Fluorination of [Os3(CO)12] and [Ir4(CO)12]
In-Chul Hwang; Konrad Seppelt; Inorganic Chemistry 42 (2003) 7116–7122; doi:10.1021/ic034611e

data_4312421
_publ_contact_author
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     Prof. Dr. Konrad Seppelt
     Institut f\"ur Chemie / Anorganische und Analytische Chemie
     Freie Universit\"at Berlin
     Fabeckstr. 34-36
     14195 Berlin
     Bundesrepublik Deutschland
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_publ_contact_author_email       seppelt@chemie.fu-berlin.de
_publ_contact_author_fax         '049 30 83852424'
_publ_contact_author_phone       '049 30 83854289'
_publ_section_title
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 Fluorination of [Os3(CO)12] and [Ir4(CO)12]
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_journal_name_full               'Inorganic Chemistry'
_journal_page_first              7116
_journal_page_last               7122
_journal_paper_doi               10.1021/ic034611e
_journal_volume                  42
_journal_year                    2003
_chemical_formula_moiety         fac-[Ir(CO)3(SbF6)2(HF(SbF6))](HF)
_chemical_formula_sum            'C3 H2 F20 Ir O3 Sb3'
_chemical_formula_weight         1023.50
_chemical_name_common
'fac - Tricarbonyl iridium tri hexafluoroantimonate dihydrogenfluorid'
_chemical_name_systematic
; 
 fac - Tricarbonyl iridium tri hexafluoroantimonate dihydrogenfluorid
;
_space_group_IT_number           62
_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_Hall  '-P 2ac 2n'
_symmetry_space_group_name_H-M   'P n m a'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   12.5060(14)
_cell_length_b                   13.4074(16)
_cell_length_c                   10.9263(19)
_cell_measurement_temperature    103(2)
_cell_volume                     1832.0(4)
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      103(2)
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measurement_device_type  'Bruker Smart CCD 1000 TM'
_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  0.0367
_diffrn_reflns_av_sigmaI/netI    0.0170
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_number            21363
_diffrn_reflns_theta_full        30.57
_diffrn_reflns_theta_max         30.57
_diffrn_reflns_theta_min         2.40
_exptl_absorpt_coefficient_mu    11.817
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.664
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
'Equilibration of symmetry equivalent reflections'
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    3.711
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       cube
_exptl_crystal_F_000             1816
_exptl_crystal_size_max          0.1
_exptl_crystal_size_mid          0.1
_exptl_crystal_size_min          0.1
_refine_diff_density_max         1.645
_refine_diff_density_min         -2.305
_refine_diff_density_rms         0.238
_refine_ls_extinction_coef       0.00053(4)
_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_ref   1.453
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     178
_refine_ls_number_reflns         2912
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.453
_refine_ls_R_factor_all          0.0328
_refine_ls_R_factor_gt           0.0316
_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^)+(0.0000P)^2^+23.7369P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0677
_refine_ls_wR_factor_ref         0.0680
_reflns_number_gt                2820
_reflns_number_total             2912
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic034611esi20030818_105927_3.cif
_cod_data_source_block           irco3
_cod_depositor_comments
;
The following automatic conversions were performed:

'_exptl_absorpt_correction_type' value 'multiscan' changed to
'multi-scan' according to the built-in table from CIF Core dictionary
named 'cif_core.dic' version 2.4.1 from 2010-06-29.

Automatic conversion script
Id: cif_fix_values 1646 2011-03-28 12:23:43Z adriana 
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_cod_database_code               4312421