Synthesis and characterization of non-chelating ruthenium‒indenylidene olefin metathesis catalysts derived from substituted 1,1-diphenyl-2-propyn-1-ols
Yu, Baoyi; Xie, Yu; Hamad, Fatma B.; Leus, Karen; Lyapkov, Alex A.; Van Hecke, Kristof; Verpoort, Francis; New J. Chem. 39 (2015) 1858–; doi:10.1039/C4NJ02034K

data_7054598
_publ_section_title
;
 Synthesis and characterization of non-chelating ruthenium--indenylidene
 olefin metathesis catalysts derived from substituted
 1,1-diphenyl-2-propyn-1-ols
;
_journal_issue                   3
_journal_name_full               'New J. Chem.'
_journal_page_first              1858
_journal_paper_doi               10.1039/C4NJ02034K
_journal_volume                  39
_journal_year                    2015
_chemical_formula_moiety         'C28 H45 Cl2 O P Ru'
_chemical_formula_sum            'C28 H45 Cl2 O P Ru'
_chemical_formula_weight         600.58
_chemical_name_systematic
;
 ? 
;
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2ybc'
_space_group_name_H-M_alt        'P 1 21/c 1'
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_date             2014-01-02
_audit_creation_method
;
  Olex2 1.2
  (compiled 2013.04.25 svn.r2679, GUI svn.r4466)
;
_audit_update_record
;
2014-02-14 deposited with the CCDC.
2014-12-17 downloaded from the CCDC.
;
_cell_angle_alpha                90.00
_cell_angle_beta                 96.478(2)
_cell_angle_gamma                90.00
_cell_formula_units_Z            8
_cell_length_a                   11.4775(3)
_cell_length_b                   19.2194(5)
_cell_length_c                   25.7969(6)
_cell_measurement_reflns_used    8246
_cell_measurement_temperature    100.0(1)
_cell_measurement_theta_max      28.1430
_cell_measurement_theta_min      3.6230
_cell_volume                     5654.2(2)
_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
;
O. V. Dolomanov, L. J. Bourhis, R. J. Gildea, J. A. K. Howard and H. Puschmann,
OLEX2: a complete structure solution, refinement and analysis program.
J. Appl. Cryst. (2009). 42, 339-341.
;
_computing_publication_material
;
O. V. Dolomanov, L. J. Bourhis, R. J. Gildea, J. A. K. Howard and H. Puschmann,
OLEX2: a complete structure solution, refinement and analysis program.
J. Appl. Cryst. (2009). 42, 339-341.
;
_computing_structure_refinement
;
SHELXL, G.M. Sheldrick, Acta Cryst.
(2008). A64, 112-122
;
_computing_structure_solution
;
SHELXS, G.M. Sheldrick, Acta Cryst.
(2008). A64, 112-122
;
_diffrn_ambient_temperature      100.0(1)
_diffrn_detector_area_resol_mean 10.4839
_diffrn_measured_fraction_theta_full 0.9982
_diffrn_measured_fraction_theta_max 0.9982
_diffrn_measurement_details
;
  1 omega  -40.00    8.00   1.0000   15.0000
omega____ theta____ kappa____ phi______ frames
    -       10.3260  -36.0000  168.0000 48

  2 omega  -12.00   50.00   1.0000   15.0000
omega____ theta____ kappa____ phi______ frames
    -       10.3260   36.0000  -35.0000 62

  3 omega    1.00   64.00   1.0000   15.0000
omega____ theta____ kappa____ phi______ frames
    -       10.3260 -124.0000   22.6079 63

  4 omega  -76.00  -13.00   1.0000   15.0000
omega____ theta____ kappa____ phi______ frames
    -      -10.9510  -19.0000   90.0000 63

  5 omega  -10.00   30.00   1.0000   15.0000
omega____ theta____ kappa____ phi______ frames
    -      -10.9510  -19.0000   90.0000 40

  6 omega  -16.00   25.00   1.0000   15.0000
omega____ theta____ kappa____ phi______ frames
    -      -10.9510  -99.0000  150.0000 41

