Xantphos-Type Complexes of Group 9: Rhodium versus Iridium
Miguel A. Esteruelas; Montserrat Oliván; Andrea Vélez; Inorganic Chemistry 52 (2013) 5339–5349; doi:10.1021/ic4002658

data_4334709
_publ_contact_author
;
  Dr. Montserrat Oliv\'an
  Departamento de Qu\'imica Inorg\'anica - ISQCH
  Facultad de Ciencias
  Universidad de Zaragoza - CSIC
  50009 Zaragoza, Spain
;
_publ_contact_author_email       molivan@unizar.es
_publ_section_title
;
 Xantphos-Type Complexes of Group 9: Rhodium versus Iridium
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              5339
_journal_page_last               5349
_journal_paper_doi               10.1021/ic4002658
_journal_volume                  52
_journal_year                    2013
_chemical_formula_sum            'C29 H43 Cl3 F3 Ir O4 P2 S'
_chemical_formula_weight         905.18
_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                101.4220(10)
_cell_angle_beta                 101.6680(10)
_cell_angle_gamma                90.3770(10)
_cell_formula_units_Z            4
_cell_length_a                   13.6250(15)
_cell_length_b                   15.8477(18)
_cell_length_c                   16.5679(19)
_cell_measurement_reflns_used    8113
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      28
_cell_measurement_theta_min      2
_cell_volume                     3430.1(7)
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_computing_data_collection       'APEX2 v2008.4-0, Bruker AXS'
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;
  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      100(2)
_diffrn_detector_area_resol_mean 8.26
_diffrn_measured_fraction_theta_full 0.973
_diffrn_measured_fraction_theta_max 0.899
_diffrn_measurement_device_type  'Bruker SMART APEX CCD system'
_diffrn_measurement_method       '\w rotations with narrow frames'
_diffrn_radiation_monochromator  graphite
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_diffrn_radiation_type           MoK\a
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_diffrn_reflns_limit_h_min       -18
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_number            40404
_diffrn_reflns_theta_full        27.50
_diffrn_reflns_theta_max         28.53
_diffrn_reflns_theta_min         1.53
_diffrn_standards_decay_%        'no decay'
_exptl_absorpt_coefficient_mu    4.330
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_exptl_absorpt_correction_T_min  0.4755
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;
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            'pale yellow'
_exptl_crystal_density_diffrn    1.753
_exptl_crystal_description       'irregular block'
_exptl_crystal_F_000             1800
_exptl_crystal_size_max          0.24
_exptl_crystal_size_mid          0.20
_exptl_crystal_size_min          0.06
_refine_diff_density_max         1.597
_refine_diff_density_min         -1.365
_refine_diff_density_rms         0.183
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.948
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     803
_refine_ls_number_reflns         15686
_refine_ls_number_restraints     8
_refine_ls_restrained_S_all      0.948
_refine_ls_R_factor_all          0.0792
_refine_ls_R_factor_gt           0.0440
_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^)+(0.0242P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0749
_refine_ls_wR_factor_ref         0.0862
_reflns_number_gt                10725
_reflns_number_total             15686
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic4002658_si_001_1.cif
_cod_data_source_block           montse22a
_cod_database_code               4334709