PPh<sub>3</sub> Propeller Diastereomers: Bonding Motif Ph<sub>PPh<sub>3</sub></sub> Face-On π-Ar in Half-Sandwich Compounds [(π-Ar)LL'MPPh<sub>3</sub>].
Brunner, Henri; Balázs, Gábor; Tsuno, Takashi; Iwabe, Haruka; ACS omega 3 (2018) 982–990; doi:10.1021/acsomega.7b01460

data_4516951
_publ_section_title
;
 PPh<sub>3</sub> Propeller Diastereomers: Bonding Motif
 Ph<sub>PPh<sub>3</sub></sub> Face-On \p-Ar in Half-Sandwich Compounds
 [(\p-Ar)LL'MPPh<sub>3</sub>].
;
_journal_issue                   1
_journal_name_full               'ACS omega'
_journal_page_first              982
_journal_page_last               990
_journal_paper_doi               10.1021/acsomega.7b01460
_journal_volume                  3
_journal_year                    2018
_chemical_absolute_configuration rm
_chemical_compound_source        'synthesis as described'
_chemical_formula_moiety         'C29 H30 Cl N O Ru'
_chemical_formula_sum            'C29 H30 Cl N O Ru'
_chemical_formula_weight         545.06
_space_group_IT_number           19
_space_group_name_Hall           'P 2ac 2ab'
_space_group_name_H-M_alt        'P 21 21 21'
_symmetry_cell_setting           orthorhombic
_symmetry_Int_Tables_number      19
_symmetry_space_group_name_Hall  'P 2ac 2ab'
_symmetry_space_group_name_H-M   'P 21 21 21'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   9.044(3)
_cell_length_b                   13.524(3)
_cell_length_c                   20.436(5)
_cell_measurement_reflns_used    22815
_cell_measurement_temperature    173(2)
_cell_measurement_theta_max      27.48
_cell_measurement_theta_min      3.01
_cell_measurement_wavelength     0.71073
_cell_volume                     2499.5(12)
_computing_publication_material  'WinGX publication routines (Farrugia, 2012)'
_computing_structure_refinement  'SHELXL-2016/6 (Sheldrick, 2016)'
_computing_structure_solution    'SIR97 (Altomare et al, 1999)'
_diffrn_ambient_temperature      173(2)
_diffrn_detector                 'curved image-plate'
_diffrn_detector_area_resol_mean 10
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device       'quarter \C-circle diffractometer'
_diffrn_measurement_device_type  'Rigaku R-Axis Rapid'
_diffrn_measurement_method       'phi or omega oscillation scans'
_diffrn_orient_matrix_type       fs_process
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.037
_diffrn_reflns_av_unetI/netI     0.029
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_limit_l_min       -24
_diffrn_reflns_number            19688
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_theta_full        24.997
_diffrn_reflns_theta_max         24.996
_diffrn_reflns_theta_min         3.008
_diffrn_source                   'sealed x-ray tube'
_exptl_absorpt_coefficient_mu    0.756
_exptl_absorpt_correction_T_max  1.0000
_exptl_absorpt_correction_T_min  0.7317
_exptl_absorpt_correction_type   multi-scan
_exptl_crystal_colour            red-orange
_exptl_crystal_density_diffrn    1.448
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             1120
_exptl_crystal_size_max          0.36
_exptl_crystal_size_mid          0.32
_exptl_crystal_size_min          0.27
_refine_diff_density_max         2.3
_refine_diff_density_min         -0.519
_refine_diff_density_rms         0.088
_refine_ls_abs_structure_details
;
 Flack x determined using 1814 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   -0.004(14)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.065
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     298
_refine_ls_number_reflns         4388
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.065
_refine_ls_R_factor_all          0.0335
_refine_ls_R_factor_gt           0.0325
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0548P)^2^+2.8687P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0875
_refine_ls_wR_factor_ref         0.0885
_reflns_Friedel_coverage         0.753
_reflns_Friedel_fraction_full    0.999
_reflns_Friedel_fraction_max     0.999
_reflns_number_gt                4289
_reflns_number_total             4388
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ao7b01460_si_002.cif
_cod_data_source_block           1519530
_cod_original_cell_volume        2499.6(12)
_cod_database_code               4516951
_shelx_estimated_absorpt_t_min   0.773
_shelx_estimated_absorpt_t_max   0.822