
 C36(H36A,H36B), C32(H32A,H32B), C31(H31A,H31B), C43(H43A,H43B), C40(H40A,H40B),
  C39(H39A,H39B), C37(H37A,H37B), C38(H38A,H38B)
6.c Aromatic/amide H refined with riding coordinates:
 C2A(H2A), C5A(H5A), C6A(H6A), C7A(H7A), C8A(H8A), C11A(H11A), C12A(H12A),
 C13A(H13A), C14A(H14A), C15A(H15A), C2B(H2B), C5B(H5B), C6B(H6B), C8B(H8B),
 C7B(H7B), C11B(H11B), C12B(H12B), C13B(H13B), C14B(H14B), C15B(H15B), C21(H21),
  C23(H23)
6.d Idealised Me refined as rotating group:
 C28(H28A,H28B,H28C), C26(H26A,H26B,H26C), C25(H25A,H25B,H25C), C27(H27A,H27B,
 H27C)
;
_shelx_res_checksum              44367
_olex2_computing_structure_refinement_long 'ShelXL (Sheldrick, 2008)'
_olex2_computing_structure_solution_long 'ShelXS (Sheldrick, 2008)'
_olex2_exptl_crystal_mounting_method 'mounted on a nylon loop'
_olex2_submission_special_instructions 'No special instructions were received'