Effects of the Heterocycle and Its Substituents on Structure and Fluxionality in Rhodium(I) and Iridium(I) Complexes with the Hindered Thiolates 6-tert-Butylpyridine-2-thiolate and 1-Alkyl-4-tert-butylimidazole-2-thiolate (alkyl = methyl andtert-butyl)
Miranda-Soto, Valentín; Pérez-Torrente, Jesús J.; Oro, Luis A.; Lahoz, Fernando J.; Martín, M. Luisa; Parra-Hake, Miguel; Grotjahn, Douglas B.; Organometallics 25 (2006) 4374–; doi:10.1021/om060317t

data_4075483
_publ_section_title
;
 Effects of the Heterocycle and Its Substituents on Structure and
 Fluxionality in Rhodium(I) and Iridium(I) Complexes with the Hindered
 Thiolates 6-tert-Butylpyridine-2-thiolate and
 1-Alkyl-4-tert-butylimidazole-2-thiolate (alkyl = methyl andtert-butyl)
;
_journal_issue                   18
_journal_name_full               Organometallics
_journal_page_first              4374
_journal_paper_doi               10.1021/om060317t
_journal_volume                  25
_journal_year                    2006
_chemical_formula_moiety         'C30 H34 Ir N2 O P S'
_chemical_formula_sum            'C30 H34 Ir N2 O P S'
_chemical_formula_weight         693.82
_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                99.912(5)
_cell_angle_beta                 94.141(5)
_cell_angle_gamma                104.632(5)
_cell_formula_units_Z            2
_cell_length_a                   9.243(5)
_cell_length_b                   9.618(5)
_cell_length_c                   16.901(5)
_cell_measurement_reflns_used    4865
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      25.45
_cell_measurement_theta_min      2.23
_cell_volume                     1421.5(11)
_computing_cell_refinement       'SAINT+ v. 6.01 (Bruker AXS, 2000)'
_computing_data_collection       'SMART v. 5.611 (Bruker AXS, 2000)'
_computing_data_reduction        'SAINT+ v. 6.01 (Bruker AXS, 2000)'
_computing_molecular_graphics    'XP program, SHELXTL v6.12, Bruker2000'
_computing_publication_material  'XCIF program, SHELXTLv6.12, BrukerAXS'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      100(2)
_diffrn_detector_area_resol_mean 8.26
_diffrn_measured_fraction_theta_full 0.987
_diffrn_measured_fraction_theta_max 0.912
_diffrn_measurement_device_type  'Bruker SMART APEX CCD system'
_diffrn_measurement_method       '\w rotations with narrow frames'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71069
_diffrn_reflns_av_R_equivalents  0.0368
_diffrn_reflns_av_sigmaI/netI    0.0495
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_number            17587
_diffrn_reflns_theta_full        27.50
_diffrn_reflns_theta_max         28.71
_diffrn_reflns_theta_min         2.23
_diffrn_standards_decay_%        'no decay'
_exptl_absorpt_coefficient_mu    4.851
_exptl_absorpt_correction_T_max  0.7835
_exptl_absorpt_correction_T_min  0.4954
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
; 
 SADABS: Area-Detector Absorption Correction. (1996)  Bruker-AXS 
 within SAINT+ package, v. 6.01.                    
;
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.621
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       'irregular block'
_exptl_crystal_F_000             688
_exptl_crystal_size_max          0.16
_exptl_crystal_size_mid          0.13
_exptl_crystal_size_min          0.05
_refine_diff_density_max         1.193
_refine_diff_density_min         -1.609
_refine_diff_density_rms         0.136
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.046
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     429
_refine_ls_number_reflns         6712
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.046
_refine_ls_R_factor_all          0.0392
_refine_ls_R_factor_gt           0.0318
_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^)+(0.0288P)^2^+0.3227P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0627
_refine_ls_wR_factor_ref         0.0650
_reflns_number_gt                5954
_reflns_number_total             6712
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            om060317tsi20060409_093204.cif
_cod_data_source_block           compd_18
_cod_original_sg_symbol_H-M      P-1
_cod_database_code               4075483