Rhodium and ruthenium complexes of methylene-bridged, <i>P</i>-stereogenic, unsymmetrical diphosphanes.
Eusamio, Javier; Medina, Yaiza M.; Córdoba, Javier C; Vidal-Ferran, Anton; Sainz, Daniel; Gutiérrez, Albert; Font-Bardia, Mercè; Grabulosa, Arnald; Dalton transactions (Cambridge, England : 2003) 52 (2023) 2424–2439; doi:10.1039/d2dt04026c

data_7712235
_publ_section_title
;
 Rhodium and ruthenium complexes of methylene-bridged,
 <i>P</i>-stereogenic, unsymmetrical diphosphanes.
;
_journal_issue                   8
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              2424
_journal_page_last               2439
_journal_paper_doi               10.1039/d2dt04026c
_journal_volume                  52
_journal_year                    2023
_chemical_absolute_configuration rm
_chemical_formula_moiety         'C50 H60 P4 Rh, B F4, C4 H8 O'
_chemical_formula_sum            'C54 H68 B F4 O P4 Rh'
_chemical_formula_weight         1046.68
_space_group_crystal_system      monoclinic
_space_group_IT_number           4
_space_group_name_Hall           'P 2yb'
_space_group_name_H-M_alt        'P 1 21 1'
_atom_sites_solution_hydrogens   geom
_audit_creation_method           SHELXL-2018/3
_audit_update_record
;
2022-11-30 deposited with the CCDC.	2023-01-23 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 96.936(5)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   15.6831(15)
_cell_length_b                   14.2537(13)
_cell_length_c                   22.935(3)
_cell_measurement_reflns_used    9746
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      30.53
_cell_measurement_theta_min      2.53
_cell_volume                     5089.4(9)
_computing_cell_refinement       'Bruker SAINT'
_computing_data_collection       'Bruker APEX3'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-2018/3 (Sheldrick, 2018)'
_computing_structure_solution    'SHELXT 2014/5 (Sheldrick, 2014)'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 0.993
_diffrn_measured_fraction_theta_max 0.980
_diffrn_measurement_device_type  'D8 Venture'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0433
_diffrn_reflns_av_unetI/netI     0.0517
_diffrn_reflns_Laue_measured_fraction_full 0.993
_diffrn_reflns_Laue_measured_fraction_max 0.980
_diffrn_reflns_limit_h_max       22
_diffrn_reflns_limit_h_min       -22
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_l_max       32
_diffrn_reflns_limit_l_min       -32
_diffrn_reflns_number            101745
_diffrn_reflns_point_group_measured_fraction_full 0.992
_diffrn_reflns_point_group_measured_fraction_max 0.969
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         30.605
_diffrn_reflns_theta_min         1.937
_diffrn_source                   microfocus
_exptl_absorpt_coefficient_mu    0.514
_exptl_absorpt_correction_T_max  0.7461
_exptl_absorpt_correction_T_min  0.6926
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   sadabs
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    1.366
_exptl_crystal_description       prism
_exptl_crystal_F_000             2184
_exptl_crystal_size_max          0.200
_exptl_crystal_size_mid          0.140
_exptl_crystal_size_min          0.120
_refine_diff_density_max         0.946
_refine_diff_density_min         -0.756
_refine_diff_density_rms         0.078
_refine_ls_abs_structure_details
;
 Flack x determined using 10315 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   -0.023(8)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.042
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1163
_refine_ls_number_reflns         30408
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.042
_refine_ls_R_factor_all          0.0517
_refine_ls_R_factor_gt           0.0365
_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^)+(0.0229P)^2^+3.3653P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0693
_refine_ls_wR_factor_ref         0.0785
_reflns_Friedel_coverage         0.906
_reflns_Friedel_fraction_full    0.992
_reflns_Friedel_fraction_max     0.956
_reflns_number_gt                25769
_reflns_number_total             30408
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d2dt04026c2.cif
_cod_data_source_block           Rh(BiphiPr)2
_cod_depositor_comments
'Adding full bibliography for 7712233--7712235.cif.'
_cod_original_cell_volume        5089.5(9)
_cod_original_sg_symbol_H-M      'P 21'
_cod_database_code               7712235
_shelx_shelxl_version_number     2018/3
_shelx_res_checksum              49788