Phosphine-Olefin Ligands: A Facile Dehydrogenative Route to Catalytically Active Rhodium Complexes
Andrew Weller; Simon Brayshaw; Thomas M. Douglas; Christopher Frost; J.Le Notre; Chemical Communications  (2006) –; doi:10.1039/b608129k

data_7101353
_publ_section_title
;
Phosphine-Olefin Ligands: A Facile Dehydrogenative Route
to Catalytically Active Rhodium Complexes
;
_journal_issue                   32
_journal_name_full               'Chemical Communications'
_journal_paper_doi               10.1039/b608129k
_journal_year                    2006
_chemical_formula_moiety         'C41 H49 P3 Rh, C32 H12 B F24, C6 H5 F'
_chemical_formula_sum            'C79 H66 B F25 P3 Rh'
_chemical_formula_weight         1696.95
_chemical_name_common            'Compound 1'
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/c 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                 113.0628(3)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   23.8394(2)
_cell_length_b                   13.1178(1)
_cell_length_c                   26.0538(2)
_cell_measurement_reflns_used    148480
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      30.034
_cell_measurement_theta_min      2.910
_cell_volume                     7496.37(10)
_computing_cell_refinement       'HKL Scalepack (Otwinowski & Minor 1997)'
_computing_data_collection
'Collect, Nonius program suite version 1.9 (1997)'
_computing_data_reduction
'Denzo and Scalepack (Otwinowski & Minor, 1997)'
_computing_molecular_graphics
'ORTEP3 for Windows - L. J. Farrugia, J. Appl. Crystallogr. 1997, 30, 565'
_computing_publication_material  'SHELX97-2, G. M. Sheldrick'
_computing_structure_refinement
;
SHELX97-2 Program for Crystal Structure Analysis. G. M. Sheldrick,
Institut f. Anorg. Chemie der Universit\"at, Tammanstrasse 4,
D-3400 G\"ottingen, Germany, 1998.
;
_computing_structure_solution
;
SIR97- Altomare A., Burla M.C., Camalli M., Cascarano G.L., Giacovazzo C. ,
Guagliardi A., Moliterni A.G.G., Polidori G.,Spagna R.
(1999) J. Appl. Cryst. 32, 115-119.
;
_diffrn_ambient_temperature      150(2)
_diffrn_measured_fraction_theta_full 0.996
_diffrn_measured_fraction_theta_max 0.996
_diffrn_measurement_device_type  'Nonius Kappa CCD'
_diffrn_measurement_method       '786 1.0 degree images with \f and \w 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  0.0666
_diffrn_reflns_av_sigmaI/netI    0.0443
_diffrn_reflns_limit_h_max       33
_diffrn_reflns_limit_h_min       -33
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       36
_diffrn_reflns_limit_l_min       -36
_diffrn_reflns_number            127183
_diffrn_reflns_theta_full        30.01
_diffrn_reflns_theta_max         30.01
_diffrn_reflns_theta_min         3.76
_exptl_absorpt_coefficient_mu    0.398
_exptl_absorpt_correction_T_max  0.8634
_exptl_absorpt_correction_T_min  0.8569
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.504
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       cube
_exptl_crystal_F_000             3440
_exptl_crystal_size_max          0.40
_exptl_crystal_size_mid          0.40
_exptl_crystal_size_min          0.38
_refine_diff_density_max         1.703
_refine_diff_density_min         -0.820
_refine_diff_density_rms         0.070
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.023
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1154
_refine_ls_number_reflns         21803
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.023
_refine_ls_R_factor_all          0.0683
_refine_ls_R_factor_gt           0.0416
_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^)+(0.0554P)^2^+4.1740P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1024
_refine_ls_wR_factor_ref         0.1152
_reflns_number_gt                15934
_reflns_number_total             21803
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            b608129k.txt
_cod_depositor_comments
;
The following automatic conversions were performed:
'_symmetry_cell_setting' value 'Monoclinic' changed to 'monoclinic'
according to '/home/saulius/struct/CIF-dictionaries/cif_core.dic'
dictionary named 'cif_core.dic' version 2.4.1 from 2010-06-29.

Automatic conversion script
Id: cif_fix_enum 1527 2010-12-29 10:47:43Z saulius 
;
_cod_original_sg_symbol_H-M      'P 21/c'
_cod_database_code               7101353