Synthesis, Spectroscopy, Structure, and Reactivity of Azapentadienyl-Rhodium-Phosphine and Azapentadienyl-Iridium-Phosphine Complexes1
Bleeke, John R.; Anutrasakda, Wipark; Rath, Nigam P.; Organometallics 32 (2013) 6410–; doi:10.1021/om400765h

data_4089602
_publ_section_title
;
 Synthesis, Spectroscopy, Structure, and Reactivity of
 Azapentadienyl-Rhodium-Phosphine and Azapentadienyl-Iridium-Phosphine
 Complexes1
;
_journal_issue                   21
_journal_name_full               Organometallics
_journal_page_first              6410
_journal_paper_doi               10.1021/om400765h
_journal_volume                  32
_journal_year                    2013
_chemical_formula_moiety         'C17 H42 N P3 Rh, C F3 O3 S'
_chemical_formula_sum            'C18 H42 F3 N O3 P3 Rh S'
_chemical_formula_weight         605.40
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2ybc'
_space_group_name_H-M_alt        'P 1 21/c 1'
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-2012
_cell_angle_alpha                90
_cell_angle_beta                 96.442(3)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   15.7407(9)
_cell_length_b                   8.2928(4)
_cell_length_c                   20.6824(12)
_cell_measurement_reflns_used    9901
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      31.78
_cell_measurement_theta_min      2.49
_cell_volume                     2682.7(3)
_computing_cell_refinement       'Bruker SAINT'
_computing_data_collection       'Bruker APEX2'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-2012 (Sheldrick, 2012)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.995
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0645
_diffrn_reflns_av_unetI/netI     0.0467
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.995
_diffrn_reflns_limit_h_max       23
_diffrn_reflns_limit_h_min       -23
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_l_max       30
_diffrn_reflns_limit_l_min       -31
_diffrn_reflns_number            62523
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.995
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         32.360
_diffrn_reflns_theta_min         2.246
_exptl_absorpt_coefficient_mu    0.933
_exptl_absorpt_correction_T_max  0.8789
_exptl_absorpt_correction_T_min  0.6993
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'sadabs v2008/1'
_exptl_crystal_colour            orange
_exptl_crystal_density_diffrn    1.499
_exptl_crystal_description       plate
_exptl_crystal_F_000             1256
_exptl_crystal_size_max          0.413
_exptl_crystal_size_mid          0.299
_exptl_crystal_size_min          0.142
_refine_diff_density_max         0.818
_refine_diff_density_min         -0.660
_refine_diff_density_rms         0.103
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.025
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     291
_refine_ls_number_reflns         9564
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.025
_refine_ls_R_factor_all          0.0491
_refine_ls_R_factor_gt           0.0315
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
; 
 w=1/[\s^2^(Fo^2^)+(0.0222P)^2^+1.2044P] 
 where P=(Fo^2^+2Fc^2^)/3 
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0602
_refine_ls_wR_factor_ref         0.0665
_reflns_Friedel_coverage         0.000
_reflns_number_gt                7540
_reflns_number_total             9564
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            om400765h_si_002.cif
_cod_data_source_block           b22912
_cod_original_sg_symbol_H-M      'P 21/c'
_cod_database_code               4089602
_shelx_estimated_absorpt_t_min   0.699
_shelx_estimated_absorpt_t_max   0.879
_shelxl_version_number           2012-6
_shelx_res_checksum              68180
_shelx_hkl_checksum              53452