POP-Pincer Silyl Complexes of Group 9: Rhodium versus Iridium
Miguel A. Esteruelas; Montserrat Oliván; Andrea Vélez; Inorganic Chemistry 52 (2013) 12108–12119; doi:10.1021/ic401931y

data_4336462
_publ_contact_author
;
  Dr. Montserrat Oliv\'an
  Departamento de Qu\'imica Inorg\'anica - ISQCH
  Universidad de Zaragoza - CSIC
  50009 Zaragoza, Spain
;
_publ_contact_author_email       molivan@unizar.es
_publ_section_title
;
 POP-Pincer Silyl Complexes of Group 9: Rhodium versus Iridium
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              12108
_journal_page_last               12119
_journal_paper_doi               10.1021/ic401931y
_journal_volume                  52
_journal_year                    2013
_chemical_formula_sum            'C51 H62 Cl O P2 Rh Si'
_chemical_formula_weight         919.40
_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                77.8960(10)
_cell_angle_beta                 84.2760(10)
_cell_angle_gamma                71.9240(10)
_cell_formula_units_Z            2
_cell_length_a                   10.2599(7)
_cell_length_b                   11.9553(8)
_cell_length_c                   20.3304(14)
_cell_measurement_reflns_used    9745
_cell_measurement_temperature    120(2)
_cell_measurement_theta_max      28
_cell_measurement_theta_min      2
_cell_volume                     2316.3(3)
_computing_cell_refinement       'APEX2 v2008.4-0, Bruker AXS'
_computing_data_collection       'APEX2 v2008.4-0, Bruker AXS'
_computing_data_reduction
;
  SAINT-Bruker integration program embedded in APEX2 v2008.4-0, Bruker AXS
;
_computing_molecular_graphics    'XP, SHELXTL v. 6.1 (Bruker, 2000)'
_computing_publication_material  'XCIF, SHELXTL v. 6.1 (Bruker, 2000)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      120(2)
_diffrn_detector_area_resol_mean 8.26
_diffrn_measured_fraction_theta_full 0.973
_diffrn_measured_fraction_theta_max 0.904
_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     0.71073
_diffrn_reflns_av_R_equivalents  0.0386
_diffrn_reflns_av_sigmaI/netI    0.0520
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       27
_diffrn_reflns_limit_l_min       -27
_diffrn_reflns_number            27059
_diffrn_reflns_theta_full        27.50
_diffrn_reflns_theta_max         28.50
_diffrn_reflns_theta_min         1.03
_diffrn_standards_decay_%        'no decay'
_exptl_absorpt_coefficient_mu    0.557
_exptl_absorpt_correction_T_max  0.862
_exptl_absorpt_correction_T_min  0.642
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
Absorption correction performed with SADABS program. This is based on the
method of Blessing: Blessing, R. H., Acta Crystallogr., Sect. A 1995, 51, 33.

SADABS: Area-Detector Absorption Correction. Bruker-AXS 
within SAINT+ package, v. 6.1 (2000).
;
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    1.318
_exptl_crystal_description       prism
_exptl_crystal_F_000             964
_exptl_crystal_size_max          0.22
_exptl_crystal_size_mid          0.13
_exptl_crystal_size_min          0.09
_refine_diff_density_max         0.747
_refine_diff_density_min         -0.793
_refine_diff_density_rms         0.086
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.071
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     488
_refine_ls_number_reflns         10623
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.071
_refine_ls_R_factor_all          0.0611
_refine_ls_R_factor_gt           0.0460
_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^)+(0.0218P)^2^+3.3991P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0873
_refine_ls_wR_factor_ref         0.0940
_reflns_number_gt                8775
_reflns_number_total             10623
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic401931y_si_001_3.cif
_cod_data_source_block           enrique135
_cod_database_code               4336462