Synthesis, Structure, and Magnetic Properties of Low-Valent Triangulo Cobalt-Hydride Clusters [XCo~3~(μ-CO)~3~(PMe~3~)~6~]
Hans-Friedrich Klein; Michael Mager; Andreas Schmidt; Martina Hüber; Wolfgang Haase; Ulrich Flörke; Hans-Jürgen Haupt; Roman Boca; Inorganic Chemistry 36 (1997) 4303–4306; doi:10.1021/ic970431r

data_4323606
_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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 Synthesis, Structure, and Magnetic Properties of Low-Valent Triangulo
 Cobalt-Hydride Clusters [XCo~3~(\m-CO)~3~(PMe~3~)~6~]
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_journal_name_full               'Inorganic Chemistry'
_journal_page_first              4303
_journal_page_last               4306
_journal_paper_doi               10.1021/ic970431r
_journal_volume                  36
_journal_year                    1997
_chemical_formula_sum            'C21 H57 Co3 O3 P6'
_chemical_formula_weight         720.27
_chemical_name_systematic
; 
  tri-\m-carbonyl-di-\m-hydrido-hydrido-hexakis-trimethylphosphane-triangulo-
  tricobalt  
;
_space_group_IT_number           167
_symmetry_cell_setting           trigonal
_symmetry_space_group_name_Hall  '-R 3 2"c'
_symmetry_space_group_name_H-M   'R -3 c :H'
_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                 90.00
_cell_angle_gamma                120.00
_cell_formula_units_Z            6
_cell_length_a                   10.679(2)
_cell_length_b                   10.679(2)
_cell_length_c                   52.729(12)
_cell_measurement_reflns_used    26
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      17
_cell_measurement_theta_min      8
_cell_volume                     5207.6(18)
_computing_structure_refinement  'SHELXTL V5 (Siemens, 1995)'
_computing_structure_solution    'SHELXTL V5 (Siemens, 1995)'
_diffrn_ambient_temperature      293(2)
_diffrn_measurement_device       'Siemens R3m/V'
_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    0.0247
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       0
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       68
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_number            3828
_diffrn_reflns_theta_max         27.56
_diffrn_reflns_theta_min         2.69
_diffrn_standards_decay_%        0
_diffrn_standards_interval_count 400
_diffrn_standards_number         3
_exptl_absorpt_coefficient_mu    1.713
_exptl_absorpt_correction_T_max  0.798
_exptl_absorpt_correction_T_min  0.756
_exptl_absorpt_correction_type   'empirical via psi-scans'
_exptl_crystal_colour            red-brown
_exptl_crystal_density_diffrn    1.376
_exptl_crystal_description       bloc
_exptl_crystal_F_000             2268
_exptl_crystal_size_max          0.40
_exptl_crystal_size_mid          0.39
_exptl_crystal_size_min          0.35
_refine_diff_density_max         0.307
_refine_diff_density_min         -0.316
_refine_diff_density_rms         0.051
_refine_ls_extinction_coef       0.00001(6)
_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   1.046
_refine_ls_goodness_of_fit_obs   1.070
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     57
_refine_ls_number_reflns         1340
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.046
_refine_ls_restrained_S_obs      1.070
_refine_ls_R_factor_all          0.0346
_refine_ls_R_factor_obs          0.0241
_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^)+(0.0258P)^2^+4.5518P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.0571
_refine_ls_wR_factor_obs         0.0533
_reflns_number_observed          1122
_reflns_number_total             1340
_reflns_observed_criterion       >2sigma(I)
_cod_data_source_file            ic970431r_2.cif
_cod_data_source_block           3
_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^)+(0.0258P)^2^+4.5518P] 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^)+(0.0258P)^2^+4.5518P] where P=(Fo^2^+2Fc^2^)/3'.

Automatic conversion script
Id: cif_fix_values 3143 2015-03-26 13:38:13Z robertas 
;
_cod_original_sg_symbol_H-M      'R -3 c'
_cod_database_code               4323606