Cyclic (amino)(barrelene)carbene Ru-complexes: synthesis and reactivity in olefin metathesis.
Talcik, Jakub; Serrato, Melinda R.; Del Vecchio, Antonio; Colombel-Rouen, Sophie; Morvan, Jennifer; Roisnel, Thierry; Jazzar, Rodolphe; Melaimi, Mohand; Bertrand, Guy; Mauduit, Marc; Dalton transactions (Cambridge, England : 2003) 53 (2024) 5346–5350; doi:10.1039/d4dt00102h

data_7715279
_publ_section_title
;
 Cyclic (amino)(barrelene)carbene Ru-complexes: synthesis and reactivity
 in olefin metathesis.
;
_journal_issue                   12
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              5346
_journal_page_last               5350
_journal_paper_doi               10.1039/d4dt00102h
_journal_volume                  53
_journal_year                    2024
_chemical_compound_source        'synthesis as described'
_chemical_formula_moiety         'C36 H33 Cl2 N O Ru'
_chemical_formula_sum            'C36 H33 Cl2 N O Ru'
_chemical_formula_weight         667.60
_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'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_atom_sites_solution_secondary   difmap
_audit_update_record
;
2023-04-03 deposited with the CCDC.	2024-02-23 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 99.104(4)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   12.2592(11)
_cell_length_b                   14.8980(13)
_cell_length_c                   19.906(2)
_cell_measurement_reflns_used    9714
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      27.5107
_cell_measurement_theta_min      2.2851
_cell_measurement_wavelength     0.710730
_cell_volume                     3589.8(6)
_computing_cell_refinement       'APEX3 (Bruker, 2015)'
_computing_data_collection       'Bruker APEX3 (Bruker, 2015)'
_computing_data_reduction        'SAINT (Bruker, 2014)'
_computing_molecular_graphics
;
   'SXGRAPH (L. Farrugia, 1999), Mercury (CSD, 2020)'
;
_computing_publication_material  'CRYSCALC (T. Roisnel, local program, 2020)'
_computing_structure_refinement  'SHELXL-2018_3 (Sheldrick, 2018)'
_computing_structure_solution    'SHELXT 2018_2 (Sheldrick, 2018)'
_diffrn_ambient_temperature      150(2)
_diffrn_detector                 '(CMOS) PHOTON 100'
_diffrn_detector_area_resol_mean 10.4167
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.995
_diffrn_measurement_device_type  'D8 VENTURE Bruker AXS'
_diffrn_measurement_method       'rotation images'
_diffrn_orient_matrix_UB_11      0.0301654
_diffrn_orient_matrix_UB_12      -0.0114649
_diffrn_orient_matrix_UB_13      -0.0430346
_diffrn_orient_matrix_UB_21      0.0665429
_diffrn_orient_matrix_UB_22      -0.0291912
_diffrn_orient_matrix_UB_23      0.0267074
_diffrn_orient_matrix_UB_31      -0.0385589
_diffrn_orient_matrix_UB_32      -0.0593460
_diffrn_orient_matrix_UB_33      -0.0048231
_diffrn_radiation_monochromator  'multilayer monochromator'
_diffrn_radiation_probe          x-ray
_diffrn_radiation_source         'Incoatec microfocus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0472
_diffrn_reflns_av_unetI/netI     0.0360
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       25
_diffrn_reflns_limit_l_min       -25
_diffrn_reflns_number            39352
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.540
_diffrn_reflns_theta_min         2.168
_diffrn_source_current           1.00
_diffrn_source_power             50.0
_diffrn_source_voltage           50.00
_exptl_absorpt_coefficient_mu    0.611
_exptl_absorpt_correction_T_max  0.890
_exptl_absorpt_correction_T_min  0.757
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
  [Sheldrick, G.M. (2014). SADABS Bruker AXS Inc., Madison, Wisconsin, USA]
;
_exptl_crystal_colour            orange
_exptl_crystal_density_diffrn    1.235
_exptl_crystal_description       prism
_exptl_crystal_F_000             1368
_exptl_crystal_size_max          0.530
_exptl_crystal_size_mid          0.440
_exptl_crystal_size_min          0.190
_refine_diff_density_max         0.596
_refine_diff_density_min         -0.770
_refine_diff_density_rms         0.080
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.051
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     374
_refine_ls_number_reflns         8230
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.051
_refine_ls_R_factor_all          0.0430
_refine_ls_R_factor_gt           0.0334
_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^)+(0.0366P)^2^+3.8664P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0813
_refine_ls_wR_factor_ref         0.0874
_reflns_number_gt                6891
_reflns_number_total             8230
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            d4dt00102h2.cif
_cod_data_source_block           JM666
_cod_depositor_comments
'Adding full bibliography for 7715275--7715279.cif.'
_cod_original_cell_volume        3589.7(6)
_cod_original_sg_symbol_H-M      'P 21/c'
_cod_database_code               7715279
_shelx_res_checksum              63619
_shelx_fab_checksum              8845