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_7035202
_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         'C38 H57 Cl2 N2 P Ru'
_chemical_formula_sum            'C38 H57 Cl2 N2 P Ru'
_chemical_formula_weight         744.80
_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             2014-12-17
_audit_creation_method
;
Olex2 1.2
(compiled 2014.11.28 svn.r3107 for OlexSys, GUI svn.r4959)
;
_audit_update_record
;
2015-02-13 deposited with the CCDC.
2015-05-15 downloaded from the CCDC.
;
_cell_angle_alpha                67.575(4)
_cell_angle_beta                 84.781(3)
_cell_angle_gamma                74.448(3)
_cell_formula_units_Z            2
_cell_length_a                   11.9873(5)
_cell_length_b                   12.0758(4)
_cell_length_c                   13.9907(6)
_cell_measurement_reflns_used    8829
_cell_measurement_temperature    100.0(1)
_cell_measurement_theta_max      74.8810
_cell_measurement_theta_min      3.3990
_cell_volume                     1803.40(14)
_computing_cell_refinement
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.34 (release 22-05-2014 CrysAlis171 .NET)
(compiled May 22 2014,16:03:01)
;
_computing_data_collection
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.34 (release 22-05-2014 CrysAlis171 .NET)
(compiled May 22 2014,16:03:01)
;
_computing_data_reduction
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.34 (release 22-05-2014 CrysAlis171 .NET)
(compiled May 22 2014,16:03:01)
;
_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    'olex2.solve (Bourhis et al., 2015)'
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      100.0(1)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 10.4839
_diffrn_detector_type            Atlas
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.969
_diffrn_measurement_details
;
  1 omega -106.00  -12.00   1.0000    2.5000
omega____ theta____ kappa____ phi______ frames
    -      -41.6798  144.0000   46.0000 94

  2 omega -114.00  -61.00   1.0000    2.5000
omega____ theta____ kappa____ phi______ frames
    -      -41.6798 -144.0000   -7.0000 53

  3 omega  -97.00   -3.00   1.0000    2.5000
omega____ theta____ kappa____ phi______ frames
    -      -41.6798  127.0000 -122.0000 94

  4 omega   34.00  110.00   1.0000    2.5000
omega____ theta____ kappa____ phi______ frames
    -       41.6798 -144.0000   -7.0000 76

  5 omega   93.00  178.00   1.0000    5.0000
omega____ theta____ kappa____ phi______ frames
    -      109.1316  127.0000 -122.0000 85

  6 omega   37.00  131.00   1.0000    5.0000
omega____ theta____ kappa____ phi______ frames
    -      109.1316 -144.0000   -7.0000 94

  7 omega   36.00  122.00   1.0000    5.0000
omega____ theta____ kappa____ phi______ frames
    -      109.1316 -127.0000  161.0000 86

  8 omega   83.00  176.00   1.0000    5.0000
omega____ theta____ kappa____ phi______ frames
    -      109.1316  144.0000   46.0000 93

  9 omega -116.00  -17.00   1.0000    2.5000
omega____ theta____ kappa____ phi______ frames
    -      -41.6798  -38.0000   60.0000 99

 10 omega -116.00  -17.00   1.0000    2.5000
omega____ theta____ kappa____ phi______ frames
    -      -41.6798  -38.0000  -30.0000 99

 11 omega    1.00   83.00   1.0000    2.5000
omega____ theta____ kappa____ phi______ frames
    -       41.6798  -99.0000 -150.0000 82

 12 omega  -33.00   66.00   1.0000    2.5000
omega____ theta____ kappa____ phi______ frames
    -       41.6798  -38.0000 -150.0000 99

 13 omega   33.00  142.00   1.0000    5.0000
omega____ theta____ kappa____ phi______ frames
    -      109.1316  -77.0000 -180.0000 109

 14 omega   83.00  178.00   1.0000    5.0000
omega____ theta____ kappa____ phi______ frames
    -      109.1316   45.0000  -90.0000 95

 15 omega   37.00  138.00   1.0000    5.0000
omega____ theta____ kappa____ phi______ frames
    -      109.1316  -61.0000  120.0000 101

 16 omega   33.00   91.00   1.0000    5.0000
omega____ theta____ kappa____ phi______ frames
    -      109.1316  -30.0000 -180.0000 58

 17 omega   33.00   91.00   1.0000    5.0000
omega____ theta____ kappa____ phi______ frames
    -      109.1316  -30.0000    0.0000 58

 18 omega   77.00  178.00   1.0000    5.0000
omega____ theta____ kappa____ phi______ frames
    -      109.1316   77.0000  -60.0000 101

