Developing P-Stereogenic, Planar‒Chiral P-Alkene Ligands: Monodentate, Bidentate, and Double Agostic Coordination Modes on Ru(II)
Herrera, Alberto; Grasruck, Alexander; Heinemann, Frank W.; Scheurer, Andreas; Chelouan, Ahmed; Frieß, Sibylle; Seidel, Falk; Dorta, Romano; Organometallics 36 (2017) 714–; doi:10.1021/acs.organomet.6b00879

data_4087143
_publ_section_title
;
 Developing P-Stereogenic, Planar--Chiral P-Alkene Ligands: Monodentate,
 Bidentate, and Double Agostic Coordination Modes on Ru(II)
;
_journal_issue                   3
_journal_name_full               Organometallics
_journal_page_first              714
_journal_paper_doi               10.1021/acs.organomet.6b00879
_journal_volume                  36
_journal_year                    2017
_chemical_formula_moiety         'C50 H52 Cl2 N2 P2 Ru'
_chemical_formula_sum            'C50 H52 Cl2 N2 P2 Ru'
_chemical_formula_weight         914.84
_chemical_name_systematic
;
 ? 
;
_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             2015-12-02
_audit_creation_method
;
Olex2 1.2
(compiled 2015.09.30 svn.r3233 for OlexSys, GUI svn.r5103)
;
_cell_angle_alpha                90
_cell_angle_beta                 90.620(3)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   30.553(4)
_cell_length_b                   10.4072(13)
_cell_length_c                   13.7519(17)
_cell_measurement_reflns_used    5823
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      23.68
_cell_measurement_theta_min      2.37
_cell_volume                     4372.5(10)
_computing_cell_refinement       'Bruker SAINT'
_computing_data_collection       'Bruker APEX2'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    'SHELXTL 6.12 (Bruker AXS, 2002)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL-2014/6 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXTL 6.12 (Bruker AXS, 2002)'
_diffrn_ambient_temperature      100.15
_diffrn_detector_area_resol_mean 83.33
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.995
_diffrn_measurement_device_type  'Bruker Kappa APEX II CCD area detector'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_radiation_monochromator  'Quazar focussing montel optics'
_diffrn_radiation_source         'ImuS micro-focus tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.1008
_diffrn_reflns_av_unetI/netI     0.0682
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.995
_diffrn_reflns_limit_h_max       39
_diffrn_reflns_limit_h_min       -39
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            62978
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.995
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.138
_diffrn_reflns_theta_min         1.333
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.591
_exptl_absorpt_correction_T_max  0.7455
_exptl_absorpt_correction_T_min  0.7058
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2014/4 (Bruker,2014/4) was used for absorption correction.
wR2(int) was 0.0791 before and 0.0649 after correction.
The Ratio of minimum to maximum transmission is 0.9467.
The \l/2 correction factor is 0.00150.
;
_exptl_crystal_colour            violet
_exptl_crystal_density_diffrn    1.390
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             1896
_exptl_crystal_size_max          0.18
_exptl_crystal_size_mid          0.1
_exptl_crystal_size_min          0.05
_refine_diff_density_max         0.696
_refine_diff_density_min         -0.708
_refine_diff_density_rms         0.103
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.056
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     522
_refine_ls_number_reflns         9651
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.056
_refine_ls_R_factor_all          0.0828
_refine_ls_R_factor_gt           0.0479
_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^)+(0.0266P)^2^+8.6034P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0908
_refine_ls_wR_factor_ref         0.1043
_reflns_Friedel_coverage         0.000
_reflns_number_gt                6823
_reflns_number_total             9651
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            om6b00879_si_001.cif
_cod_data_source_block           rd1511
_cod_original_cell_volume        4372.5(9)
_cod_database_code               4087143
_shelxl_version_number           2014/6
_shelx_estimated_absorpt_t_max   0.971
_shelx_estimated_absorpt_t_min   0.901
_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 Aromatic/amide H refined with riding coordinates:
 C2(H2), C3(H3), C4(H4), C5(H5), C8(H8), C10(H10), C11(H11), C12(H12),
 C13(H13), C16(H16), C17(H17), C18(H18), C19(H19), C20(H20), C27(H27), C28(H28),
  C29(H29), C30(H30), C33(H33), C35(H35), C36(H36), C37(H37), C38(H38),
 C41(H41), C42(H42), C43(H43), C44(H44), C45(H45)
2.b Idealised Me refined as rotating group:
 C22(H22A,H22B,H22C), C23(H23A,H23B,H23C), C24(H24A,H24B,H24C), C25(H25A,H25B,
 H25C), C47(H47A,H47B,H47C), C48(H48A,H48B,H48C), C49(H49A,H49B,H49C), C50(H50A,
 H50B,H50C)
;
_shelx_res_checksum              99296
_shelx_hkl_checksum              29125
_olex2_submission_special_instructions 'No special instructions were received'