Ruthenium macrocycles bearing pyridine bis(carboxamide): synthesis, structure, and catalytic activity for hydrosilylation
Sato, Hiroki; Tsukamoto, Tadashi; Sogawa, Hiromitsu; Kuwata, Shigeki; Takata, Toshikazu; New Journal of Chemistry 45 (2021) 18282–18289; doi:10.1039/D0NJ06133F

data_7061047
_publ_section_title
;
 Ruthenium macrocycles bearing pyridine bis(carboxamide): synthesis,
 structure, and catalytic activity for hydrosilylation
;
_journal_issue                   39
_journal_name_full               'New Journal of Chemistry'
_journal_page_first              18282
_journal_page_last               18289
_journal_paper_doi               10.1039/D0NJ06133F
_journal_volume                  45
_journal_year                    2021
_chemical_formula_moiety         'C51 H50 N3 O10 P Ru, H2 O'
_chemical_formula_sum            'C51 H52 N3 O11 P Ru'
_chemical_formula_weight         1015.03
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_update_record
;
2020-02-01 deposited with the CCDC.	2021-08-30 downloaded from the CCDC.
;
_cell_angle_alpha                78.66(3)
_cell_angle_beta                 73.19(3)
_cell_angle_gamma                84.04(3)
_cell_formula_units_Z            2
_cell_length_a                   12.906(8)
_cell_length_b                   13.325(8)
_cell_length_c                   14.696(8)
_cell_measurement_reflns_used    6769
_cell_measurement_temperature    93
_cell_measurement_theta_max      27.46
_cell_measurement_theta_min      5.01
_cell_volume                     2369(2)
_computing_cell_refinement       CrystalClear
_computing_data_collection       'CrystalClear (Rigaku Inc., 2008)'
_computing_data_reduction        CrystalClear
_computing_molecular_graphics    'CrystalStructure 4.3'
_computing_publication_material  'CrystalStructure 4.3 (Rigaku, 2018)'
_computing_structure_refinement  'SHELXL Version 2014/7 (Sheldrick, 2008)'
_computing_structure_solution    'SIR92 (Altomare, et al., 1994)'
_diffrn_ambient_temperature      93
_diffrn_detector_area_resol_mean 7.111
_diffrn_measured_fraction_theta_full 0.979
_diffrn_measured_fraction_theta_max 0.956
_diffrn_measurement_device_type  'Rigaku Saturn724'
_diffrn_measurement_method       \w
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71075
_diffrn_reflns_av_R_equivalents  0.0577
_diffrn_reflns_av_unetI/netI     0.1597
_diffrn_reflns_Laue_measured_fraction_full 0.979
_diffrn_reflns_Laue_measured_fraction_max 0.956
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            19292
_diffrn_reflns_point_group_measured_fraction_full 0.979
_diffrn_reflns_point_group_measured_fraction_max 0.956
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.480
_diffrn_reflns_theta_min         3.035
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.429
_exptl_absorpt_correction_T_max  0.950
_exptl_absorpt_correction_T_min  0.677
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'REQAB (Rigaku, 1998)'
_exptl_crystal_colour            orange
_exptl_crystal_density_diffrn    1.423
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             1052.00
_exptl_crystal_recrystallization_method
'Re-crystallisation from solvent: benzene'
_exptl_crystal_size_max          0.240
_exptl_crystal_size_mid          0.130
_exptl_crystal_size_min          0.120
_refine_diff_density_max         1.67
_refine_diff_density_min         -0.60
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.896
_refine_ls_hydrogen_treatment    mixed
_refine_ls_number_parameters     610
_refine_ls_number_reflns         10379
_refine_ls_number_restraints     3
_refine_ls_R_factor_all          0.0784
_refine_ls_R_factor_gt           0.0573
_refine_ls_shift/su_max          0.001
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w = 1/[\s^2^(Fo^2^)+(0.0546P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1374
_refine_ls_wR_factor_ref         0.1454
_reflns_Friedel_coverage         0.000
_reflns_number_gt                6004
_reflns_number_total             10379
_reflns_threshold_expression     F^2^>2.0\s(F^2^)
_cod_data_source_file            d0nj06133f2.cif
_cod_data_source_block           RuMC33CO2PPh3
_cod_database_code               7061047
_shelx_res_checksum              16087