Multinuclear NMR, X-ray, and DFT Studies on RhCl(diene)(phosphoramidite) Complexes
Filipuzzi, Serena; Männel, Elisabeth; Pregosin, Paul S.; Albinati, Alberto; Rizzato, Silvia; Veiros, Luis F.; Organometallics 27 (2008) 4580–; doi:10.1021/om800082c

data_4071286
_publ_section_title
;
 Multinuclear NMR, X-ray, and DFT Studies on RhCl(diene)(phosphoramidite)
 Complexes
;
_journal_issue                   18
_journal_name_full               Organometallics
_journal_page_first              4580
_journal_paper_doi               10.1021/om800082c
_journal_volume                  27
_journal_year                    2008
_chemical_formula_sum            'C45 H44 Cl3 N O2 P Rh'
_chemical_formula_weight         871.04
_chemical_name_common            '[RhCl(1,5-COD)(phosphoramidite)]'
_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                 103.231(4)
_cell_angle_gamma                90.00
_cell_formula_units_Z            2
_cell_length_a                   11.2340(17)
_cell_length_b                   11.493(3)
_cell_length_c                   15.8389(13)
_cell_measurement_reflns_used    954
_cell_measurement_temperature    123(2)
_cell_measurement_theta_max      25.79
_cell_measurement_theta_min      2.52
_cell_volume                     1990.7(6)
_computing_cell_refinement       'SAINTPLUS  (Bruker AXS, 1999)'
_computing_data_collection       'SMART      (Bruker AXS, 2001)'
_computing_data_reduction        'SAINTPLUS  (Bruker AXS, 1999)'
_computing_molecular_graphics
'ORTEP for Windows v1.074 (L.J. Farrugia 1997)'
_computing_publication_material
'WinGX v1.64.05(L.J. Farrugia,J. Appl. Cryst.,1999,32, 837)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      120(2)
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device_type  'Bruker APEX CCD'
_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  0.0317
_diffrn_reflns_av_sigmaI/netI    0.0416
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            18258
_diffrn_reflns_theta_full        26.03
_diffrn_reflns_theta_max         26.03
_diffrn_reflns_theta_min         1.86
_exptl_absorpt_coefficient_mu    0.710
_exptl_absorpt_correction_T_max  1.0000
_exptl_absorpt_correction_T_min  0.8161
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_process_details   'Sadabs 2.01 (Bruker AXS, 1999)'
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.453
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prismatic
_exptl_crystal_F_000             896
_exptl_crystal_size_max          0.4
_exptl_crystal_size_mid          0.4
_exptl_crystal_size_min          0.2
_refine_diff_density_max         1.337
_refine_diff_density_min         -0.880
_refine_diff_density_rms         0.085
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   -0.04(2)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.046
_refine_ls_hydrogen_treatment    riding
_refine_ls_matrix_type           full
_refine_ls_number_parameters     478
_refine_ls_number_reflns         7806
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.046
_refine_ls_R_factor_all          0.0402
_refine_ls_R_factor_gt           0.0355
_refine_ls_shift/su_max          0.010
_refine_ls_shift/su_mean         0.002
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0513P)^2^+1.5345P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0875
_refine_ls_wR_factor_ref         0.0905
_reflns_number_gt                7322
_reflns_number_total             7806
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            om800082c_si_002.cif
_cod_data_source_block           preg102
_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_values 1715 2011-07-08 13:25:40Z adriana 
;
_cod_original_sg_symbol_H-M      P21
_cod_database_code               4071286
_compound_number                 4