Unprecedented Reactivity of Iridium(I) Secondary Phosphine Oxide Complexes: Formation of P-Coordinated Phosphinate Complexes by P−Aryl Bond Cleavage
Liniger, Marc; Gschwend, Björn; Neuburger, Markus; Schaffner, Silvia; Pfaltz, Andreas; Organometallics 29 (2010) 5953–; doi:10.1021/om1007874

data_4067032
_publ_section_related_literature
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? 
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_publ_section_title
;
 Unprecedented Reactivity of Iridium(I) Secondary Phosphine Oxide
 Complexes: Formation of P-Coordinated Phosphinate Complexes by
 P&#x2212;Aryl Bond Cleavage
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_journal_issue                   22
_journal_name_full               Organometallics
_journal_page_first              5953
_journal_paper_doi               10.1021/om1007874
_journal_volume                  29
_journal_year                    2010
_chemical_absolute_configuration ad
_chemical_formula_moiety         'C82 H108 Ir2 N4 Na2 O14 P4, 4(C H4 O)'
_chemical_formula_sum            'C86 H124 Ir2 N4 Na2 O18 P4'
_chemical_formula_weight         2056.01
_space_group_IT_number           1
_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
_audit_creation_date             09-02-26
_audit_creation_method           CRYSTALS_ver_12.86
_cell_angle_alpha                94.386(2)
_cell_angle_beta                 105.047(2)
_cell_angle_gamma                118.562(2)
_cell_formula_units_Z            1
_cell_length_a                   12.3030(6)
_cell_length_b                   12.5477(6)
_cell_length_c                   18.1296(9)
_cell_measurement_reflns_used    9365
_cell_measurement_temperature    123
_cell_measurement_theta_max      31
_cell_measurement_theta_min      3
_cell_volume                     2306.5(2)
_computing_cell_refinement       'DENZO/SCALEPACK (Otwinowski & Minor, 1997)'
_computing_data_collection       'COLLECT (Nonius, 1997-2001).'
_computing_data_reduction        'DENZO/SCALEPACK (Otwinowski & Minor, 1997)'
_computing_molecular_graphics    'CAMERON (Watkin et al., 1996)'
_computing_publication_material  'CRYSTALS (Betteridge et al., 2003)'
_computing_structure_refinement  'CRYSTALS (Betteridge et al., 2003)'
_computing_structure_solution    'SIR92 (Altomare et al., 1994)'
_diffrn_ambient_temperature      123
_diffrn_measured_fraction_theta_full 0.996
_diffrn_measured_fraction_theta_max 0.962
_diffrn_measurement_device       'Nonius KappaCCD'
_diffrn_measurement_device_type  Area
_diffrn_measurement_method       '\f & \w scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.023
_diffrn_reflns_limit_h_max       25
_diffrn_reflns_limit_h_min       -25
_diffrn_reflns_limit_k_max       26
_diffrn_reflns_limit_k_min       -26
_diffrn_reflns_limit_l_max       37
_diffrn_reflns_limit_l_min       -37
_diffrn_reflns_number            165710
_diffrn_reflns_theta_full        32.010
_diffrn_reflns_theta_max         47.776
_diffrn_reflns_theta_min         1.902
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    3.026
_exptl_absorpt_correction_T_max  0.76
_exptl_absorpt_correction_T_min  0.70
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'DENZO/SCALEPACK (Otwinowski & Minor, 1997)'
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.480
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             1047.750
_exptl_crystal_size_max          0.36
_exptl_crystal_size_mid          0.12
_exptl_crystal_size_min          0.09
_refine_diff_density_max         2.67
_refine_diff_density_min         -1.32
_refine_ls_abs_structure_details 'Flack (1983), 0 Friedel-pairs'
_refine_ls_abs_structure_Flack   .0021(11)
_refine_ls_extinction_method     None
_refine_ls_goodness_of_fit_ref   1.0858
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1055
_refine_ls_number_reflns         66386
_refine_ls_number_restraints     5
_refine_ls_R_factor_all          0.0285
_refine_ls_R_factor_gt           0.0213
_refine_ls_shift/su_max          0.001330
_refine_ls_structure_factor_coef F
_refine_ls_weighting_details
;
 Method, part 1, Chebychev polynomial, (Watkin, 1994, Prince, 1982) 
 [weight] = 1.0/[A~0~*T~0~(x)+A~1~*T~1~(x) ... +A~n-1~]*T~n-1~(x)] 
 where A~i~ are the Chebychev coefficients listed below and x= Fcalc/Fmax 
 Method = Robust Weighting (Prince, 1982) 
 W = [weight] * [1-(deltaF/6*sigmaF)^2^]^2^ 
 A~i~ are: 
 0.125 0.155E-02 0.283E-01 
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.0258
_refine_ls_wR_factor_gt          0.0202
_refine_ls_wR_factor_ref         0.0196
_reflns_limit_h_max              25
_reflns_limit_h_min              -25
_reflns_limit_k_max              26
_reflns_limit_k_min              -26
_reflns_limit_l_max              37
_reflns_limit_l_min              -37
_reflns_number_gt                69824
_reflns_number_total             80739
_reflns_threshold_expression     I>2.0\s(I)
_oxford_diffrn_Wilson_B_factor   0.93
_oxford_diffrn_Wilson_scale      43.60
_oxford_refine_ls_r_factor_ref   0.0200
_oxford_refine_ls_scale          0.15530(2)
_oxford_reflns_number_all        80695
_oxford_reflns_threshold_expression_ref I>3.0\s(I)
_oxford_structure_analysis_title 'ml011_5_s_123k_0m in P1'
_cod_data_source_file            om1007874_si_001.cif
_cod_data_source_block           ml011_5_s
_cod_depositor_comments
;
The following automatic conversions were performed:

'_symmetry_cell_setting' value 'Triclinic' changed to 'triclinic'
according to /home/saulius/struct/CIF-dictionaries/cif_core.dic
dictionary named 'cif_core.dic' version 2.4.1 from 2010-06-29.

Automatic conversion script
Id: cif_fix_values 1715 2011-07-08 13:25:40Z adriana 
;
_cod_original_sg_symbol_Hall     'P 1 '
_cod_original_sg_symbol_H-M      'P 1 '
_cod_database_code               4067032