Highly efficient Rh(I) and Ir(I) single and dual metal catalysed dihydroalkoxylation reactions of alkyne diols.
Ho, Joanne Hui Hui; Hodgson, Richard; Wagler, Jörg; Messerle, Barbara Ann; Dalton transactions (Cambridge, England : 2003) 39 (2010) 4062–4069; doi:10.1039/b926773e

data_7025300
_publ_section_title
;
 Highly efficient Rh(I) and Ir(I) single and dual metal catalysed
 dihydroalkoxylation reactions of alkyne diols.
;
_journal_issue                   17
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              4062
_journal_page_last               4069
_journal_paper_doi               10.1039/b926773e
_journal_volume                  39
_journal_year                    2010
_chemical_formula_moiety         'C32 H12 B F24, C9 H8 N4 O2 Rh '
_chemical_formula_sum            'C41 H20 B F24 N4 O2 Rh'
_chemical_formula_weight         1170.33
_chemical_name_systematic
;
?
;
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                92.0450(10)
_cell_angle_beta                 105.2590(10)
_cell_angle_gamma                98.5870(10)
_cell_formula_units_Z            2
_cell_length_a                   10.39710(10)
_cell_length_b                   14.9619(2)
_cell_length_c                   15.1133(2)
_cell_measurement_reflns_used    57628
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      30.034
_cell_measurement_theta_min      2.546
_cell_volume                     2235.78(5)
_computing_cell_refinement       'HKL Scalepack (Otwinowski & Minor 1997)'
_computing_data_collection       'Nonius Collect, KappaCCD'
_computing_data_reduction
'Denzo and Scalepak (Otwinowski & Minor, 1997)'
_computing_molecular_graphics    'ORTEP32 for windows (Farugia)'
_computing_publication_material  'Ciftab (Sheldrick, 1997)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device_type  'Nonius Kappa CCD area detector'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0405
_diffrn_reflns_av_sigmaI/netI    0.0317
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       21
_diffrn_reflns_limit_k_min       -21
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            62552
_diffrn_reflns_theta_full        30.00
_diffrn_reflns_theta_max         30.00
_diffrn_reflns_theta_min         2.66
_exptl_absorpt_coefficient_mu    0.524
_exptl_absorpt_correction_T_max  0.933
_exptl_absorpt_correction_T_min  0.815
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
multi-scan from symmetry-related measurements
Sortav (Blessing 1995)
;
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.738
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       piece
_exptl_crystal_F_000             1152
_exptl_crystal_size_max          0.31
_exptl_crystal_size_mid          0.28
_exptl_crystal_size_min          0.14
_refine_diff_density_max         1.267
_refine_diff_density_min         -0.878
_refine_diff_density_rms         0.087
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.019
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     668
_refine_ls_number_reflns         13056
_refine_ls_number_restraints     58
_refine_ls_restrained_S_all      1.126
_refine_ls_R_factor_all          0.0549
_refine_ls_R_factor_gt           0.0447
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0502P)^2^+3.5020P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1086
_refine_ls_wR_factor_ref         0.1132
_reflns_number_gt                11222
_reflns_number_total             13056
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            b926773e.txt
_cod_data_source_block           rh00601
_cod_original_sg_symbol_Hall     -P1
_cod_original_sg_symbol_H-M      P-1
_cod_database_code               7025300