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_7035200
_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         'C53 H75 Cl2 N2 P Ru'
_chemical_formula_sum            'C53 H75 Cl2 N2 P Ru'
_chemical_formula_weight         943.09
_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             2015-02-13
_audit_creation_method
;
Olex2 1.2
(compiled 2015.01.26 svn.r3151 for OlexSys, GUI svn.r4998)
;
_audit_update_record
;
2015-02-13 deposited with the CCDC.
2015-05-15 downloaded from the CCDC.
;
_cell_angle_alpha                70.009(3)
_cell_angle_beta                 76.910(3)
_cell_angle_gamma                70.625(4)
_cell_formula_units_Z            4
_cell_length_a                   13.8813(6)
_cell_length_b                   16.8687(7)
_cell_length_c                   24.0954(7)
_cell_measurement_reflns_used    8061
_cell_measurement_temperature    100.0(1)
_cell_measurement_theta_max      74.7690
_cell_measurement_theta_min      3.9490
_cell_volume                     4961.1(4)
_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
;
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)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2008)'
_computing_structure_solution    'ShelXS (Sheldrick, 2008)'
_diffrn_ambient_temperature      100.0(1)
_diffrn_detector_area_resol_mean 10.4839
_diffrn_measured_fraction_theta_full 0.987
_diffrn_measured_fraction_theta_max 0.987
_diffrn_measurement_details
;
  1 omega  -86.00    3.00   1.0000    2.5000
omega____ theta____ kappa____ phi______ frames
    -      -41.6798  111.0000 -117.0000 89

  2 omega   24.00   80.00   1.0000    2.5000
omega____ theta____ kappa____ phi______ frames
    -       41.6798 -111.0000  148.0000 56

  3 omega  -64.00  -39.00   1.0000   12.0000
omega____ theta____ kappa____ phi______ frames
    -      -43.5000  111.0000 -117.0000 25

  4 omega   47.00   93.00   1.0000   12.0000
omega____ theta____ kappa____ phi______ frames
    -      109.1316 -111.0000  148.0000 46

  5 omega  100.00  130.00   1.0000   12.0000
omega____ theta____ kappa____ phi______ frames
    -      109.1316  111.0000 -117.0000 30

  6 omega  -50.00   33.00   1.0000    2.5000
omega____ theta____ kappa____ phi______ frames
    -      -41.6798   38.0000 -180.0000 83

  7 omega -116.00  -80.00   1.0000   12.0000
omega____ theta____ kappa____ phi______ frames
    -      -43.5000  -94.0000  -60.0000 36

  8 omega  -55.00   30.00   1.0000   12.0000
omega____ theta____ kappa____ phi______ frames
    -      -43.5000   45.0000   60.0000 85

  9 omega   36.00   89.00   1.0000   12.0000
omega____ theta____ kappa____ phi______ frames
    -      109.1316  -45.0000  150.0000 53

 10 omega   34.00   91.00   1.0000   12.0000
omega____ theta____ kappa____ phi______ frames
    -      109.1316  -30.0000   60.0000 57

 11 omega   48.00  105.00   1.0000   12.0000
omega____ theta____ kappa____ phi______ frames
    -      109.1316  -94.0000  -90.0000 57

 12 omega   33.00   91.00   1.0000   12.0000
omega____ theta____ kappa____ phi______ frames
    -      109.1316  -30.0000 -180.0000 58

 13 omega   39.00   91.00   1.0000   12.0000
omega____ theta____ kappa____ phi______ frames
    -      109.1316  -94.0000 -180.0000 52

 14 omega   27.00  105.00   1.0000   12.0000
omega____ theta____ kappa____ phi______ frames
    -      109.1316  -94.0000    0.0000 78

 15 omega   81.00  178.00   1.0000   12.0000
omega____ theta____ kappa____ phi______ frames
    -      109.1316   30.0000  120.0000 97

 16 omega   95.00  177.00   1.0000   12.0000
omega____ theta____ kappa____ phi______ frames
    -      109.1316  125.0000 -180.0000 82

 17 omega   41.00   90.00   1.0000   12.0000
omega____ theta____ kappa____ phi______ frames
    -      109.1316  -45.0000 -120.0000 49

 18 omega   34.00   89.00   1.0000   12.0000
omega____ theta____ kappa____ phi______ frames
    -      109.1316  -30.0000  -60.0000 55

