Dynamic π-Bonding of Imidazolyl Substituent in a Formally 16-Electron Cp*Ru(κ2-P,N)+ Catalyst Allows Dramatic Rate Increases in (E)-Selective Monoisomerization of Alkenes
Paulson, Erik R.; Moore, Curtis E.; Rheingold, Arnold L.; Pullman, David P.; Sindewald, Ryan W.; Cooksy, Andrew L.; Grotjahn, Douglas B.; ACS Catalysis 9 (2019) 7217–; doi:10.1021/acscatal.8b04345

data_4514657
_publ_section_title
;
 Dynamic \p-Bonding of Imidazolyl Substituent in a Formally 16-Electron
 Cp*Ru(\k2-P,N)+ Catalyst Allows Dramatic Rate Increases in (E)-Selective
 Monoisomerization of Alkenes
;
_journal_issue                   8
_journal_name_full               'ACS Catalysis'
_journal_page_first              7217
_journal_paper_doi               10.1021/acscatal.8b04345
_journal_volume                  9
_journal_year                    2019
_chemical_formula_moiety         'C24 H39 F3 N2 P Ru, F6 P'
_chemical_formula_sum            'C24 H39 F9 N2 P2 Ru'
_chemical_formula_weight         689.58
_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
_audit_creation_date             2018-10-22
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_cell_angle_alpha                90
_cell_angle_beta                 113.1800(10)
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   22.5581(7)
_cell_length_b                   12.7798(4)
_cell_length_c                   22.1335(7)
_cell_measurement_reflns_used    9790
_cell_measurement_temperature    100
_cell_measurement_theta_max      28.30
_cell_measurement_theta_min      2.53
_cell_volume                     5865.7(3)
_computing_cell_refinement       'SAINT v8.34A (Bruker, 2013)'
_computing_data_collection       'APEX2 v2013.6-2 (Bruker, 2013)'
_computing_data_reduction        'SAINT v8.34A (Bruker, 2013)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'XL (Sheldrick, 2008)'
_computing_structure_solution    'ShelXT (Sheldrick, 2008)'
_diffrn_ambient_temperature      100.0
_diffrn_detector_area_resol_mean 7.9
_diffrn_detector_type            'CCD Area Detector'
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.995
_diffrn_measurement_device       'Kappa Four-Circle Diffractometer'
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0387
_diffrn_reflns_av_unetI/netI     0.0288
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.995
_diffrn_reflns_limit_h_max       29
_diffrn_reflns_limit_h_min       -30
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -29
_diffrn_reflns_number            59436
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.995
_diffrn_reflns_theta_full        26.000
_diffrn_reflns_theta_max         28.326
_diffrn_reflns_theta_min         0.982
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.718
_exptl_absorpt_correction_T_max  0.0962
_exptl_absorpt_correction_T_min  0.0663
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2014/5 (Bruker,2014/5) was used for absorption correction.
wR2(int) was 0.1261 before and 0.0483 after correction.
The Ratio of minimum to maximum transmission is 0.6892.
The \l/2 correction factor is 0.00150.
;
_exptl_crystal_colour            blue
_exptl_crystal_colour_primary    blue
_exptl_crystal_density_diffrn    1.562
_exptl_crystal_description       plate
_exptl_crystal_F_000             2816
_exptl_crystal_size_max          0.28
_exptl_crystal_size_mid          0.16
_exptl_crystal_size_min          0.08
_refine_diff_density_max         1.865
_refine_diff_density_min         -1.263
_refine_diff_density_rms         0.088
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.029
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     709
_refine_ls_number_reflns         14544
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.029
_refine_ls_R_factor_all          0.0468
_refine_ls_R_factor_gt           0.0372
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0458P)^2^+7.7748P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0948
_refine_ls_wR_factor_ref         0.1040
_reflns_Friedel_coverage         0.000
_reflns_number_gt                12155
_reflns_number_total             14544
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            cs8b04345_si_005.cif
_cod_data_source_block           Complex6
_cod_database_code               4514657
_shelx_shelxl_version_number     2016/6
_shelx_estimated_absorpt_t_max   0.945
_shelx_estimated_absorpt_t_min   0.824
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2.a Ternary CH refined with riding coordinates:
 C47(H47), C23(H23), C44(H44), C20(H20)
2.b Aromatic/amide H refined with riding coordinates:
 C36(H36), C12(H12)
2.c Idealised Me refined as rotating group:
 C33(H33A,H33B,H33C), C24(H24A,H24B,H24C), C21(H21A,H21B,H21C), C38(H38A,H38B,
 H38C), C46(H46A,H46B,H46C), C43(H43A,H43B,H43C), C14(H14A,H14B,H14C), C16(H16A,
 H16B,H16C), C31(H31A,H31B,H31C), C48(H48A,H48B,H48C), C9(H9A,H9B,H9C),
 C41(H41A,H41B,H41C), C40(H40A,H40B,H40C), C8(H8A,H8B,H8C), C34(H34A,H34B,H34C),
  C7(H7A,H7B,H7C), C19(H19A,H19B,H19C), C17(H17A,H17B,H17C), C45(H45A,H45B,
 H45C), C42(H42A,H42B,H42C), C10(H10A,H10B,H10C), C32(H32A,H32B,H32C), C18(H18A,
 H18B,H18C), C22(H22A,H22B,H22C)
;
_shelx_res_checksum              27059
_shelx_hkl_checksum              48505
_olex2_submission_special_instructions 'No special instructions were received'