Synthesis, Structural Analysis, and Catalytic Properties of Tetrakis(binaphthyl or octahydrobinaphthyl phosphate) Dirhodium(II,II) Complexes
Hrdina, Radim; Guénée, Laure; Moraleda, Delphine; Lacour, Jérôme; Organometallics 32 (2013) 473–; doi:10.1021/om300935u

data_4079827
_publ_section_title
;
 Synthesis, Structural Analysis, and Catalytic Properties of
 Tetrakis(binaphthyl or octahydrobinaphthyl phosphate) Dirhodium(II,II)
 Complexes
;
_journal_issue                   2
_journal_name_full               Organometallics
_journal_page_first              473
_journal_paper_doi               10.1021/om300935u
_journal_volume                  32
_journal_year                    2013
_chemical_absolute_configuration ad
_chemical_formula_moiety         'C84 H58 O19 P4 Rh2, 8(C4 H8 O2), 0.5O'
_chemical_formula_sum            'C116 H122 O35.5 P4 Rh2'
_chemical_formula_weight         2413.84
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           4
_symmetry_cell_setting           monoclinic
_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
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 101.1014(12)
_cell_angle_gamma                90.00
_cell_formula_units_Z            2
_cell_length_a                   14.72965(19)
_cell_length_b                   20.6819(2)
_cell_length_c                   18.2822(2)
_cell_measurement_reflns_used    31111
_cell_measurement_temperature    180(2)
_cell_measurement_theta_max      73.2899
_cell_measurement_theta_min      2.4608
_cell_volume                     5465.22(11)
_computing_cell_refinement
;
CrysAlisPro, Agilent Technologies,
Version 1.171.35.11 (release 16-05-2011 CrysAlis171 .NET)
(compiled May 16 2011,17:55:39)
;
_computing_data_collection
;
CrysAlisPro, Agilent Technologies,
Version 1.171.35.11 (release 16-05-2011 CrysAlis171 .NET)
(compiled May 16 2011,17:55:39)
;
_computing_data_reduction
;
CrysAlisPro, Agilent Technologies,
Version 1.171.35.11 (release 16-05-2011 CrysAlis171 .NET)
(compiled May 16 2011,17:55:39)
;
_computing_molecular_graphics    'Ortep 3 (Farrugia, 1997)'
_computing_publication_material  'ShelX_Acta (Sheldrick, 2008)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      180(2)
_diffrn_detector_area_resol_mean 10.4679
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.989
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at zero, Atlas'
_diffrn_measurement_method       '\w scans'
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_source         'SuperNova (Cu) X-ray Source'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0383
_diffrn_reflns_av_sigmaI/netI    0.0441
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       25
_diffrn_reflns_limit_k_min       -25
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_number            45660
_diffrn_reflns_theta_full        66.97
_diffrn_reflns_theta_max         73.45
_diffrn_reflns_theta_min         2.46
_exptl_absorpt_coefficient_mu    3.711
_exptl_absorpt_correction_T_max  0.738
_exptl_absorpt_correction_T_min  0.387
_exptl_absorpt_correction_type   analytical
_exptl_absorpt_process_details
;
CrysAlisPro, Agilent Technologies,
Version 1.171.35.11 (release 16-05-2011 CrysAlis171 .NET)
(compiled May 16 2011,17:55:39)
Analytical numeric absorption correction using a multifaceted crystal
            model based on expressions derived by R.C. Clark & J.S. Reid.
(Clark, R. C. & Reid, J. S. (1995). Acta Cryst. A51, 887-897)
;
_exptl_crystal_colour            green
_exptl_crystal_density_diffrn    1.467
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             2504
_exptl_crystal_size_max          0.3775
_exptl_crystal_size_mid          0.2685
_exptl_crystal_size_min          0.0875
_refine_diff_density_max         0.885
_refine_diff_density_min         -1.328
_refine_diff_density_rms         0.073
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   -0.027(4)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.028
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1425
_refine_ls_number_reflns         21332
_refine_ls_number_restraints     5
_refine_ls_restrained_S_all      1.028
_refine_ls_R_factor_all          0.0441
_refine_ls_R_factor_gt           0.0430
_refine_ls_shift/su_max          0.003
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0940P)^2^+0.0973P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1157
_refine_ls_wR_factor_ref         0.1182
_reflns_number_gt                20729
_reflns_number_total             21332
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            om300935u_si_002.cif
_cod_data_source_block           1a
_cod_original_cell_volume        5465.21(11)
_cod_original_sg_symbol_Hall     'P 2Yb'
_cod_original_sg_symbol_H-M      'P 21'
_cod_original_formula_sum        'C116 H122 O35.50 P4 Rh2'
_cod_database_code               4079827