 19 omega   36.00   98.00   1.0000    5.0000
omega____ theta____ kappa____ phi______ frames
    -      109.1316  -45.0000  -30.0000 62

 20 omega   34.00  140.00   1.0000    5.0000
omega____ theta____ kappa____ phi______ frames
    -      109.1316  -77.0000  -30.0000 106

 21 omega   81.00  178.00   1.0000    5.0000
omega____ theta____ kappa____ phi______ frames
    -      109.1316   30.0000    0.0000 97
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at zero, Atlas'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_UB_11      -0.0465940000
_diffrn_orient_matrix_UB_12      0.0565344000
_diffrn_orient_matrix_UB_13      -0.1120357000
_diffrn_orient_matrix_UB_21      0.1185958000
_diffrn_orient_matrix_UB_22      0.0244132000
_diffrn_orient_matrix_UB_23      -0.0397794000
_diffrn_orient_matrix_UB_31      0.0395287000
_diffrn_orient_matrix_UB_32      -0.1286991000
_diffrn_orient_matrix_UB_33      -0.0076053000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0415
_diffrn_reflns_av_unetI/netI     0.0446
_diffrn_reflns_laue_measured_fraction_full 0.998
_diffrn_reflns_laue_measured_fraction_max 0.969
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            20352
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.969
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         75.388
_diffrn_reflns_theta_min         3.418
_diffrn_source                   'sealed X-ray tube'
_diffrn_source_type              'SuperNova (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    5.507
_exptl_absorpt_correction_T_max  0.913
_exptl_absorpt_correction_T_min  0.820
_exptl_absorpt_correction_type   analytical
_exptl_absorpt_process_details
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.34 (release 22-05-2014 CrysAlis171 .NET)
(compiled May 22 2014,16:03:01)
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)
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    1.372
_exptl_crystal_description       plate
_exptl_crystal_F_000             784
_exptl_crystal_size_max          0.0968
_exptl_crystal_size_mid          0.0658
_exptl_crystal_size_min          0.0377
_refine_diff_density_max         0.731
_refine_diff_density_min         -1.303
_refine_diff_density_rms         0.073
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.031
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     401
_refine_ls_number_reflns         7221
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.031
_refine_ls_R_factor_all          0.0458
_refine_ls_R_factor_gt           0.0360
_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^)+(0.0445P)^2^+0.8253P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0874
_refine_ls_wR_factor_ref         0.0933
_reflns_Friedel_coverage         0.000
_reflns_number_gt                6186
_reflns_number_total             7221
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c5dt00967g2.cif
_cod_data_source_block           fv089
_cod_depositor_comments
'Adding full bibliography for 7035200--7035203.cif.'
_cod_database_code               7035202
_shelxl_version_number           2013-4
_chemical_oxdiff_formula         'C38 H57 Cl2 N2 P Ru'
_reflns_odcompleteness_completeness 99.94
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     66.97
_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.a Ternary CH refined with riding coordinates:
 C21(H21), C27(H27), C33(H33)
2.b Secondary CH2 refined with riding coordinates:
 C9(H9A,H9B), C10(H10A,H10B), C22(H22A,H22B), C23(H23A,H23B), C24(H24A,H24B),
 C25(H25A,H25B), C26(H26A,H26B), C28(H28A,H28B), C29(H29A,H29B), C30(H30A,H30B),
  C31(H31A,H31B), C32(H32A,H32B), C34(H34A,H34B), C35(H35A,H35B), C36(H36A,
 H36B), C37(H37A,H37B), C38(H38A,H38B)
2.c Aromatic/amide H refined with riding coordinates:
 C1(H1), C3(H3), C4(H4), C5(H5), C6(H6), C7(H7), C13(H13), C15(H15)
2.d Idealised Me refined as rotating group:
 C17(H17A,H17B,H17C), C18(H18A,H18B,H18C), C19(H19A,H19B,H19C), C20(H20A,H20B,
 H20C)
;
_shelx_res_checksum              38527
_ins_header
;
TITL FV089 in P-1 
REM P-1 (#2 in standard setting)
CELL 1.54184  11.987287  12.075808  13.990677  67.5749  84.7809  74.4483
ZERR    4.00   0.000469   0.000403   0.000600   0.0036   0.0033   0.0032
LATT  1
SFAC C H N P Cl Ru
UNIT 80.00 80.00 8.00 4.00 8.00 4.00
TREF
HKLF 4
END
;
_olex2_date_sample_data_collection 2014-11-25
_olex2_exptl_crystal_mounting_method 'mounted on a nylon loop'
_olex2_submission_special_instructions 'No special instructions were received'