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_4087144
_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         'C35 H40 Cl4 N P Ru2, C1 H1 Cl3'
_chemical_formula_sum            'C36 H41 Cl7 N P Ru2'
_chemical_formula_weight         968.96
_chemical_name_systematic
;
 ? 
;
_space_group_crystal_system      monoclinic
_space_group_IT_number           15
_space_group_name_Hall           '-C 2yc'
_space_group_name_H-M_alt        'C 1 2/c 1'
_symmetry_space_group_name_Hall  '-C 2yc'
_symmetry_space_group_name_H-M   'C 1 2/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                 131.4450(10)
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   29.282(4)
_cell_length_b                   17.432(3)
_cell_length_c                   20.054(5)
_cell_measurement_reflns_used    9927
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      27.74
_cell_measurement_theta_min      2.34
_cell_volume                     7673(3)
_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 0.999
_diffrn_measured_fraction_theta_max 0.999
_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  0.0526
_diffrn_reflns_av_unetI/netI     0.0302
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_limit_h_max       38
_diffrn_reflns_limit_h_min       -38
_diffrn_reflns_limit_k_max       22
_diffrn_reflns_limit_k_min       -22
_diffrn_reflns_limit_l_max       26
_diffrn_reflns_limit_l_min       -26
_diffrn_reflns_number            72755
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.860
_diffrn_reflns_theta_min         1.492
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    1.344
_exptl_absorpt_correction_T_max  0.7456
_exptl_absorpt_correction_T_min  0.6828
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2014/4 (Bruker,2014/4) was used for absorption correction.
wR2(int) was 0.1006 before and 0.0538 after correction.
The Ratio of minimum to maximum transmission is 0.9158.
The \l/2 correction factor is 0.00150.
;
_exptl_crystal_colour            orange
_exptl_crystal_density_diffrn    1.678
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       needle
_exptl_crystal_F_000             3888
_exptl_crystal_size_max          0.26
_exptl_crystal_size_mid          0.12
_exptl_crystal_size_min          0.08
_refine_diff_density_max         1.424
_refine_diff_density_min         -2.019
_refine_diff_density_rms         0.151
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.081
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     468
_refine_ls_number_reflns         9119
_refine_ls_number_restraints     150
_refine_ls_restrained_S_all      1.101
_refine_ls_R_factor_all          0.0634
_refine_ls_R_factor_gt           0.0443
_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^)+(0.0577P)^2^+70.0388P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1143
_refine_ls_wR_factor_ref         0.1313
_reflns_Friedel_coverage         0.000
_reflns_number_gt                7149
_reflns_number_total             9119
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            om6b00879_si_001.cif
_cod_data_source_block           rd1510
_cod_database_code               4087144
_shelxl_version_number           2014/6
_shelx_estimated_absorpt_t_max   0.900
_shelx_estimated_absorpt_t_min   0.721
_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. Uiso/Uaniso restraints and constraints
C36 \\sim Cl5 \\sim Cl6 \\sim Cl7 \\sim C36A \\sim Cl5A \\sim Cl6A \\sim Cl7A:
within 2A with sigma of 0.003 and sigma for terminal atoms of 0.006
Uanis(C36) \\sim Ueq, Uanis(Cl5) \\sim Ueq, Uanis(Cl6) \\sim Ueq, Uanis(Cl7)
\\sim Ueq, Uanis(C36A) \\sim Ueq, Uanis(Cl5A) \\sim Ueq, Uanis(Cl6A) \\sim Ueq,
Uanis(Cl7A) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
3. Same fragment restrains
{C36, Cl5, Cl6, Cl7} sigma for 1-2: 0.02, 1-3: 0.04
as
{C36A, Cl5A, Cl6A, Cl7A}
4. Others
 Sof(C36A)=Sof(H36A)=Sof(Cl5A)=Sof(Cl6A)=Sof(Cl7A)=1-FVAR(1)
 Sof(C36)=Sof(H36)=Sof(Cl5)=Sof(Cl6)=Sof(Cl7)=FVAR(1)
5.a Ternary CH refined with riding coordinates:
 C7(H7), C27(H27), C28(H28), C30(H30), C31(H31), C32(H32), C36(H36), C36A(H36A)
5.b Aromatic/amide H refined with riding coordinates:
 C2(H2), C3(H3), C4(H4), C5(H5), C10(H10), C11(H11), C12(H12), C13(H13),
 C16(H16), C17(H17), C18(H18), C19(H19), C20(H20)
5.c Idealised Me refined as rotating group:
 C22(H22A,H22B,H22C), C23(H23A,H23B,H23C), C24(H24A,H24B,H24C), C25(H25A,H25B,
 H25C), C33(H33A,H33B,H33C), C34(H34A,H34B,H34C), C35(H35A,H35B,H35C)
;
_shelx_res_checksum              1667
_shelx_hkl_checksum              75980
_olex2_submission_special_instructions 'No special instructions were received'