Metal fragment condensation and carbon‒carbon bond cleavage in reactions of [Fe3(CO)12] with internal propargyl alcohols. Structures of the “bow tie” acetylide complexes [Fe5(CO)14(C2R)2] (R =Me or Et)
Brait, Sabrina; Gervasio, Giuliana; Marabello, Domenica; Sappa, Enrico; Journal of the Chemical Society, Dalton Transactions  (2000) 989–; doi:10.1039/a908308a

data_7009041
_publ_section_title
;
 Metal fragment condensation and carbon--carbon bond cleavage in
 reactions of [Fe3(CO)12] with internal propargyl alcohols. Structures
 of the &#x201C;bow tie&#x201D; acetylide complexes [Fe5(CO)14(C2R)2]
 (R&#x2005;=Me or Et)
;
_journal_issue                   6
_journal_name_full
'Journal of the Chemical Society, Dalton Transactions'
_journal_page_first              989
_journal_paper_doi               10.1039/a908308a
_journal_year                    2000
_chemical_formula_sum            'C22 H10 Fe5 O14'
_chemical_formula_weight         777.55
_space_group_IT_number           2
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           'manual editing'
_cell_angle_alpha                88.53(4)
_cell_angle_beta                 84.83(4)
_cell_angle_gamma                76.67(4)
_cell_formula_units_Z            2
_cell_length_a                   9.009(5)
_cell_length_b                   9.949(5)
_cell_length_c                   15.673(8)
_cell_measurement_reflns_used    30
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      17.5
_cell_measurement_theta_min      10
_cell_volume                     1361.4(13)
_computing_cell_refinement       'Siemens P3'
_computing_data_collection       'Siemens P3'
_computing_data_reduction        'Siemens P3'
_computing_structure_refinement  'SHELXL-93 (Sheldrick,1993)'
_computing_structure_solution    'SHELXS-86 (Sheldrick,1990)'
_diffrn_ambient_temperature      293(2)
_diffrn_measurement_device       ' Siemens P4 '
_diffrn_measurement_method       theta-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  0.0331
_diffrn_reflns_av_sigmaI/netI    0.0959
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_number            4932
_diffrn_reflns_theta_max         25.05
_diffrn_reflns_theta_min         2.10
_diffrn_standards_decay_%        0
_diffrn_standards_interval_count 50
_diffrn_standards_number         2
_exptl_absorpt_coefficient_mu    2.669
_exptl_absorpt_correction_T_max  0.216
_exptl_absorpt_correction_T_min  0.156
_exptl_absorpt_correction_type   'semi-empirical from psi-scan'
_exptl_crystal_colour            black
_exptl_crystal_density_diffrn    1.897
_exptl_crystal_description       prism
_exptl_crystal_F_000             768
_exptl_crystal_size_max          '0.14 x 0.26 x 0.54 '
_refine_diff_density_max         0.557
_refine_diff_density_min         -0.487
_refine_diff_density_rms         0.106
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_all   1.043
_refine_ls_goodness_of_fit_obs   1.120
_refine_ls_matrix_type           full
_refine_ls_number_parameters     400
_refine_ls_number_reflns         4749
_refine_ls_number_restraints     0
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_refine_ls_restrained_S_obs      1.120
_refine_ls_R_factor_all          0.1219
_refine_ls_R_factor_obs          0.0532
_refine_ls_shift/esd_max         0.150
_refine_ls_shift/esd_mean        0.010
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0417P)^2^+1.4963P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.1168
_refine_ls_wR_factor_obs         0.0946
_reflns_number_observed          2723
_reflns_number_total             4749
_reflns_observed_criterion       >2sigma(I)
_cod_data_source_file            a908308a.txt
_cod_data_source_block           Fe5(CO)14(C2Et)2
_cod_depositor_comments
;
The following automatic conversions were performed:

'_refine_ls_weighting_scheme' value 'calc
w=1/[\s^2^(Fo^2^)+(0.0417P)^2^+1.4963P] 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^)+(0.0417P)^2^+1.4963P] 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        1361(1)
_cod_database_code               7009041