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_7009040
_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            'C20 H6 Fe5 O14'
_chemical_formula_weight         749.50
_space_group_IT_number           14
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/c 1'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           'manual editing'
_cell_angle_alpha                90.00
_cell_angle_beta                 100.24(2)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   8.784(2)
_cell_length_b                   20.684(6)
_cell_length_c                   14.325(3)
_cell_measurement_reflns_used    30
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      17.5
_cell_measurement_theta_min      10
_cell_volume                     2561.2(11)
_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       omega
_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  0.0245
_diffrn_reflns_av_sigmaI/netI    0.0644
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       0
_diffrn_reflns_limit_k_max       24
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            4809
_diffrn_reflns_theta_max         25.00
_diffrn_reflns_theta_min         1.75
_diffrn_standards_decay_%        0
_diffrn_standards_interval_count 50
_diffrn_standards_number         2
_exptl_absorpt_coefficient_mu    2.833
_exptl_absorpt_correction_T_max  0.176
_exptl_absorpt_correction_T_min  0.131
_exptl_absorpt_correction_type   'semi-empirical from psi-scan'
_exptl_crystal_colour            black
_exptl_crystal_density_diffrn    1.944
_exptl_crystal_description       prism
_exptl_crystal_F_000             1472
_exptl_crystal_size_max          '0.12 x 0.20 x 0.42 '
_refine_diff_density_max         0.369
_refine_diff_density_min         -0.314
_refine_diff_density_rms         0.080
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_all   1.036
_refine_ls_goodness_of_fit_obs   1.104
_refine_ls_matrix_type           full
_refine_ls_number_parameters     370
_refine_ls_number_reflns         4502
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.037
_refine_ls_restrained_S_obs      1.104
_refine_ls_R_factor_all          0.0921
_refine_ls_R_factor_obs          0.0417
_refine_ls_shift/esd_max         0.115
_refine_ls_shift/esd_mean        0.005
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0251P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.0796
_refine_ls_wR_factor_obs         0.0656
_reflns_number_observed          2838
_reflns_number_total             4502
_reflns_observed_criterion       >2sigma(I)
_cod_data_source_file            a908308a.txt
_cod_data_source_block           Fe5(CO)14(C2Me)2
_cod_depositor_comments
;
The following automatic conversions were performed:

'_refine_ls_weighting_scheme' value 'calc
w=1/[\s^2^(Fo^2^)+(0.0251P)^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^)+(0.0251P)^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 
;
_cod_original_cell_volume        2561(1)
_cod_database_code               7009040