Activation of an Unstrained C(sp2)‒C(sp2) Single Bond Using Chelate-Bisphosphinite Rhodium(I) Complexes
Obenhuber, Andreas; Ruhland, Klaus; Organometallics 30 (2011) 4039–; doi:10.1021/om200288e

data_4064708
_publ_section_title
;
 Activation of an Unstrained C(sp2)--C(sp2) Single Bond Using
 Chelate-Bisphosphinite Rhodium(I) Complexes
;
_journal_issue                   15
_journal_name_full               Organometallics
_journal_page_first              4039
_journal_paper_doi               10.1021/om200288e
_journal_volume                  30
_journal_year                    2011
_chemical_formula_sum            'C25 H36 Cl O3 P2 Rh'
_chemical_formula_weight         584.84
_chemical_melting_point          ?
_chemical_name_systematic
; 
 Rhodium(I) 
;
_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                 95.424(1)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   15.1685(1)
_cell_length_b                   11.2434(1)
_cell_length_c                   15.2618(2)
_cell_measurement_reflns_used    46347
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      25.2498
_cell_measurement_theta_min      2.6831
_cell_volume                     2591.18(4)
_computing_cell_refinement
;
 CrysAlis RED, Oxford Diffraction Ltd.,
 Version 1.171.32.5 (release 08-05-2007 CrysAlis171 .NET)
 (compiled May  8 2007,13:10:02)
;
_computing_data_collection
;
 CrysAlis CCD, Oxford Diffraction Ltd.,
 Version 1.171.32.5 (release 08-05-2007 CrysAlis171 .NET)
 (compiled May  8 2007,13:10:02)
;
_computing_data_reduction
;
 CrysAlis RED, Oxford Diffraction Ltd.,
 Version 1.171.32.5 (release 08-05-2007 CrysAlis171 .NET)
 (compiled May  8 2007,13:10:02)
;
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1997)'
_diffrn_ambient_temperature      150(2)
_diffrn_detector                 ' CCD plate '
_diffrn_detector_area_resol_mean 16.0238
_diffrn_measured_fraction_theta_full 0.995
_diffrn_measured_fraction_theta_max 0.995
_diffrn_measurement_device       ' \k-geometry diffractometer '
_diffrn_measurement_device_type  ' Oxford-Diffraction Xcalibur3 '
_diffrn_measurement_method       ' phi- and omega-rotation '
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'Enhance (Mo) X-ray Source'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0254
_diffrn_reflns_av_sigmaI/netI    0.0099
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_h_min       -18
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_number            63777
_diffrn_reflns_theta_full        25.36
_diffrn_reflns_theta_max         25.36
_diffrn_reflns_theta_min         2.69
_diffrn_standards_decay_%        0
_exptl_absorpt_coefficient_mu    0.910
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.77886
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;   
 CrysAlis RED, Oxford Diffraction Ltd.,
 Version 1.171.32.5 (release 08-05-2007 CrysAlis171 .NET)
 (compiled May  8 2007,13:10:02)
 Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.499
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       fragment
_exptl_crystal_F_000             1208
_exptl_crystal_size_max          0.20
_exptl_crystal_size_mid          0.15
_exptl_crystal_size_min          0.10
_refine_diff_density_max         0.844
_refine_diff_density_min         -0.515
_refine_diff_density_rms         0.075
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.194
_refine_ls_hydrogen_treatment    refall
_refine_ls_matrix_type           full
_refine_ls_number_parameters     433
_refine_ls_number_reflns         4737
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.194
_refine_ls_R_factor_all          0.0355
_refine_ls_R_factor_gt           0.0302
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0191P)^2^+4.6340P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0621
_refine_ls_wR_factor_ref         0.0661
_reflns_number_gt                4213
_reflns_number_total             4737
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            om200288e_si_001.cif
_cod_data_source_block           ruhl_ac
_cod_depositor_comments
;
The following automatic conversions were performed:

'_chemical_melting_point' value 'not measured' was changed to '?' -
the value is undefined or not given.

'_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 

The following automatic conversions were performed:

'_exptl_crystal_density_meas' value 'not measured' was changed to '?'
- the value is perceived as not measured.

Automatic conversion script
Id: cif_fix_values 3008 2015-01-20 13:52:24Z robertas 
;
_cod_original_sg_symbol_H-M      P2(1)/c
_cod_database_code               4064708