Allenylphosphonium Complexes of Rhodium and Iridium
Cade, Ian A.; Colebatch, Annie L.; Hill, Anthony F.; Willis, Anthony C.; Organometallics 33 (2014) 3198–; doi:10.1021/om500450e

data_4083595
_publ_section_title
;
 Allenylphosphonium Complexes of Rhodium and Iridium
;
_journal_issue                   12
_journal_name_full               Organometallics
_journal_page_first              3198
_journal_paper_doi               10.1021/om500450e
_journal_volume                  33
_journal_year                    2014
_chemical_compound_source        'Research School of Chemistry'
_chemical_formula_moiety         'C58 H48 Cl Ir O P3, 0.5(F6 P), C H2 Cl2'
_chemical_formula_sum            'C59 H50 Cl3 F3 Ir O P3.5'
_chemical_formula_weight         1239.03
_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
_cell_angle_alpha                79.893(3)
_cell_angle_beta                 83.090(3)
_cell_angle_gamma                75.388(3)
_cell_formula_units_Z            2
_cell_length_a                   14.0258(7)
_cell_length_b                   14.9269(9)
_cell_length_c                   16.7575(9)
_cell_measurement_reflns_used    9551
_cell_measurement_temperature    200
_cell_measurement_theta_max      25
_cell_measurement_theta_min      2.55
_cell_volume                     3331.6(3)
_computing_cell_refinement       'DENZO/SCALEPACK (Otwinowski & Minor, 1997)'
_computing_data_collection       'COLLECT (Nonius, 2001).'
_computing_data_reduction        'DENZO/SCALEPACK (Otwinowski & Minor, 1997)'
_computing_molecular_graphics    'Ortep-3 for Windows v. 2.01'
_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      200
_diffrn_measured_fraction_theta_full 0.965
_diffrn_measured_fraction_theta_max 0.965
_diffrn_measurement_device       'Nonius KappaCCD'
_diffrn_measurement_device_type  Area
_diffrn_measurement_method       \w
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.035
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_number            31035
_diffrn_reflns_theta_full        25.158
_diffrn_reflns_theta_max         25.158
_diffrn_reflns_theta_min         2.572
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    2.249
_exptl_absorpt_correction_T_max  0.73
_exptl_absorpt_correction_T_min  0.57
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'DENZO/SCALEPACK (Otwinowski & Minor, 1997)'
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.235
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             1239
_exptl_crystal_size_max          0.380
_exptl_crystal_size_mid          0.190
_exptl_crystal_size_min          0.140
_platon_squeeze_details
;

;
_refine_diff_density_max         1.51
_refine_diff_density_min         -1.77
_refine_ls_extinction_method     None
_refine_ls_goodness_of_fit_ref   1.0189
_refine_ls_hydrogen_treatment    none
_refine_ls_matrix_type           full
_refine_ls_number_parameters     637
_refine_ls_number_reflns         11476
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0549
_refine_ls_R_factor_gt           0.0444
_refine_ls_shift/su_max          0.0033702
_refine_ls_shift/su_mean         0.3131096
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
;
 Method= Modified Sheldrick 
 w=1/[\s^2^(F^2^) + ( 0.06P)^2^ + 9.34P] 
 ,where P=(max(Fo^2^,0) + 2Fc^2^)/3 
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.1218
_refine_ls_wR_factor_gt          0.1100
_refine_ls_wR_factor_ref         0.1218
_reflns_limit_h_max              16
_reflns_limit_h_min              -16
_reflns_limit_k_max              17
_reflns_limit_k_min              -17
_reflns_limit_l_max              19
_reflns_limit_l_min              0
_reflns_number_gt                9873
_reflns_number_total             11514
_reflns_threshold_expression     I>2.0\s(I)
_oxford_diffrn_Wilson_B_factor   3.01
_oxford_diffrn_Wilson_scale      15.50
_oxford_refine_ls_r_factor_ref   0.0549
_oxford_refine_ls_scale          0.26709(17)
_oxford_reflns_number_all        11476
_oxford_reflns_threshold_expression_ref I>-10.0\s(I)
_cod_data_source_file            om500450e_si_001.cif
_cod_data_source_block           1
_cod_depositor_comments
;
The following automatic conversions were performed:

'_symmetry_cell_setting' value 'Triclinic' changed to 'triclinic'
according to
/usr/data/users/saulius/crontab/automatic-downloads/rss-feeds/ACS/lib/dictionaries/cif_core.dic
dictionary named 'cif_core.dic' version 2.4.2 from 2011-04-26.

Automatic conversion script
Id: cif_fix_values 2281 2013-09-26 08:29:07Z andrius 

 Adding full bibliography for 4083595--4083597.cif.
;
_cod_original_sg_symbol_H-M      'P -1 '
_cod_original_formula_sum        'C59 H50 Cl3 F3 Ir1 O1 P3.50'
_cod_database_code               4083595