A new polymorph of a carbonyliron complex from tetraphenylhexapentaene: bis(μ~3~,η^2^,σ^2^-diphenylallenylidene)octacarbonyltriiron
Zachara, Janusz; Zimniak, Andrzej; Acta Crystallographica Section C 55 (1999) 58–60; doi:10.1107/S010827019801107X

data_2008087
_publ_section_title
;
 A new polymorph of a carbonyliron complex from
 tetraphenylhexapentaene:
 bis(\m~3~,\h^2^,\s^2^-diphenylallenylidene)octacarbonyltriiron
;
_journal_issue                   1
_journal_name_full               'Acta Crystallographica Section C'
_journal_page_first              58
_journal_page_last               60
_journal_paper_doi               10.1107/S010827019801107X
_journal_volume                  55
_journal_year                    1999
_chemical_formula_iupac          '[Fe3 (C15 H10)2 (CO)8]'
_chemical_formula_moiety         'C38 H20 Fe3 O8'
_chemical_formula_structural     'Fe3 (C15 H10)2 (CO)8'
_chemical_formula_sum            'C38 H20 Fe3 O8'
_chemical_formula_weight         772.09
_chemical_melting_point          444
_chemical_name_systematic
;
octacarbonyl-1\k^3^C,2\k^3^C,3\k^2^C-bis(\m~3~-3,3-diphenylallenylidene
-1:2\k^2^C^1^:3(1,2-\h^2^))-triangulo-triiron(0)(3 Fe--Fe)
;
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/c 1'
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 99.313(13)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   17.174(3)
_cell_length_b                   8.9483(16)
_cell_length_c                   22.132(4)
_cell_measurement_reflns_used    25
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      17.30
_cell_measurement_theta_min      7.75
_cell_volume                     3356.4(10)
_computing_cell_refinement       'P3/P4-PC Diffractometer Program'
_computing_data_collection
'P3/P4-PC Diffractometer Program (Siemens, 1991a)'
_computing_data_reduction        'XDISK (Siemens, 1991b)'
_computing_molecular_graphics    'ORTEPIII (Burnett & Johnson, 1996)'
_computing_publication_material  'SHELXL97 and PARST96 (Nardelli, 1995)'
_computing_structure_refinement  'SHELXL97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS86 (Sheldrick, 1990)'
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 0.980
_diffrn_measured_fraction_theta_max 0.980
_diffrn_measurement_device       'Siemens P3'
_diffrn_measurement_method       'profile data from \w--2\q'
_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  0.022
_diffrn_reflns_av_sigmaI/netI    0.0186
_diffrn_reflns_limit_h_max       20
_diffrn_reflns_limit_h_min       0
_diffrn_reflns_limit_k_max       10
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       26
_diffrn_reflns_limit_l_min       -26
_diffrn_reflns_number            6040
_diffrn_reflns_theta_full        25.0
_diffrn_reflns_theta_max         25.0
_diffrn_reflns_theta_min         2.0
_diffrn_standards_decay_%        0.0
_diffrn_standards_interval_count 70
_diffrn_standards_number         2
_exptl_absorpt_coefficient_mu    1.332
_exptl_absorpt_correction_T_max  0.819
_exptl_absorpt_correction_T_min  0.633
_exptl_absorpt_correction_type   '\y scan'
_exptl_absorpt_process_details
;
 Ellipsoid correction - XEMP (Siemens, 1990)
;
_exptl_crystal_colour            'dark red'
_exptl_crystal_density_diffrn    1.528
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prismatic
_exptl_crystal_F_000             1560
_exptl_crystal_size_max          0.30
_exptl_crystal_size_mid          0.25
_exptl_crystal_size_min          0.15
_refine_diff_density_max         0.255
_refine_diff_density_min         -0.233
_refine_ls_extinction_coef       0.0077(3)
_refine_ls_extinction_method     SHELXL97
_refine_ls_goodness_of_fit_all   1.033
_refine_ls_goodness_of_fit_ref   1.033
_refine_ls_hydrogen_treatment    refU
_refine_ls_matrix_type           full
_refine_ls_number_parameters     463
_refine_ls_number_reflns         5841
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.033
_refine_ls_R_factor_all          0.037
_refine_ls_R_factor_gt           0.029
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w = 1/[\s^2^(F~o~^2^)+(0.0412P)^2^+0.9826P] where P=(F~o~^2^+2F~c~^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.074
_refine_ls_wR_factor_obs         0.071
_refine_ls_wR_factor_ref         0.074
_reflns_number_gt                4932
_reflns_number_total             5841
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            jz1302.cif
_cod_data_source_block           4aza
_cod_original_sg_symbol_H-M      'P 21/c'
_cod_database_code               2008087
_cod_database_fobs_code          2008087