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_4067033
_publ_section_related_literature
; 
? 
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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_formula_moiety         'C25 H30 Ir N O3 P'
_chemical_formula_sum            'C25 H30 Ir N O3 P'
_chemical_formula_weight         615.71
_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
_audit_creation_date             09-02-18
_audit_creation_method           CRYSTALS_ver_12.86
_cell_angle_alpha                90.959(3)
_cell_angle_beta                 102.327(3)
_cell_angle_gamma                109.466(3)
_cell_formula_units_Z            4
_cell_length_a                   13.0064(9)
_cell_length_b                   13.3860(9)
_cell_length_c                   14.1812(9)
_cell_measurement_reflns_used    9929
_cell_measurement_temperature    123
_cell_measurement_theta_max      28
_cell_measurement_theta_min      3
_cell_volume                     2263.8(3)
_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    'SIR97 (Altomare et al., 1999)'
_diffrn_ambient_temperature      123
_diffrn_measured_fraction_theta_full 0.964
_diffrn_measured_fraction_theta_max 0.904
_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  0.044
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            42039
_diffrn_reflns_theta_full        25.265
_diffrn_reflns_theta_max         28.072
_diffrn_reflns_theta_min         1.707
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    5.996
_exptl_absorpt_correction_T_max  0.58
_exptl_absorpt_correction_T_min  0.38
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'DENZO/SCALEPACK (Otwinowski & Minor, 1997)'
_exptl_crystal_colour            orange
_exptl_crystal_density_diffrn    1.806
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             1212
_exptl_crystal_size_max          0.31
_exptl_crystal_size_mid          0.16
_exptl_crystal_size_min          0.09
_refine_diff_density_max         5.08
_refine_diff_density_min         -2.72
_refine_ls_extinction_method     None
_refine_ls_goodness_of_fit_ref   1.1182
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     559
_refine_ls_number_reflns         7215
_refine_ls_number_restraints     119
_refine_ls_R_factor_all          0.0851
_refine_ls_R_factor_gt           0.0613
_refine_ls_shift/su_max          0.013042
_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: 
 0.998 1.12 1.00 0.427 0.270 
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.0779
_refine_ls_wR_factor_gt          0.0609
_refine_ls_wR_factor_ref         0.0596
_reflns_limit_h_max              16
_reflns_limit_h_min              -17
_reflns_limit_k_max              17
_reflns_limit_k_min              -17
_reflns_limit_l_max              18
_reflns_limit_l_min              0
_reflns_number_gt                7506
_reflns_number_total             9944
_reflns_threshold_expression     I>2.0\s(I)
_oxford_diffrn_Wilson_B_factor   1.50
_oxford_diffrn_Wilson_scale      119.65
_oxford_refine_ls_r_factor_ref   0.0590
_oxford_refine_ls_scale          0.06771(11)
_oxford_reflns_number_all        9917
_oxford_reflns_threshold_expression_ref I>3.0\s(I)
_oxford_structure_analysis_title 'ml007_2_123k_0m in P-1'
_cod_data_source_file            om1007874_si_001.cif
_cod_data_source_block           ml007_2_123k
_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_original_formula_sum        'C25 H30 Ir1 N1 O3 P1'
_cod_database_code               4067033