Rhodium and Iridium Complexes with a New Scorpionate Phosphane Ligand
Angel L. Serrano; Miguel A. Casado; José A. López; Cristina Tejel; Inorganic Chemistry 52 (2013) 7593–7607; doi:10.1021/ic400684s

data_4335353
_publ_contact_author
;
  Dr. Cristina Tejel
  I.S.Q.C.H. - Departamento de Qu\'imica Inorg\'anica 
  Facultad de Ciencias
  Universidad de Zaragoza
  50009 Zaragoza, Spain
;
_publ_contact_author_email       ctejel@unizar.es
_publ_section_title
;
 Rhodium and Iridium Complexes with a New Scorpionate Phosphane Ligand
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              7593
_journal_page_last               7607
_journal_paper_doi               10.1021/ic400684s
_journal_volume                  52
_journal_year                    2013
_chemical_formula_moiety         'C29 H31 B Ir N2 O5 P, 0.5(C6 H14)'
_chemical_formula_sum            'C32 H38 B Ir N2 O5 P'
_chemical_formula_weight         764.62
_chemical_name_systematic
;
 ?
;
_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                 90.491(2)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   18.5058(18)
_cell_length_b                   9.3837(9)
_cell_length_c                   18.6119(18)
_cell_measurement_reflns_used    3490
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      22.72
_cell_measurement_theta_min      2.19
_cell_volume                     3231.9(5)
_computing_cell_refinement       'SAINT+ v. 7.56A (Bruker AXS, 2008)'
_computing_data_collection       'APEX2 v. 4.0 (Bruker AXS, 2008)'
_computing_data_reduction        'SAINT+ v. 7.56A (Bruker AXS, 2008)'
_computing_molecular_graphics
;
ORTEP3 for Windows - L. J. Farrugia, 
J. Appl. Crystallogr. 1997, 30, 565.
;
_computing_structure_refinement
;
SHELX97 - Programs for Crystal Structure Analysis (Release 97-2). 
G. M. Sheldrick, Institut fur Anorganische Chemie der Universitat, 
Tammanstrasse 4, D-3400 Gottingen, Germany, 1998.
;
_computing_structure_solution
;
SHELX97 - Programs for Crystal Structure Analysis (Release 97-2). 
G. M. Sheldrick, Institut fur Anorganische Chemie der Universitat, 
Tammanstrasse 4, D-3400 Gottingen, Germany, 1998.
;
_diffrn_ambient_temperature      100(2)
_diffrn_detector_area_resol_mean 8.26
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 1.000
_diffrn_measurement_device_type  'Bruker SMART APEX CCD system'
_diffrn_measurement_method       '\w rotations with narrow frames'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0820
_diffrn_reflns_av_sigmaI/netI    0.0732
_diffrn_reflns_limit_h_max       22
_diffrn_reflns_limit_h_min       -22
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            24471
_diffrn_reflns_theta_full        25.20
_diffrn_reflns_theta_max         25.20
_diffrn_reflns_theta_min         2.19
_diffrn_source                   'normal-focus sealed tube'
_diffrn_standards_decay_%        0
_exptl_absorpt_coefficient_mu    4.222
_exptl_absorpt_correction_T_max  0.8723
_exptl_absorpt_correction_T_min  0.7292
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
; 
  SADABS-2008/1: Area-Detector Absorption Correction. Bruker-AXS 
;
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.571
_exptl_crystal_description       plate
_exptl_crystal_F_000             1524
_exptl_crystal_size_max          0.053
_exptl_crystal_size_mid          0.041
_exptl_crystal_size_min          0.020
_refine_diff_density_max         1.521
_refine_diff_density_min         -0.845
_refine_diff_density_rms         0.157
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.030
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     373
_refine_ls_number_reflns         5818
_refine_ls_number_restraints     27
_refine_ls_restrained_S_all      1.031
_refine_ls_R_factor_all          0.0704
_refine_ls_R_factor_gt           0.0402
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0362P)^2^+1.2380P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0793
_refine_ls_wR_factor_ref         0.0896
_reflns_number_gt                4237
_reflns_number_total             5818
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic400684s_si_002_1.cif
_cod_data_source_block           ctb97as
_cod_database_code               4335353