On the reactivity toward ketones of new methyl amino complexes of Rh(III) and Ag(I). Synthesis of ortho-rhodiated acetophenone methyl imine complexes.
Vicente, José; Chicote, María Teresa; Vicente-Hernandez, Inmaculada; Bautista, Delia; Inorganic chemistry 46 (2007) 8939–8949; doi:10.1021/ic700963h

data_4339583
_publ_section_title
;
 On the reactivity toward ketones of new methyl amino complexes of Rh(III)
 and Ag(I). Synthesis of ortho-rhodiated acetophenone methyl imine
 complexes.
;
_journal_issue                   21
_journal_name_full               'Inorganic chemistry'
_journal_page_first              8939
_journal_page_last               8949
_journal_paper_doi               10.1021/ic700963h
_journal_volume                  46
_journal_year                    2007
_chemical_formula_sum            'C22 H36 Cl2 D6 N3 O9 Rh'
_chemical_formula_weight         678.40
_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                68.798(2)
_cell_angle_beta                 86.115(2)
_cell_angle_gamma                82.602(2)
_cell_formula_units_Z            2
_cell_length_a                   10.3800(5)
_cell_length_b                   11.1724(5)
_cell_length_c                   13.4906(6)
_cell_measurement_reflns_used    6858
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      28.09
_cell_measurement_theta_min      2.53
_cell_volume                     1446.08(12)
_computing_cell_refinement       'Bruker SAINT'
_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      293(2)
_diffrn_detector_area_resol_mean 8.26
_diffrn_measured_fraction_theta_full 0.994
_diffrn_measured_fraction_theta_max 0.990
_diffrn_measurement_device_type  'Bruker SMART APEX CCD'
_diffrn_measurement_method       \w-scan
_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  0.0167
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_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       17
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            16361
_diffrn_reflns_theta_full        26.00
_diffrn_reflns_theta_max         26.73
_diffrn_reflns_theta_min         1.97
_exptl_absorpt_coefficient_mu    0.827
_exptl_absorpt_correction_T_max  0.9073
_exptl_absorpt_correction_T_min  0.7779
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   SADABS
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.558
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             692
_exptl_crystal_size_max          0.32
_exptl_crystal_size_mid          0.22
_exptl_crystal_size_min          0.12
_refine_diff_density_max         0.943
_refine_diff_density_min         -0.811
_refine_diff_density_rms         0.072
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.080
_refine_ls_hydrogen_treatment    'NH free, methyls rigid, others riding'
_refine_ls_matrix_type           full
_refine_ls_number_parameters     359
_refine_ls_number_reflns         6080
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.080
_refine_ls_R_factor_all          0.0295
_refine_ls_R_factor_gt           0.0291
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0319P)^2^+1.8417P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0716
_refine_ls_wR_factor_ref         0.0719
_reflns_number_gt                6007
_reflns_number_total             6080
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic700963h-file001.cif
_cod_data_source_block           17ivas
_cod_depositor_comments
;
The following automatic conversions were performed:

'_symmetry_cell_setting' value 'Triclinic' changed to 'triclinic'
according to
/usr/data/users/saulius/automatic-downloads/retrospective/ACS/lib/dictionaries/cif_core.dic
dictionary named 'cif_core.dic' version 2.4.2 from 2011-04-26.

Automatic conversion script
Id: cif_fix_values 2281 2013-09-26 08:29:07Z andrius 
;
_cod_original_cell_volume        1446.08(11)
_cod_original_formula_sum        'C22 H36 D6 Cl2 N3 O9 Rh'
_cod_database_code               4339583