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_4516953
_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         'C47 H45 N O P Ru, F6 P, (C H2 Cl2)2'
_chemical_formula_sum            'C49 H49 Cl4 F6 N O P2 Ru'
_chemical_formula_weight         1086.7
_space_group_IT_number           4
_space_group_name_Hall           'P 2yb'
_space_group_name_H-M_alt        'P 1 21 1'
_symmetry_cell_setting           monoclinic
_symmetry_Int_Tables_number      4
_symmetry_space_group_name_Hall  'P 2yb'
_symmetry_space_group_name_H-M   'P 1 21 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_cell_angle_alpha                90
_cell_angle_beta                 98.590(14)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   10.429(3)
_cell_length_b                   16.431(5)
_cell_length_c                   14.060(5)
_cell_measurement_reflns_used    20559
_cell_measurement_temperature    173(2)
_cell_measurement_theta_max      27.48
_cell_measurement_theta_min      3.17
_cell_measurement_wavelength     0.71073
_cell_volume                     2382.3(13)
_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 0.997
_diffrn_measured_fraction_theta_max 0.997
_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  0.0334
_diffrn_reflns_av_unetI/netI     0.0445
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.997
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_number            18634
_diffrn_reflns_point_group_measured_fraction_full 0.988
_diffrn_reflns_point_group_measured_fraction_max 0.988
_diffrn_reflns_theta_full        24.999
_diffrn_reflns_theta_max         24.999
_diffrn_reflns_theta_min         3.17
_diffrn_source                   'sealed x-ray tube'
_exptl_absorpt_coefficient_mu    0.682
_exptl_absorpt_correction_T_max  1.0000
_exptl_absorpt_correction_T_min  0.7749
_exptl_absorpt_correction_type   multi-scan
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    1.515
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             1108
_exptl_crystal_size_max          0.51
_exptl_crystal_size_mid          0.38
_exptl_crystal_size_min          0.20
_refine_diff_density_max         2.326
_refine_diff_density_min         -0.852
_refine_diff_density_rms         0.11
_refine_ls_abs_structure_details
;
 Flack x determined using 3305 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   -0.029(14)
_refine_ls_extinction_coef       0.0062(16)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     'SHELXL-2016/6 (Sheldrick 2016)'
_refine_ls_goodness_of_fit_ref   1.057
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     578
_refine_ls_number_reflns         8291
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.057
_refine_ls_R_factor_all          0.06
_refine_ls_R_factor_gt           0.0561
_refine_ls_shift/su_max          0
_refine_ls_shift/su_mean         0
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0952P)^2^+3.6529P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1479
_refine_ls_wR_factor_ref         0.1519
_reflns_Friedel_coverage         0.907
_reflns_Friedel_fraction_full    0.977
_reflns_Friedel_fraction_max     0.977
_reflns_number_gt                7733
_reflns_number_total             8291
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ao7b01460_si_002.cif
_cod_data_source_block           1519532
_cod_original_sg_symbol_H-M      'P 21'
_cod_database_code               4516953
_shelx_estimated_absorpt_t_min   0.722
_shelx_estimated_absorpt_t_max   0.876