Dicarbonyl[η^4^-(<i>E</i>)-(2,6,6-trimethylcyclohepta-2,4-dienylidene)ethyl acetate](triphenylphosphine)iron
Petrowitsch, Tanja; Schürmann, Markus; Preut, Hans; Eilbracht, Peter; Acta Crystallographica Section C 53 (1997) IUC9700023–; doi:10.1107/S0108270197099356

data_2006719
_publ_section_title
;
 Dicarbonyl[\h^4^-(<i>E</i>)-(2,6,6-trimethylcyclohepta-2,4-dienylidene)ethyl
 acetate](triphenylphosphine)iron
;
_journal_issue                   11
_journal_name_full               'Acta Crystallographica Section C'
_journal_page_first              IUC9700023
_journal_paper_doi               10.1107/S0108270197099356
_journal_volume                  53
_journal_year                    1997
_chemical_formula_iupac          '[Fe (C O)2 (C14 H20 O2) (C18 H15 P)]'
_chemical_formula_sum            'C34 H35 Fe O4 P'
_chemical_formula_weight         594.47
_chemical_name_systematic
;
Dicarbonyl[\h^4^-((E)-(2,6,6-Trimethyl-cyclohepta-2,4-dienylidene)-ethyl
acetat)]triphenylphosphine-iron
;
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_audit_creation_method           SHELXL
_cell_angle_alpha                114.5590(10)
_cell_angle_beta                 95.9190(10)
_cell_angle_gamma                95.2490(10)
_cell_formula_units_Z            2
_cell_length_a                   9.4810(10)
_cell_length_b                   12.5920(10)
_cell_length_c                   14.3220(10)
_cell_measurement_reflns_used    9734
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      24.67
_cell_measurement_theta_min      4.43
_cell_volume                     1529.7(2)
_computing_cell_refinement
'DENZO and SCALEPACK (Otwinowski & Minor, 1997)'
_computing_data_collection       'Nonius KappaCCD'
_computing_data_reduction
'DENZO and SCALEPACK (Otwinowski & Minor, 1997)'
_computing_publication_material
'SHELXL-93 (Sheldrick, 1993), PARST95 (Nardelli, 1995)'
_computing_structure_refinement  'SHELXL-93 (Sheldrick, 1993)'
_computing_structure_solution    'SHELXS-86 (Sheldrick, 1990)'
_diffrn_ambient_temperature      293(2)
_diffrn_detector_area_resol_mean '19 vertical, 18 horizontal'
_diffrn_measurement_device_type  'Nonius KappaCCD'
_diffrn_measurement_method
'360 frames via \w-rotation (\D\w=1\%) and two times 10s per frame'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71069
_diffrn_reflns_av_R_equivalents  0.0460
_diffrn_reflns_av_sigmaI/netI    0.0843
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_number            9734
_diffrn_reflns_theta_max         24.67
_diffrn_reflns_theta_min         4.43
_diffrn_standards_decay_%        0
_diffrn_standards_number         none
_exptl_absorpt_coefficient_mu    0.581
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            orange
_exptl_crystal_density_diffrn    1.291
_exptl_crystal_density_meas      ?
_exptl_crystal_description       plate
_exptl_crystal_F_000             624
_exptl_crystal_size_max          0.8
_exptl_crystal_size_mid          0.25
_exptl_crystal_size_min          0.2
_refine_diff_density_max         0.458
_refine_diff_density_min         -0.298
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_all   0.740
_refine_ls_goodness_of_fit_obs   0.824
_refine_ls_hydrogen_treatment    refall
_refine_ls_matrix_type           full
_refine_ls_number_parameters     482
_refine_ls_number_reflns         4867
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.740
_refine_ls_restrained_S_obs      0.824
_refine_ls_R_factor_all          0.0870
_refine_ls_R_factor_obs          .0389
_refine_ls_shift/esd_max         0.012
_refine_ls_shift/esd_mean        0.002
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0806P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.1088
_refine_ls_wR_factor_obs         .0906
_reflns_number_gt                2915
_reflns_number_total             4867
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            qa0015.cif
_cod_data_source_block           ccd181
_cod_depositor_comments
;
The following automatic conversions were performed:
'_geom_bond_publ_flag' value 'Yes' changed to 'yes' according to
'/home/saulius/struct/CIF-dictionaries/cif_core.dic' dictionary named
'cif_core.dic' version 2.4.1 from 2010-06-29 (27 times).

Automatic conversion script
Id: cif_fix_enum 1527 2010-12-29 10:47:43Z saulius 

The following automatic conversions were performed:

'_exptl_crystal_density_meas' value 'not determined' was changed to
'?' - the value is perceived as not measured.

Automatic conversion script
Id: cif_fix_values 3008 2015-01-20 13:52:24Z robertas 

The following automatic conversions were performed:

'_refine_ls_weighting_scheme' value 'calc
w=1/[\s^2^(Fo^2^)+(0.0806P)^2^] 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^)+(0.0806P)^2^]
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_database_code               2006719