Photochemical Alkyne Insertions into the Iron‒Thiocarbonyl Bond of [Fe2(CS)(CO)3(Cp)2]
Marchetti, Fabio; Zacchini, Stefano; Zanotti, Valerio; Organometallics 35 (2016) 2630–; doi:10.1021/acs.organomet.6b00349

data_4088724
_publ_section_title
;
 Photochemical Alkyne Insertions into the Iron--Thiocarbonyl Bond of
 [Fe2(CS)(CO)3(Cp)2]
;
_journal_issue                   16
_journal_name_full               Organometallics
_journal_page_first              2630
_journal_paper_doi               10.1021/acs.organomet.6b00349
_journal_volume                  35
_journal_year                    2016
_chemical_formula_sum            'C21 H23 F3 Fe2 O5 S2'
_chemical_formula_weight         588.21
_space_group_IT_number           14
_space_group_name_Hall           '-P 2yn'
_space_group_name_H-M_alt        'P 1 21/n 1'
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_H-M   'P 1 21/n 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 98.39(3)
_cell_angle_gamma                90.00
_cell_formula_units_Z            8
_cell_length_a                   17.733(4)
_cell_length_b                   14.481(3)
_cell_length_c                   19.052(4)
_cell_measurement_reflns_used    881
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      20.7625
_cell_measurement_theta_min      2.161
_cell_volume                     4840.0(18)
_computing_cell_refinement       'APEX2 (Bruker AXS, 2006)'
_computing_data_collection       'APEX2 (Bruker AXS, 2006)'
_computing_data_reduction        'SAINT (Bruker AXS, 2004)'
_computing_molecular_graphics    'ORTEPII (Johnson, 1996)'
_computing_publication_material  'XCIF (Bruker AXS, 2001)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 1.000
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       'phi and omega scans'
_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  0.1040
_diffrn_reflns_av_sigmaI/netI    0.0819
_diffrn_reflns_limit_h_max       21
_diffrn_reflns_limit_h_min       -21
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_number            41875
_diffrn_reflns_theta_full        25.03
_diffrn_reflns_theta_max         25.03
_diffrn_reflns_theta_min         1.47
_exptl_absorpt_coefficient_mu    1.424
_exptl_absorpt_correction_T_max  0.8591
_exptl_absorpt_correction_T_min  0.7736
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_process_details
; 
 Data were corrected for Lorentz polarization and absorption
 effects (empirical absorption correction SADABS).
 R(int) =  0.0748 (selected reflections only, before parameter refinement)
 R(int) =  0.0557 (selected reflections only, after parameter refinement)
;
_exptl_crystal_colour            black
_exptl_crystal_density_diffrn    1.614
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             2400
_exptl_crystal_size_max          0.19
_exptl_crystal_size_mid          0.14
_exptl_crystal_size_min          0.11
_refine_diff_density_max         1.207
_refine_diff_density_min         -0.847
_refine_diff_density_rms         0.122
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.044
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     589
_refine_ls_number_reflns         8556
_refine_ls_number_restraints     324
_refine_ls_restrained_S_all      1.067
_refine_ls_R_factor_all          0.1413
_refine_ls_R_factor_gt           0.0876
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.1289P)^2^+16.4444P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2261
_refine_ls_wR_factor_ref         0.2659
_reflns_number_gt                5061
_reflns_number_total             8556
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            om6b00349_si_002.cif
_cod_data_source_block           4a
_cod_depositor_comments
;
The following automatic conversions were performed:

data item '_symmetry_cell_setting' value 'Monoclinic' was changed to
'monoclinic' in accordance with the
/home/saulius/struct/COD-crude-data/automatic-downloads/DataCite-retrospective/ACS/depositions/lib/dictionaries/cif_core.dic
dictionary named 'cif_core.dic' version 2.4.2 last updated on
2011-04-26.

Automatic conversion script
Id: cif_fix_values 6909 2019-04-08 15:41:33Z antanas 
;
_cod_original_cell_volume        4840.1(17)
_cod_original_sg_symbol_H-M      P2(1)/n
_cod_database_code               4088724