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_7054600
_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         'C17 H16 O'
_chemical_formula_sum            'C17 H16 O'
_chemical_formula_weight         236.30
_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             2013-01-02
_audit_creation_method
;
  Olex2 1.2
  (compiled Dec  5 2012 16:20:19, GUI svn.r4385)
;
_audit_update_record
;
2014-05-27 deposited with the CCDC.
2014-12-17 downloaded from the CCDC.
;
_cell_angle_alpha                90.00
_cell_angle_beta                 92.308(3)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   6.6764(2)
_cell_length_b                   16.5673(6)
_cell_length_c                   11.6107(3)
_cell_measurement_reflns_used    2821
_cell_measurement_temperature    100.0(1)
_cell_measurement_theta_max      74.0830
_cell_measurement_theta_min      4.6460
_cell_volume                     1283.22(7)
_computing_cell_refinement
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.24 (release 03-12-2012 CrysAlis171 .NET)
(compiled Dec  3 2012,18:21:49)
;
_computing_data_collection
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.24 (release 03-12-2012 CrysAlis171 .NET)
(compiled Dec  3 2012,18:21:49)
;
_computing_data_reduction
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.24 (release 03-12-2012 CrysAlis171 .NET)
(compiled Dec  3 2012,18:21:49)
;
_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 0.9971
_diffrn_measured_fraction_theta_max 0.9971
_diffrn_measurement_details
;
  1 omega  -44.00  -19.00   1.0000    1.0000
omega____ theta____ kappa____ phi______ frames
    -      -41.6798   55.0000   80.0000 25

  2 omega  -33.00   18.00   1.0000    1.0000
omega____ theta____ kappa____ phi______ frames
    -      -41.6798   55.0000   63.0000 51

  3 omega    8.00   68.00   1.0000    1.0000
omega____ theta____ kappa____ phi______ frames
    -       41.6798  -55.0000  -80.0000 60

  4 omega   16.00   67.00   1.0000    1.0000
omega____ theta____ kappa____ phi______ frames
    -       41.6798   55.0000 -116.0000 51

  5 omega -113.00  -34.00   1.0000    1.0000
omega____ theta____ kappa____ phi______ frames
    -      -43.5000  -55.0000  116.0000 79

  6 omega   75.00  109.00   1.0000    1.0000
omega____ theta____ kappa____ phi______ frames
    -      109.1316  -55.0000  -63.0000 34

  7 omega   82.00  108.00   1.0000    1.0000
omega____ theta____ kappa____ phi______ frames
    -      109.1316   55.0000 -116.0000 26

  8 omega  110.00  136.00   1.0000    1.0000
omega____ theta____ kappa____ phi______ frames
    -      109.1316   55.0000  -99.0000 26

  9 omega   51.00   76.00   1.0000    1.0000
omega____ theta____ kappa____ phi______ frames
    -      109.1316  -55.0000  -80.0000 25

 10 omega -126.00  -89.00   1.0000    1.0000
omega____ theta____ kappa____ phi______ frames
    -      -43.5000  -94.0000   30.0000 37

 11 omega   33.00   89.00   1.0000    1.0000
omega____ theta____ kappa____ phi______ frames
    -      109.1316  -30.0000 -150.0000 56

 12 omega   46.00   97.00   1.0000    1.0000
omega____ theta____ kappa____ phi______ frames
    -      109.1316  -45.0000  120.0000 51

 13 omega   39.00   91.00   1.0000    1.0000
omega____ theta____ kappa____ phi______ frames
    -      109.1316  -30.0000  -90.0000 52

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

 15 omega   35.00   64.00   1.0000    1.0000
omega____ theta____ kappa____ phi______ frames
    -      109.1316  -30.0000 -180.0000 29

 16 omega   81.00  178.00   1.0000    1.0000
omega____ theta____ kappa____ phi______ frames
    -      109.1316   30.0000 -180.0000 97
;
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at zero, Atlas'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_UB_11      -0.1740263000
_diffrn_orient_matrix_UB_12      -0.0597328000
_diffrn_orient_matrix_UB_13      0.0146097000
_diffrn_orient_matrix_UB_21      0.0628513000
_diffrn_orient_matrix_UB_22      -0.0101273000
_diffrn_orient_matrix_UB_23      0.1284309000
_diffrn_orient_matrix_UB_31      -0.1380025000
_diffrn_orient_matrix_UB_32      0.0705797000
_diffrn_orient_matrix_UB_33      0.0308568000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_type           'Cu K\a'
_diffrn_radiation_wavelength     1.5418
_diffrn_reflns_av_R_equivalents  0.0233
_diffrn_reflns_av_unetI/netI     0.0269
_diffrn_reflns_limit_h_max       5
_diffrn_reflns_limit_h_min       -7
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       13
_diffrn_reflns_limit_l_min       -13
_diffrn_reflns_number            5337
_diffrn_reflns_theta_full        66.59
_diffrn_reflns_theta_max         66.59
_diffrn_reflns_theta_min         4.65
_diffrn_source                   'SuperNova (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    0.574
_exptl_absorpt_correction_T_max  0.971
_exptl_absorpt_correction_T_min  0.896
_exptl_absorpt_correction_type   analytical
_exptl_absorpt_process_details
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.24 (release 03-12-2012 CrysAlis171 .NET)
(compiled Dec  3 2012,18:21:49)
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            colourless
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.223
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             504
_exptl_crystal_size_max          0.3825
_exptl_crystal_size_mid          0.2452
_exptl_crystal_size_min          0.0662
_refine_diff_density_max         0.186
_refine_diff_density_min         -0.211
_refine_diff_density_rms         0.042
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.062
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     166
_refine_ls_number_reflns         2252
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.062
_refine_ls_R_factor_all          0.0450
_refine_ls_R_factor_gt           0.0383
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0605P)^2^+0.1596P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1005
_refine_ls_wR_factor_ref         0.1072
_reflns_number_gt                1907
_reflns_number_total             2252
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c4nj02034k2.cif
_cod_data_source_block           fv021
_cod_depositor_comments
'Adding full bibliography for 7054596--7054603.cif.'
_cod_database_code               7054600
_chemical_oxdiff_formula         'C17 H16 O1'
_reflns_odcompleteness_completeness 99.71
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     66.97
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  H5 of C5, H7 of C7, H9 of C9, H10 of C10, H11 of C11, H12 of C12, H16 of
  C16, H3 of C3, H4 of C4
 At 1.5 times of:
  {H14A,H14B,H14C} of C14, {H17A,H17B,H17C} of C17, H1 of O1
2.a Aromatic/amide H refined with riding coordinates:
 C3(H3), C4(H4), C5(H5), C7(H7), C9(H9), C10(H10), C11(H11), C12(H12)
2.b Idealised Me refined as rotating group:
 C14(H14A,H14B,H14C), C17(H17A,H17B,H17C)
2.c Idealised tetrahedral OH refined as rotating group:
 O1(H1)
2.d :
 C16(H16)
;