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_4516952
_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 P1'
_chemical_formula_sum            'C47 H45 F6 N O P2 Ru'
_chemical_formula_weight         916.85
_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                 98.100(1)
_cell_angle_gamma                90
_cell_formula_units_Z            6
_cell_length_a                   10.50060(10)
_cell_length_b                   17.86340(10)
_cell_length_c                   34.44680(10)
_cell_measurement_reflns_used    31726
_cell_measurement_temperature    110.00(2)
_cell_measurement_theta_max      66.5840
_cell_measurement_theta_min      3.5650
_cell_measurement_wavelength     1.54184
_cell_volume                     6396.95(7)
_computing_publication_material  'WinGX publication routines (Farrugia, 2012)'
_computing_structure_refinement  'SHELXL-2016/6 (Sheldrick, 2016)'
_computing_structure_solution    'SIR2004 (Burla et al., 2005)'
_diffrn_ambient_temperature      110.00(10)
_diffrn_measured_fraction_theta_full 0.99
_diffrn_measured_fraction_theta_max 0.99
_diffrn_measurement_device_type  'SuperNova, Single source at offset), Atlas'
_diffrn_measurement_method       '\w scans'
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_source         'SuperNova (Cu) X-ray Source'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54178
_diffrn_reflns_av_R_equivalents  0.0318
_diffrn_reflns_av_unetI/netI     0.0373
_diffrn_reflns_Laue_measured_fraction_full 0.99
_diffrn_reflns_Laue_measured_fraction_max 0.99
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       21
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_l_max       40
_diffrn_reflns_limit_l_min       -40
_diffrn_reflns_number            48030
_diffrn_reflns_point_group_measured_fraction_full 0.97
_diffrn_reflns_point_group_measured_fraction_max 0.97
_diffrn_reflns_theta_full        66.601
_diffrn_reflns_theta_max         66.601
_diffrn_reflns_theta_min         3.583
_exptl_absorpt_coefficient_mu    4.219
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.46716
_exptl_absorpt_correction_type   multi-scan
_exptl_crystal_colour            orange
_exptl_crystal_density_diffrn    1.428
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       rod
_exptl_crystal_F_000             2850
_exptl_crystal_size_max          0.1924
_exptl_crystal_size_mid          0.0584
_exptl_crystal_size_min          0.0197
_platon_squeeze_details
;
;
_refine_diff_density_max         1.259
_refine_diff_density_min         -0.798
_refine_diff_density_rms         0.078
_refine_ls_abs_structure_details
;
 Flack x determined using 9590 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   -0.014(3)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.012
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1557
_refine_ls_number_reflns         21912
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.012
_refine_ls_R_factor_all          0.0427
_refine_ls_R_factor_gt           0.0414
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0687P)^2^+7.6114P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1086
_refine_ls_wR_factor_ref         0.11
_reflns_Friedel_coverage         0.893
_reflns_Friedel_fraction_full    0.949
_reflns_Friedel_fraction_max     0.949
_reflns_number_gt                21255
_reflns_number_total             21912
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ao7b01460_si_002.cif
_cod_data_source_block           1519531
_cod_depositor_comments
;

2020-05-14
Z value and formula fixed to values more according to usual
chemical conventions.                 miguel
;
_cod_original_cell_volume        6396.99(7)
_cod_original_sg_symbol_H-M      'P 21'
_cod_original_formula_moiety     '(C47 H45 N O P Ru)3, (F6 P1)3'
_cod_original_formula_sum        'C141 H135 F18 N3 O3 P6 Ru3'
_cod_original_formula_units_Z    2
_cod_original_formula_weight     2750.54
_cod_database_code               4516952
_shelx_estimated_absorpt_t_min   0.501
_shelx_estimated_absorpt_t_max   0.92