Iridium(III, 0, and -I) Complexes Stabilized by 1,1'-Bis(diphenylphosphino)ferrocene (dppf): Synthesis and Characterization. Crystal Structures of [Na(THF)5][Ir(dppf)2].THF and [Ir(dppf)2]
Bruno Longato; Lorenzo Riello; Giuliano Bandoli; Giuseppe Pilloni; Inorganic Chemistry 38 (1999) 2818–2823; doi:10.1021/ic981166s

data_4322067
_publ_section_title
;
 Iridium(III, 0, and -I) Complexes Stabilized by
 1,1'-Bis(diphenylphosphino)ferrocene (dppf): Synthesis and
 Characterization. Crystal Structures of [Na(THF)5][Ir(dppf)2].THF and
 [Ir(dppf)2]
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              2818
_journal_page_last               2823
_journal_paper_doi               10.1021/ic981166s
_journal_volume                  38
_journal_year                    1999
_chemical_formula_sum            'C92 H104 Fe2 Ir Na O6 P4'
_chemical_formula_weight         1756.52
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     heavy
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL
_cell_angle_alpha                90.00
_cell_angle_beta                 98.77(2)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   13.325(3)
_cell_length_b                   23.976(5)
_cell_length_c                   26.774(7)
_cell_measurement_reflns_used    50
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      15.7
_cell_measurement_theta_min      10.6
_cell_volume                     8454(3)
_computing_cell_refinement       'Siemens P3/P4-PC Ver.4.27 (1991)'
_computing_data_collection       'Siemens P3/P4-PC Ver.4.27 (1991)'
_computing_data_reduction        'Siemens P3/P4-PC Ver.4.27 (1991)'
_computing_molecular_graphics    'SHELXTL/PC Ver.5.03 (Sheldrick, 1994)'
_computing_publication_material  'SHELXTL/PC Ver.5.03 (Sheldrick, 1994)'
_computing_structure_refinement  'SHELXL-93 (Sheldrick, 1993)'
_computing_structure_solution    'SHELXTL/PC Ver.5.03 (Sheldrick, 1994)'
_diffrn_ambient_temperature      293(2)
_diffrn_measurement_device       'Nicolet R3m/V diffractometer'
_diffrn_measurement_method       'omega-2 theta'
_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  0.0470
_diffrn_reflns_av_sigmaI/netI    0.0590
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       0
_diffrn_reflns_limit_k_max       24
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       26
_diffrn_reflns_limit_l_min       -27
_diffrn_reflns_number            9061
_diffrn_reflns_theta_max         21.06
_diffrn_reflns_theta_min         2.02
_diffrn_standards_decay_%        'no decay'
_diffrn_standards_interval_count 150
_diffrn_standards_number         2
_exptl_absorpt_coefficient_mu    2.042
_exptl_absorpt_correction_T_max  0.77
_exptl_absorpt_correction_T_min  0.46
_exptl_absorpt_correction_type   psi-scan
_exptl_crystal_colour            dark_green
_exptl_crystal_density_diffrn    1.380
_exptl_crystal_description       parallelepipeds
_exptl_crystal_F_000             3616
_exptl_crystal_size_max          0.25
_exptl_crystal_size_mid          0.15
_exptl_crystal_size_min          0.10
_refine_diff_density_max         1.434
_refine_diff_density_min         -0.884
_refine_diff_density_rms         0.118
_refine_ls_extinction_coef       0.00008(10)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     SHELXL
_refine_ls_goodness_of_fit_all   1.138
_refine_ls_goodness_of_fit_obs   1.115
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     831
_refine_ls_number_reflns         8496
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.611
_refine_ls_restrained_S_obs      1.115
_refine_ls_R_factor_all          0.0727
_refine_ls_R_factor_obs          0.0427
_refine_ls_shift/esd_max         -1.156
_refine_ls_shift/esd_mean        0.019
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.1000P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.2096
_refine_ls_wR_factor_obs         0.1174
_reflns_number_observed          6454
_reflns_number_total             8570
_reflns_observed_criterion       >2sigma(I)
_cod_data_source_file            ic981166s_2.cif
_cod_data_source_block           Ir(-1)
_cod_depositor_comments
;
The following automatic conversions were performed:

'_refine_ls_weighting_scheme' value 'calc
w=1/[\s^2^(Fo^2^)+(0.1000P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' was
changed to 'calc'. New tag '_refine_ls_weighting_details' was
created. The value of the new tag was set to
'w=1/[\s^2^(Fo^2^)+(0.1000P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'.

Automatic conversion script
Id: cif_fix_values 3143 2015-03-26 13:38:13Z robertas 
;
_cod_original_cell_volume        8453.7(35)
_cod_database_code               4322067