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_7035203
_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         '2(C51 H69 Cl2 N2 P Ru), C H2 Cl2'
_chemical_formula_sum            'C103 H140 Cl6 N4 P2 Ru2'
_chemical_formula_weight         1910.97
_chemical_name_systematic
;
 ?
;
_space_group_crystal_system      monoclinic
_space_group_IT_number           15
_space_group_name_Hall           '-C 2yc'
_space_group_name_H-M_alt        'C 1 2/c 1'
_symmetry_space_group_name_Hall  '-C 2yc'
_symmetry_space_group_name_H-M   'C 1 2/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_audit_creation_date             2014-07-31
_audit_creation_method
;
Olex2 1.2
(compiled 2014.07.22 svn.r2960 for OlexSys, GUI svn.r4862)
;
_audit_update_record
;
2015-02-14 deposited with the CCDC.
2015-05-15 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 94.2889(14)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   33.7446(6)
_cell_length_b                   14.6670(3)
_cell_length_c                   19.0468(3)
_cell_measurement_reflns_used    13228
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      27.7300
_cell_measurement_theta_min      3.0390
_cell_volume                     9400.5(3)
_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
;
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
_diffrn_detector_area_resol_mean 10.4839
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.879
_diffrn_measurement_details
;
  1 omega   21.00   86.00   1.0000    4.0000
omega____ theta____ kappa____ phi______ frames
    -       10.3260 -160.0000   24.0000 65

  2 omega    5.00   30.00   1.0000    4.0000
omega____ theta____ kappa____ phi______ frames
    -       10.3260 -118.0000  176.0000 25

  3 omega  -89.00  -64.00   1.0000    4.0000
omega____ theta____ kappa____ phi______ frames
    -      -10.9510  160.0000   55.0000 25

  4 omega    0.00   27.00   1.0000    4.0000
omega____ theta____ kappa____ phi______ frames
    -       10.3260  -99.0000   90.0000 27

  5 omega  -16.00   86.00   1.0000    4.0000
omega____ theta____ kappa____ phi______ frames
    -       10.3260   77.0000 -180.0000 102

  6 omega  -44.00  -18.00   1.0000    4.0000
omega____ theta____ kappa____ phi______ frames
    -       10.3260  -38.0000   60.0000 26

  7 omega   32.00   84.00   1.0000    4.0000
omega____ theta____ kappa____ phi______ frames
    -       10.3260   38.0000  -90.0000 52

  8 omega   44.00   78.00   1.0000    4.0000
omega____ theta____ kappa____ phi______ frames
    -       10.3260   57.0000  150.0000 34

  9 omega   11.00   38.00   1.0000    4.0000
omega____ theta____ kappa____ phi______ frames
    -      -10.9510   38.0000 -180.0000 27

 10 omega  -14.00   34.00   1.0000    4.0000
omega____ theta____ kappa____ phi______ frames
    -       10.3260   38.0000   90.0000 48
;
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at zero, Atlas'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_UB_11      -0.0060648000
_diffrn_orient_matrix_UB_12      0.0369842000
_diffrn_orient_matrix_UB_13      -0.0222579000
_diffrn_orient_matrix_UB_21      0.0029467000
_diffrn_orient_matrix_UB_22      0.0304175000
_diffrn_orient_matrix_UB_23      0.0288776000
_diffrn_orient_matrix_UB_31      0.0199716000
_diffrn_orient_matrix_UB_32      0.0067494000
_diffrn_orient_matrix_UB_33      -0.0080774000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0783
_diffrn_reflns_av_unetI/netI     0.0880
_diffrn_reflns_laue_measured_fraction_full 0.998
_diffrn_reflns_laue_measured_fraction_max 0.879
_diffrn_reflns_limit_h_max       42
_diffrn_reflns_limit_h_min       -46
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_limit_l_min       -25
_diffrn_reflns_number            55212
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.879
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         29.778
_diffrn_reflns_theta_min         3.041
_diffrn_source                   'SuperNova (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    0.575
_exptl_absorpt_correction_T_max  0.995
_exptl_absorpt_correction_T_min  0.985
_exptl_absorpt_correction_type   analytical
_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)
Analytical numeric absorption correction using a multifaceted crystal
            model based on expressions derived by R.C. Clark & J.S. Reid.
(Clark, R. C. & Reid, J. S. (1995). Acta Cryst. A51, 887-897)
;
_exptl_crystal_colour            red
_exptl_crystal_colour_primary    red
_exptl_crystal_density_diffrn    1.350
_exptl_crystal_description       block
_exptl_crystal_F_000             4024.0
_exptl_crystal_size_max          0.431
_exptl_crystal_size_mid          0.1352
_exptl_crystal_size_min          0.1048
_refine_diff_density_max         0.887
_refine_diff_density_min         -1.291
_refine_diff_density_rms         0.112
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.052
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     531
_refine_ls_number_reflns         11830
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.052
_refine_ls_R_factor_all          0.0991
_refine_ls_R_factor_gt           0.0576
_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^)+(0.0403P)^2^+27.2294P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1080
_refine_ls_wR_factor_ref         0.1252
_reflns_Friedel_coverage         0.000
_reflns_number_gt                8243
_reflns_number_total             11830
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c5dt00967g2.cif
_cod_data_source_block           fv071
_cod_depositor_comments
'Adding full bibliography for 7035200--7035203.cif.'
_cod_database_code               7035203
_shelxl_version_number           2013-4
_chemical_oxdiff_formula         'Ru1 C51 H69 Cl2 N2 P1'
_reflns_odcompleteness_completeness 99.76
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     26.32
_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. Others
 Fixed Sof: H1AA(0.5) H1AB(0.5)
3.a Ternary CH refined with riding coordinates:
 C46(H46), C40(H40), C34(H34), C28(H28)
3.b Secondary CH2 refined with riding coordinates:
 C29(H29A,H29B), C44(H44A,H44B), C47(H47A,H47B), C49(H49A,H49B), C51(H51A,
 H51B), C42(H42A,H42B), C33(H33A,H33B), C39(H39A,H39B), C41(H41A,H41B),
 C50(H50A,H50B), C35(H35A,H35B), C18(H18A,H18B), C32(H32A,H32B), C17(H17A,H17B),
  C30(H30A,H30B), C48(H48A,H48B), C31(H31A,H31B), C45(H45A,H45B), C38(H38A,
 H38B), C36(H36A,H36B), C37(H37A,H37B), C43(H43A,H43B), C1A(H1AA,H1AB)
3.c Aromatic/amide H refined with riding coordinates:
 C7(H7), C2(H2), C21(H21), C8(H8), C23(H23), C14(H14), C11(H11), C13(H13),
 C12(H12), C15(H15), C5(H5), C6(H6)
3.d Idealised Me refined as rotating group:
 C25(H25A,H25B,H25C), C26(H26A,H26B,H26C), C27(H27A,H27B,H27C)
;
_shelx_res_checksum              12018
_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'