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_4323286
_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     'Au2 C55 H52 Cl O7 P3 Re2 * C H2 Cl2'
_chemical_formula_sum            'C56 H54 Au2 Cl3 O7 P3 Re2'
_chemical_formula_weight         1804.58
_chemical_name_systematic
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 \m-dicyclohexylphosphido-P,P-bis(triphenylphosphido-gold)-
 chloro-heptacarbonyl-dirhenium dichloromethane solvate
;
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL
_cell_angle_alpha                90.00
_cell_angle_beta                 105.14(2)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   18.615(5)
_cell_length_b                   13.606(2)
_cell_length_c                   24.223(6)
_cell_measurement_reflns_used    30
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      15
_cell_measurement_theta_min      7
_cell_volume                     5922(2)
_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  0.0622
_diffrn_reflns_av_sigmaI/netI    0.1762
_diffrn_reflns_limit_h_max       23
_diffrn_reflns_limit_h_min       -24
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       31
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_number            13991
_diffrn_reflns_theta_max         27.57
_diffrn_reflns_theta_min         2.31
_diffrn_standards_decay_%        10
_diffrn_standards_interval_count 400
_diffrn_standards_number         3
_exptl_absorpt_coefficient_mu    9.278
_exptl_absorpt_correction_T_max  0.527
_exptl_absorpt_correction_T_min  0.464
_exptl_absorpt_correction_type   psi-scans
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    2.024
_exptl_crystal_description       prism
_exptl_crystal_F_000             3400
_exptl_crystal_size_max          0.58
_exptl_crystal_size_mid          0.11
_exptl_crystal_size_min          0.10
_refine_diff_density_max         1.747
_refine_diff_density_min         -1.138
_refine_diff_density_rms         0.219
_refine_ls_extinction_coef       0.00000(2)
_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   0.970
_refine_ls_goodness_of_fit_obs   1.111
_refine_ls_hydrogen_treatment    riding
_refine_ls_matrix_type           full
_refine_ls_number_parameters     587
_refine_ls_number_reflns         13664
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.971
_refine_ls_restrained_S_obs      1.111
_refine_ls_R_factor_all          0.1936
_refine_ls_R_factor_obs          0.0744
_refine_ls_shift/esd_max         0.000
_refine_ls_shift/esd_mean        0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0505P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.1596
_refine_ls_wR_factor_obs         0.1194
_reflns_number_observed          6090
_reflns_number_total             13666
_reflns_observed_criterion       >2sigma(I)
_cod_data_source_file            ic9606690_2.cif
_cod_data_source_block           4a
_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^)+(0.0505P)^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^)+(0.0505P)^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 
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_cod_original_cell_volume        5922.1(23)
_cod_database_code               4323286