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_4514658
_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         'C40 H48 Cl4 F12 Ru4'
_chemical_formula_sum            'C40 H48 Cl4 F12 Ru4'
_chemical_formula_weight         1302.86
_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   geom
_atom_sites_solution_primary     direct
_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                114.576(2)
_cell_angle_beta                 96.8470(10)
_cell_angle_gamma                99.3550(10)
_cell_formula_units_Z            4
_cell_length_a                   11.6853(6)
_cell_length_b                   20.7278(10)
_cell_length_c                   21.1082(10)
_cell_measurement_reflns_used    9354
_cell_measurement_temperature    100
_cell_measurement_theta_max      28.32
_cell_measurement_theta_min      2.23
_cell_volume                     4487.1(4)
_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, 2015)'
_diffrn_ambient_temperature      100
_diffrn_detector                 'Bruker APEX-II CCD'
_diffrn_detector_area_resol_mean 7.9
_diffrn_detector_type            'CCD Area Detector'
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measurement_device       'Kappa Four-Circle Diffractometer'
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_monochromator  'Double Bounce Multilayer Mirrors'
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0321
_diffrn_reflns_av_unetI/netI     0.0291
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.997
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       26
_diffrn_reflns_limit_k_min       -27
_diffrn_reflns_limit_l_max       25
_diffrn_reflns_limit_l_min       -28
_diffrn_reflns_number            98822
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.997
_diffrn_reflns_theta_full        26.000
_diffrn_reflns_theta_max         28.333
_diffrn_reflns_theta_min         1.085
_diffrn_source                   'Micro Focus Rotating Anode'
_diffrn_source_type              'Bruker TXS'
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    1.638
_exptl_absorpt_correction_T_max  0.0962
_exptl_absorpt_correction_T_min  0.0633
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2014/5 (Bruker,2014/5) was used for absorption correction.
wR2(int) was 0.0605 before and 0.0424 after correction.
The Ratio of minimum to maximum transmission is 0.6580.
The \l/2 correction factor is 0.00150.
;
_exptl_crystal_colour            brown
_exptl_crystal_colour_primary    brown
_exptl_crystal_density_diffrn    1.929
_exptl_crystal_description       block
_exptl_crystal_F_000             2560
_exptl_crystal_size_max          0.33
_exptl_crystal_size_mid          0.3
_exptl_crystal_size_min          0.27
_refine_diff_density_max         1.377
_refine_diff_density_min         -0.886
_refine_diff_density_rms         0.099
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.042
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1113
_refine_ls_number_reflns         22324
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.042
_refine_ls_R_factor_all          0.0397
_refine_ls_R_factor_gt           0.0285
_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^)+(0.0189P)^2^+8.9434P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0601
_refine_ls_wR_factor_ref         0.0654
_reflns_Friedel_coverage         0.000
_reflns_number_gt                18443
_reflns_number_total             22324
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            cs8b04345_si_002.cif
_cod_data_source_block           Rutetramerfig4
_cod_depositor_comments
;
The following automatic conversions were performed:

'_diffrn_radiation_probe' value 'X-ray' changed to 'x-ray' according
to
/home/data/users/saulius/crontab/automatic-downloads/current/ACS/lib/dictionaries/cif_core.dic
dictionary named 'cif_core.dic' version 2.4.2 from 2011-04-26.

Automatic conversion script
Id: cif_fix_values 4973 2017-02-22 13:04:09Z antanas 
;
_cod_database_code               4514658
_shelx_shelxl_version_number     2016/6
_shelx_estimated_absorpt_t_max   0.666
_shelx_estimated_absorpt_t_min   0.614
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.5 times of:
  All C(H,H,H) groups
2.a Idealised Me refined as rotating group:
 C018(H01A,H01B,H01C), C01K(H01D,H01E,H01F), C01S(H01G,H01H,H01I), C01X(H01J,
 H01K,H01L), C021(H02A,H02B,H02C), C022(H02D,H02E,H02F), C023(H02G,H02H,H02I),
 C024(H02Z,H,HA), C025(H02,HB,HC), C029(H02J,H02K,H02L), C02A(H02M,H02N,H02O),
 C02F(H02P,H02Q,H02R), C02H(H02S,H02T,H02U), C02L(H02V,H02W,H02X), C02M(H0AA,HD,
 HE), C02P(H1AA,HF,HG), C02R(H02Y,HH,HI), C02S(H2AA,HJ,HK), C02V(H3AA,HL,HM),
 C030(H03M,H03N,H03O), C031(H03P,H03Q,H03R), C032(H03S,H03T,H03U), C033(H03A,
 H03B,H03C), C034(H03V,H03W,H03X), C035(H03Y,HN,HO), C036(H03Z,HP,HQ),
 C037(H03D,H03E,H03F), C038(H03,HR,HS), C039(H03G,H03H,H03I), C03A(H03J,H03K,
 H03L), C03B(H4AA,HT,HU), C03C(H5AA,HV,HW)
;
_shelx_res_checksum              16555
_shelx_hkl_checksum              34921
_olex2_submission_special_instructions 'No special instructions were received'