 19 omega   91.00  178.00   1.0000   12.0000
omega____ theta____ kappa____ phi______ frames
    -      109.1316   45.0000 -180.0000 87
;
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at zero, Atlas'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_UB_11      0.0222966000
_diffrn_orient_matrix_UB_12      -0.0463948000
_diffrn_orient_matrix_UB_13      0.0648680000
_diffrn_orient_matrix_UB_21      -0.0673885000
_diffrn_orient_matrix_UB_22      0.0829616000
_diffrn_orient_matrix_UB_23      0.0176736000
_diffrn_orient_matrix_UB_31      -0.0950290000
_diffrn_orient_matrix_UB_32      -0.0346325000
_diffrn_orient_matrix_UB_33      0.0136069000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0766
_diffrn_reflns_av_unetI/netI     0.1317
_diffrn_reflns_laue_measured_fraction_full 0.963
_diffrn_reflns_laue_measured_fraction_max 0.987
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_l_max       28
_diffrn_reflns_limit_l_min       -28
_diffrn_reflns_number            33426
_diffrn_reflns_point_group_measured_fraction_full 0.963
_diffrn_reflns_point_group_measured_fraction_max 0.987
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         66.600
_diffrn_reflns_theta_min         3.656
_diffrn_source                   'SuperNova (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    4.114
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.82436
_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            red
_exptl_crystal_colour_primary    red
_exptl_crystal_density_diffrn    1.263
_exptl_crystal_description       block
_exptl_crystal_F_000             2000
_exptl_crystal_size_max          0.1499
_exptl_crystal_size_mid          0.0532
_exptl_crystal_size_min          0.0459
_refine_diff_density_max         1.432
_refine_diff_density_min         -0.757
_refine_diff_density_rms         0.102
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.053
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1098
_refine_ls_number_reflns         17300
_refine_ls_number_restraints     70
_refine_ls_restrained_S_all      1.053
_refine_ls_R_factor_all          0.0959
_refine_ls_R_factor_gt           0.0625
_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^)+(0.0357P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1392
_refine_ls_wR_factor_ref         0.1674
_reflns_Friedel_coverage         0.000
_reflns_number_gt                11950
_reflns_number_total             17300
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c5dt00967g2.cif
_cod_data_source_block           fv044
_cod_depositor_comments
'Adding full bibliography for 7035200--7035203.cif.'
_cod_database_code               7035200
_shelxl_version_number           2013-4
_chemical_oxdiff_formula         'C20 H20 Cl2 P1 N2 Ru'
_reflns_odcompleteness_completeness 98.67
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     66.49
_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, All C(H,H,H,H,H,H) groups
2. Restrained distances
 C31A-C32A = C32A-C33A = C33A-C34A = C34A-C35A
 1.5 with sigma of 0.01
 C31A-C32B = C32B-C33B = C33B-C34B = C34B-C35A
 1.5 with sigma of 0.01
3. Rigid bond restraints
 C31A, C32A, C33A, C34A, C35A
 with sigma for 1-2 distances of 0.005 and sigma for 1-3 distances of 0.005
 C31A, C32B, C33B, C34B, C35A
 with sigma for 1-2 distances of 0.005 and sigma for 1-3 distances of 0.005
4. Uiso/Uaniso restraints and constraints
C31A \\sim C32A \\sim C33A \\sim C34A \\sim C35A: within 1.7A with sigma of
0.01 and sigma for terminal atoms of 0.02
C31A \\sim C32B \\sim C33B \\sim C34B \\sim C35A: within 1.7A with sigma of
0.01 and sigma for terminal atoms of 0.02
5. Others
 Sof(H31C)=Sof(H31D)=Sof(C32B)=Sof(H32C)=Sof(H32D)=Sof(C33B)=Sof(H33C)=
 Sof(H33D)=Sof(C34B)=Sof(H34C)=Sof(H34D)=Sof(H35D)=Sof(H35E)=Sof(H35F)=1-FVAR(1)
 Sof(H31A)=Sof(H31B)=Sof(C32A)=Sof(H32A)=Sof(H32B)=Sof(C33A)=Sof(H33A)=
 Sof(H33B)=Sof(C34A)=Sof(H34A)=Sof(H34B)=Sof(H35A)=Sof(H35B)=Sof(H35C)=FVAR(1)
6.a Ternary CH refined with riding coordinates:
 C36(H36), C42(H42), C48(H48), C36A(H36A), C42A(H42A), C48A(H48A)
6.b Secondary CH2 refined with riding coordinates:
 C17(H17C,H17D), C18(H18C,H18D), C28(H28C,H28D), C29(H29C,H29D), C30(H30C,
 H30D), C31(H31E,H31F), C32(H32E,H32F), C33(H33E,H33F), C34(H34E,H34F),
 C37(H37C,H37D), C38(H38C,H38D), C39(H39C,H39D), C40(H40C,H40D), C41(H41C,H41D),
  C43(H43C,H43D), C44(H44C,H44D), C45(H45C,H45D), C46(H46C,H46D), C47(H47C,
 H47D), C49(H49C,H49D), C50(H50C,H50D), C51(H51C,H51D), C52(H52C,H52D),
 C53(H53C,H53D), C17A(H17A,H17B), C18A(H18A,H18B), C28A(H28A,H28B), C29A(H29A,
 H29B), C30A(H30A,H30B), C31A(H31A,H31B), C31A(H31C,H31D), C32A(H32A,H32B),
 C33A(H33A,H33B), C34A(H34A,H34B), C32B(H32C,H32D), C33B(H33C,H33D), C34B(H34C,
 H34D), C37A(H37A,H37B), C38A(H38A,H38B), C39A(H39A,H39B), C40A(H40A,H40B),
 C41A(H41A,H41B), C43A(H43A,H43B), C44A(H44A,H44B), C45A(H45A,H45B), C46A(H46A,
 H46B), C47A(H47A,H47B), C49A(H49A,H49B), C50A(H50A,H50B), C51A(H51A,H51B),
 C52A(H52A,H52B), C53A(H53A,H53B)
6.c Me refined with riding coordinates:
 C35A(H35A,H35B,H35C), C35A(H35D,H35E,H35F)
6.d Aromatic/amide H refined with riding coordinates:
 C2(H2), C5(H5), C6(H6), C7(H7), C8(H8), C11(H11), C12(H12), C13(H13),
 C14(H14), C15(H15), C21(H21), C23(H23), C3A(H3A), C4A(H4A), C5A(H5A), C6A(H6A),
  C9A(H9A), C11A(H11A), C12A(H12A), C13A(H13A), C14A(H14A), C15A(H15A),
 C21A(H21A), C23A(H23A)
6.e Idealised Me refined as rotating group:
 C25(H25D,H25E,H25F), C26(H26D,H26E,H26F), C27(H27D,H27E,H27F), C35(H35G,H35H,
 H35I), C25A(H25A,H25B,H25C), C26A(H26A,H26B,H26C), C27A(H27A,H27B,H27C)
;
_shelx_res_checksum              37066
_olex2_exptl_crystal_mounting_method 'mounted on a nylon loop'
_olex2_submission_special_instructions 'No special instructions were received'