Amine-Assisted C−Cl Bond Activation of Aryl Chlorides by a (Phebox)Rh-Chloro Complex
Ito, Jun-ichi; Miyakawa, Takeshi; Nishiyama, Hisao; Organometallics 27 (2008) 3312–; doi:10.1021/om8002174

data_4071544
_publ_section_title
;
 Amine-Assisted C&#x2212;Cl Bond Activation of Aryl Chlorides by a
 (Phebox)Rh-Chloro Complex
;
_journal_issue                   13
_journal_name_full               Organometallics
_journal_page_first              3312
_journal_paper_doi               10.1021/om8002174
_journal_volume                  27
_journal_year                    2008
_chemical_formula_sum            'C26.5 H33.5 Cl5 N3 O2 Rh'
_chemical_formula_weight         706.22
_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                105.268(7)
_cell_angle_beta                 97.952(6)
_cell_angle_gamma                90.103(7)
_cell_formula_units_Z            4
_cell_length_a                   13.364(4)
_cell_length_b                   15.834(5)
_cell_length_c                   16.154(5)
_cell_measurement_reflns_used    3588
_cell_measurement_temperature    153(2)
_cell_measurement_theta_max      24.45
_cell_measurement_theta_min      2.17
_cell_volume                     3263.3(17)
_computing_cell_refinement       'Bruker SMART'
_computing_data_collection       'Bruker SMART'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      153(2)
_diffrn_detector_area_resol_mean 8.366
_diffrn_measured_fraction_theta_full 0.975
_diffrn_measured_fraction_theta_max 0.975
_diffrn_measurement_device_type  '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  0.0478
_diffrn_reflns_av_sigmaI/netI    0.1083
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -13
_diffrn_reflns_number            22966
_diffrn_reflns_theta_full        27.74
_diffrn_reflns_theta_max         27.74
_diffrn_reflns_theta_min         1.88
_exptl_absorpt_coefficient_mu    0.960
_exptl_absorpt_correction_T_max  1.000000
_exptl_absorpt_correction_T_min  0.734031
_exptl_absorpt_correction_type   empirical
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.438
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             1438
_exptl_crystal_size_max          0.70
_exptl_crystal_size_mid          0.30
_exptl_crystal_size_min          0.10
_refine_diff_density_max         2.471
_refine_diff_density_min         -1.618
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_refine_ls_extinction_method     none
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_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     682
_refine_ls_number_reflns         14967
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.022
_refine_ls_R_factor_all          0.1251
_refine_ls_R_factor_gt           0.0697
_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^)+(0.1109P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1737
_refine_ls_wR_factor_ref         0.2041
_reflns_number_gt                9098
_reflns_number_total             14967
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            om8002174-file002.cif
_cod_data_source_block           Complex_5
_cod_depositor_comments
;
The following automatic conversions were performed:

'_symmetry_cell_setting' value 'Triclinic' changed to 'triclinic'
according to /home/saulius/struct/CIF-dictionaries/cif_core.dic
dictionary named 'cif_core.dic' version 2.4.1 from
2010-06-29.

'_exptl_absorpt_correction_type' value 'Empirical'
changed to 'empirical' 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_cell_volume        3263.2(18)
_cod_original_sg_symbol_H-M      P-1
_cod_original_formula_sum        'C26.50 H33.50 Cl5 N3 O2 Rh'
_cod_database_code               4071544