Synthesis of [Ag(NHCMe2)2]ClO4 and Its Use as a Source of Acetimine. 1. Synthesis of the First Acetimine Rhodium Complexes and the First Crystal Structure of a Diacetonamine Complex
José Vicente; María-Teresa Chicote; Rita Guerrero; Inmaculada Vicente-Hernández; Peter G. Jones; Inorganic Chemistry 42 (2003) 7644–7651; doi:10.1021/ic035002+

data_4327493
_publ_section_title
;
 Synthesis of [Ag(NHCMe2)2]ClO4 and Its Use as a Source of Acetimine. 1.
 Synthesis of the First Acetimine Rhodium Complexes and the First Crystal
 Structure of a Diacetonamine Complex
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              7644
_journal_page_last               7651
_journal_paper_doi               10.1021/ic035002+
_journal_volume                  42
_journal_year                    2003
_chemical_formula_sum            'C29 H34 Cl N O4 P Rh'
_chemical_formula_weight         629.90
_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                 93.951(4)
_cell_angle_gamma                90.00
_cell_formula_units_Z            8
_cell_length_a                   9.7384(8)
_cell_length_b                   32.027(3)
_cell_length_c                   17.5949(14)
_cell_measurement_reflns_used    7016
_cell_measurement_temperature    133(2)
_cell_measurement_theta_max      30.5
_cell_measurement_theta_min      2.2
_cell_volume                     5474.7(8)
_computing_cell_refinement       'Bruker SAINT'
_computing_data_collection       'Bruker SMART'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    'Siemens XP'
_computing_publication_material  SHELXL-97
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      133(2)
_diffrn_detector_area_resol_mean 8.192
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 1.000
_diffrn_measurement_device_type  'Bruker SMART 1000 CCD'
_diffrn_measurement_method       '\w- & \f-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  0.0495
_diffrn_reflns_av_sigmaI/netI    0.0409
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       45
_diffrn_reflns_limit_k_min       -44
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_limit_l_min       -24
_diffrn_reflns_number            96871
_diffrn_reflns_theta_full        30.00
_diffrn_reflns_theta_max         30.03
_diffrn_reflns_theta_min         1.27
_exptl_absorpt_coefficient_mu    0.816
_exptl_absorpt_correction_T_max  0.928
_exptl_absorpt_correction_T_min  0.828
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   SADABS
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.528
_exptl_crystal_description       'square prism'
_exptl_crystal_F_000             2592
_exptl_crystal_size_max          0.36
_exptl_crystal_size_mid          0.18
_exptl_crystal_size_min          0.18
_refine_diff_density_max         2.740
_refine_diff_density_min         -0.446
_refine_diff_density_rms         0.096
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.012
_refine_ls_hydrogen_treatment
'NH free with SADI, rigid methyls, others riding'
_refine_ls_matrix_type           full
_refine_ls_number_parameters     711
_refine_ls_number_reflns         16011
_refine_ls_number_restraints     29
_refine_ls_restrained_S_all      1.011
_refine_ls_R_factor_all          0.0557
_refine_ls_R_factor_gt           0.0334
_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^)+(0.0443P)^2^+3.3624P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0815
_refine_ls_wR_factor_ref         0.0902
_reflns_number_gt                11916
_reflns_number_total             16011
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic0350022Bsi20031008_020335.cif
_cod_data_source_block           rodeo
_cod_original_cell_volume        5474.6(8)
_cod_original_sg_symbol_H-M      'P 21/c'
_cod_database_code               4327493