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_4335356
_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         'C41 H40 B N2 O P2 Rh'
_chemical_formula_sum            'C41 H40 B N2 O P2 Rh'
_chemical_formula_weight         752.41
_chemical_name_systematic
;
 ?
;
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 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                 102.177(3)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   11.203(2)
_cell_length_b                   24.429(4)
_cell_length_c                   13.786(2)
_cell_measurement_reflns_used    2707
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      24.42
_cell_measurement_theta_min      2.25
_cell_volume                     3688.0(10)
_computing_cell_refinement       'SAINT+ v. 7.56A (Bruker AXS, 2008)'
_computing_data_collection       'SMART v. 5.611 (Bruker AXS, 2000)'
_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 0.998
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device_type  'Bruker SMART APEX CCD system'
_diffrn_measurement_method       '\W rotations with narrow frames'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'normal-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0546
_diffrn_reflns_av_sigmaI/netI    0.0643
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       29
_diffrn_reflns_limit_k_min       -29
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       -10
_diffrn_reflns_number            21901
_diffrn_reflns_theta_full        26.00
_diffrn_reflns_theta_max         26.00
_diffrn_reflns_theta_min         1.67
_diffrn_standards_decay_%        'no decay'
_exptl_absorpt_coefficient_mu    0.584
_exptl_absorpt_correction_T_max  0.9475
_exptl_absorpt_correction_T_min  0.8342
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
; 
  SADABS-2008/1: Area-Detector Absorption Correction. Bruker-AXS 
;
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.355
_exptl_crystal_description       'prismatic block'
_exptl_crystal_F_000             1552
_exptl_crystal_size_max          0.14
_exptl_crystal_size_mid          0.11
_exptl_crystal_size_min          0.07
_refine_diff_density_max         0.710
_refine_diff_density_min         -0.360
_refine_diff_density_rms         0.083
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.998
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     433
_refine_ls_number_reflns         7220
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.998
_refine_ls_R_factor_all          0.0653
_refine_ls_R_factor_gt           0.0407
_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^)+(0.0406P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0841
_refine_ls_wR_factor_ref         0.0939
_reflns_number_gt                5300
_reflns_number_total             7220
_reflns_threshold_expression     >2\s(I)
_cod_data_source_file            ic400684s_si_002_4.cif
_cod_data_source_block           ctb49as
_cod_database_code               4335356