Stepwise Synthesis of the Functionalized Metallatetrahedron Re~2~(AuPPh~3~)~2~(μ-PCy~2~)(CO)~7~X (X = Cl, Br, I)
Hans-Jürgen Haupt; Meinhard Schwefer; Hans Egold; Ulrich Flörke; Inorganic Chemistry 36 (1997) 184–188; doi:10.1021/ic9606690

data_4323285
_publ_contact_author
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Dr Ulrich Fl\"orke
Anorganische und Analytische Chemie
Universit\"at-GH Paderborn
Warburgerstr. 100
D-33098 Paderborn, FRG
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_publ_contact_author_email       floe@mvaxac.uni-paderborn.de
_publ_contact_author_fax         '49 5251 60 3423'
_publ_contact_author_phone       '49 5251 60 2496'
_publ_section_title
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 Stepwise Synthesis of the Functionalized Metallatetrahedron
 Re~2~(AuPPh~3~)~2~(\m-PCy~2~)(CO)~7~X (X = Cl, Br, I)
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_journal_name_full               'Inorganic Chemistry'
_journal_page_first              184
_journal_page_last               188
_journal_paper_doi               10.1021/ic9606690
_journal_volume                  36
_journal_year                    1997
_chemical_formula_structural     '[C26 H28 O8 P Re2][Li]*2 THF * H2O'
_chemical_formula_sum            'C34 H46 Li O11 P Re2'
_chemical_formula_weight         1041.02
_chemical_name_systematic
; 
 lithium-\m-dicyclohexylphosphido-P,P-heptacarbonyl-dirhenium-benzoylate
 water bis-tetrahydrofurane solvate 
;
_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
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL
_cell_angle_alpha                98.010(10)
_cell_angle_beta                 89.940(10)
_cell_angle_gamma                112.220(10)
_cell_formula_units_Z            2
_cell_length_a                   10.536(2)
_cell_length_b                   11.433(2)
_cell_length_c                   19.125(3)
_cell_measurement_reflns_used    30
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      15
_cell_measurement_theta_min      7.5
_cell_volume                     2108.5(7)
_computing_structure_refinement  'SHELXTL V5'
_computing_structure_solution    'SHELXTL V5'
_diffrn_ambient_temperature      293(2)
_diffrn_measurement_device       'Siemens R3m'
_diffrn_measurement_method       omega-2theta
_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  0.0307
_diffrn_reflns_av_sigmaI/netI    0.0407
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_number            9800
_diffrn_reflns_theta_max         27.56
_diffrn_reflns_theta_min         2.25
_diffrn_standards_decay_%        7
_diffrn_standards_interval_count 400
_diffrn_standards_number         3
_exptl_absorpt_coefficient_mu    5.823
_exptl_absorpt_correction_T_max  0.597
_exptl_absorpt_correction_T_min  0.171
_exptl_absorpt_correction_type   'empirical via psi-scans'
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.640
_exptl_crystal_description       prism
_exptl_crystal_F_000             1012
_exptl_crystal_size_max          0.55
_exptl_crystal_size_mid          0.48
_exptl_crystal_size_min          0.15
_refine_diff_density_max         1.360
_refine_diff_density_min         -1.080
_refine_diff_density_rms         0.197
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_all   1.054
_refine_ls_goodness_of_fit_obs   1.071
_refine_ls_hydrogen_treatment    riding
_refine_ls_matrix_type           full
_refine_ls_number_parameters     472
_refine_ls_number_reflns         9531
_refine_ls_number_restraints     114
_refine_ls_restrained_S_all      1.056
_refine_ls_restrained_S_obs      1.070
_refine_ls_R_factor_all          0.0912
_refine_ls_R_factor_obs          0.0537
_refine_ls_shift/esd_max         -0.001
_refine_ls_shift/esd_mean        0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0972P)^2^+3.9949P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.1705
_refine_ls_wR_factor_obs         0.1401
_reflns_number_observed          6374
_reflns_number_total             9535
_reflns_observed_criterion       >2sigma(I)
_cod_data_source_file            ic9606690_1.cif
_cod_data_source_block           Li[2]
_cod_depositor_comments
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The following automatic conversions were performed:

'_refine_ls_weighting_scheme' value 'calc
w=1/[\s^2^(Fo^2^)+(0.0972P)^2^+3.9949P] 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^)+(0.0972P)^2^+3.9949P] where P=(Fo^2^+2Fc^2^)/3'.

Automatic conversion script
Id: cif_fix_values 3143 2015-03-26 13:38:13Z robertas 
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_cod_original_cell_volume        2108.5(6)
_cod_database_code               4323285