Reactivity of Rhodium(I) Complexes Bearing Nitrogen-Containing Ligands toward CH3I: Synthesis and Full Characterization of Neutral cis-[RhX(CO)2(L)] and Acetyl [RhI(μ-I)(COMe)(CO)(L)]2 Complexes
Romain J. Adcock; Duc Hanh Nguyen; Sonia Ladeira; Carole Le Berre; Philippe Serp; Philippe Kalck; Inorganic Chemistry 51 (2012) 8670–8685; doi:10.1021/ic2019988

data_4329981
_publ_section_title
;
 Reactivity of Rhodium(I) Complexes Bearing Nitrogen-Containing Ligands
 toward CH3I: Synthesis and Full Characterization of Neutral
 cis-[RhX(CO)2(L)] and Acetyl [RhI(\m-I)(COMe)(CO)(L)]2 Complexes
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              8670
_journal_page_last               8685
_journal_paper_doi               10.1021/ic2019988
_journal_volume                  51
_journal_year                    2012
_chemical_compound_source        'synthesis as described'
_chemical_formula_moiety         'C5 H4 I N2 O2 Rh'
_chemical_formula_sum            'C5 H4 I N2 O2 Rh'
_chemical_formula_weight         353.91
_chemical_name_systematic
;
 ?
;
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_Int_Tables_number      14
_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
_cell_angle_alpha                90
_cell_angle_beta                 121.741(2)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   10.3601(3)
_cell_length_b                   7.0604(2)
_cell_length_c                   14.5503(4)
_cell_measurement_reflns_used    4633
_cell_measurement_temperature    180(2)
_cell_measurement_theta_max      30.61
_cell_measurement_theta_min      2.86
_cell_measurement_wavelength     0.71073
_cell_volume                     905.12(5)
_computing_cell_refinement       'Bruker SMART'
_computing_data_collection       'Bruker SMART'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    'Ortep-3 for Windows (Farrugia, 1997)'
_computing_publication_material  'WinGX publication routines (Farrugia, 1999)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      180(2)
_diffrn_measured_fraction_theta_full 0.996
_diffrn_measured_fraction_theta_max 0.996
_diffrn_measurement_device_type  'Bruker Kappa APEX II'
_diffrn_measurement_method       \w-\f
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0326
_diffrn_reflns_av_unetI/netI     0.0283
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       9
_diffrn_reflns_limit_k_min       -10
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            12040
_diffrn_reflns_theta_full        30.61
_diffrn_reflns_theta_max         30.61
_diffrn_reflns_theta_min         2.86
_diffrn_standards_decay_%        0
_diffrn_standards_interval_count 0
_diffrn_standards_interval_time  0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    5.252
_exptl_absorpt_correction_T_max  0.900
_exptl_absorpt_correction_T_min  0.778
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
        [c.f. r.h. blessing, acta cryst. (1995), a51, 33-38]
;
_exptl_crystal_colour            orange
_exptl_crystal_density_diffrn    2.597
_exptl_crystal_description       plate
_exptl_crystal_F_000             648
_exptl_crystal_size_max          0.14
_exptl_crystal_size_mid          0.04
_exptl_crystal_size_min          0.02
_refine_diff_density_max         1.103
_refine_diff_density_min         -0.541
_refine_diff_density_rms         0.112
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.008
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     103
_refine_ls_number_reflns         2777
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.008
_refine_ls_R_factor_all          0.0371
_refine_ls_R_factor_gt           0.021
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0178P)^2^+0.5761P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0441
_refine_ls_wR_factor_ref         0.0498
_reflns_number_gt                2096
_reflns_number_total             2777
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic2019988_si_002_07.cif
_cod_data_source_block           4e
_cod_original_sg_symbol_H-M      'P 21/c'
_cod_database_code               4329981