  7 omega  -77.00  -47.00   1.0000   15.0000
omega____ theta____ kappa____ phi______ frames
    -      -10.9510  149.0000  -43.1771 30
;
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at zero, Atlas'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_UB_11      -0.0430651000
_diffrn_orient_matrix_UB_12      0.0067574000
_diffrn_orient_matrix_UB_13      -0.0213582000
_diffrn_orient_matrix_UB_21      -0.0364020000
_diffrn_orient_matrix_UB_22      0.0156760000
_diffrn_orient_matrix_UB_23      0.0171569000
_diffrn_orient_matrix_UB_31      0.0262965000
_diffrn_orient_matrix_UB_32      0.0327224000
_diffrn_orient_matrix_UB_33      -0.0038250000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.7107
_diffrn_reflns_av_R_equivalents  0.1085
_diffrn_reflns_av_unetI/netI     0.1281
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       24
_diffrn_reflns_limit_k_min       -23
_diffrn_reflns_limit_l_max       27
_diffrn_reflns_limit_l_min       -32
_diffrn_reflns_number            47765
_diffrn_reflns_theta_full        26.37
_diffrn_reflns_theta_max         26.37
_diffrn_reflns_theta_min         2.77
_diffrn_source                   'SuperNova (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    0.819
_exptl_absorpt_correction_T_max  0.994
_exptl_absorpt_correction_T_min  0.988
_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    1.411
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             2512
_exptl_crystal_size_max          0.1888
_exptl_crystal_size_mid          0.0893
_exptl_crystal_size_min          0.082
_refine_diff_density_max         1.007
_refine_diff_density_min         -1.139
_refine_diff_density_rms         0.130
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.968
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     599
_refine_ls_number_reflns         11553
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.968
_refine_ls_R_factor_all          0.1065
_refine_ls_R_factor_gt           0.0543
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0384P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1042
_refine_ls_wR_factor_ref         0.1250
_reflns_number_gt                7197
_reflns_number_total             11553
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c4nj02034k2.cif
_cod_data_source_block           fv062
_cod_depositor_comments
'Adding full bibliography for 7054596--7054603.cif.'
_cod_database_code               7054598
_chemical_oxdiff_formula         'Ru C35 H40 O1 Cl2 P1'
_reflns_odcompleteness_completeness 99.82
_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.a Ternary CH refined with riding coordinates:
 C11(H11), C11A(H11A), C17A(H17A), C17(H17), C23(H23), C8A(H8A), C23A(H23A),
 C8(H8)
2.b Secondary CH2 refined with riding coordinates:
 C28A(H28C,H28D), C14A(H14C,H14D), C16(H16A,H16B), C28(H28A,H28B), C14(H14A,
 H14B), C13A(H13C,H13D), C12(H12A,H12B), C26(H26A,H26B), C18A(H18C,H18D),
 C21A(H21C,H21D), C15A(H15C,H15D), C16A(H16C,H16D), C13(H13A,H13B), C15(H15A,
 H15B), C27(H27A,H27B), C24(H24A,H24B), C22(H22A,H22B), C18(H18A,H18B),
 C12A(H12C,H12D), C25(H25A,H25B), C19A(H19C,H19D), C25A(H25C,H25D), C22A(H22C,
 H22D), C24A(H24C,H24D), C26A(H26C,H26D), C20A(H20C,H20D), C27A(H27C,H27D),
 C20(H20A,H20B), C19(H19A,H19B), C21(H21A,H21B)
2.c Aromatic/amide H refined with riding coordinates:
 C1A(H1A), C1(H1), C4A(H4A), C3A(H3A), C6A(H6A), C4(H4), C6(H6), C3(H3),
 C5(H5), C5A(H5A)
2.d Idealised Me refined as rotating group:
 C10(H10A,H10B,H10C), C9A(H9AA,H9AB,H9AC), C9(H9A,H9B,H9C), C10A(H10D,H10E,H10F)
;