Highly selective macrocyclic ring-closing metathesis of terminal olefins in non-chlorinated solvents at low dilution
DUMAS, Adrien; Colombel-Rouen, Sophie; Curbet, Idriss; Forcher, Gwénaël; Tripoteau, Fabien; Caijo, Frédéric; Rouen, Mathieu; Queval, Pierre; Basle, Olivier; Mauduit, Marc; Catalysis Science & Technology  (2019) –; doi:10.1039/C8CY02115E

data_1550289
_publ_section_title
;
 Highly selective macrocyclic ring-closing metathesis of terminal olefins
 in non-chlorinated solvents at low dilution
;
_journal_name_full               'Catalysis Science &amp; Technology'
_journal_paper_doi               10.1039/C8CY02115E
_journal_year                    2019
_chemical_formula_sum            'C53.5 H66 Cl3 N4 O1.5 Ru'
_chemical_formula_weight         996.52
_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   mixed
_audit_block_doi                 10.5517/cc148t9j
_audit_creation_method           SHELXL-2014/6
_audit_update_record
;
2015-02-25 deposited with the CCDC.
2018-11-26 downloaded from the CCDC.
;
_cell_angle_alpha                93.877(6)
_cell_angle_beta                 90.681(6)
_cell_angle_gamma                98.321(7)
_cell_formula_units_Z            4
_cell_length_a                   11.9610(10)
_cell_length_b                   16.5910(10)
_cell_length_c                   26.614(2)
_cell_measurement_reflns_used    4655
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      25.6250
_cell_measurement_theta_min      3.2560
_cell_volume                     5212.6(7)
_computing_cell_refinement
'CrysAlis RED, Oxford Diffraction Ltd.,Version 1.171.37.35'
_computing_data_collection
'CrysAlis CCD, Oxford Diffraction Ltd.,Version 1.171.37.35'
_computing_data_reduction
'CrysAlis RED, Oxford Diffraction Ltd.,Version 1.171.37.35'
_computing_molecular_graphics    'MERCURY 3.3(CCDC, 2014)'
_computing_publication_material  'WINGX (Farrugia, 1999)'
_computing_structure_refinement  'SHELXL-2014/6 (Sheldrick, 2014)'
_computing_structure_solution    'SIR-97_(Altomare & al., 1999)'
_diffrn_ambient_temperature      150(2)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 16.1852
_diffrn_detector_type            Sapphire3
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'Xcalibur, Sapphire3'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0840
_diffrn_reflns_av_unetI/netI     0.1736
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -21
_diffrn_reflns_limit_l_max       29
_diffrn_reflns_limit_l_min       -33
_diffrn_reflns_number            43396
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         26.999
_diffrn_reflns_theta_min         2.950
_exptl_absorpt_coefficient_mu    0.496
_exptl_absorpt_correction_T_max  0.992
_exptl_absorpt_correction_T_min  0.933
_exptl_absorpt_correction_type   analytical
_exptl_absorpt_process_details
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.35h (release 09-02-2015 CrysAlis171 .NET)
(compiled Feb  9 2015,16:26:32)
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            yellow
_exptl_crystal_density_diffrn    1.270
_exptl_crystal_description       plate
_exptl_crystal_F_000             2088
_exptl_crystal_size_max          0.342
_exptl_crystal_size_mid          0.086
_exptl_crystal_size_min          0.028
_refine_diff_density_max         1.606
_refine_diff_density_min         -1.020
_refine_diff_density_rms         0.152
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.982
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1112
_refine_ls_number_reflns         22728
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.982
_refine_ls_R_factor_all          0.1584
_refine_ls_R_factor_gt           0.0815
_refine_ls_shift/su_max          0.004
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0984P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1870
_refine_ls_wR_factor_ref         0.2286
_reflns_Friedel_coverage         0.000
_reflns_number_gt                12260
_reflns_number_total             22728
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c8cy02115e2.cif
_cod_data_source_block           shelx
_cod_depositor_comments
;

2019-02-15
Z value and formula fixed to values more according to usual
chemical conventions.                 miguel
;
_cod_original_formula_sum            'C107 H132 Cl6 N8 O3 Ru2'
_cod_original_formula_weight         1993.04
_cod_original_formula_units_Z            2
_cod_database_code               1550289
_shelxl_version_number           2014/6
_shelx_res_checksum              76715