Ferrocenecarboxylic anhydride: identification of a new polymorph.
Tazi, Mehdi; Roisnel, Thierry; Mongin, Florence; Erb, William; Acta crystallographica. Section C, Structural chemistry 73 (2017) 760–766; doi:10.1107/S205322961701124X

data_2311899
_publ_section_title
;
 Ferrocenecarboxylic anhydride: identification of a new polymorph.
;
_journal_coeditor_code           YF3122
_journal_issue                   'Pt 10'
_journal_name_full
'Acta crystallographica. Section C, Structural chemistry'
_journal_page_first              760
_journal_page_last               766
_journal_paper_doi               10.1107/S205322961701124X
_journal_volume                  73
_journal_year                    2017
_chemical_formula_iupac          '[Fe2 (C5 H5)2 (C12 H8 O3)]'
_chemical_formula_moiety         'C22 H18 Fe2 O3'
_chemical_formula_sum            'C22 H18 Fe2 O3'
_chemical_formula_weight         442.06
_chemical_name_systematic
;
Ferrocenecarboxylic anhydride
;
_space_group_crystal_system      monoclinic
_space_group_IT_number           9
_space_group_name_Hall           'C -2yc'
_space_group_name_H-M_alt        'C 1 c 1'
_atom_sites_solution_hydrogens   geom
_cell_angle_alpha                90
_cell_angle_beta                 91.997(3)
_cell_angle_gamma                90
_cell_formula_units_Z            12
_cell_length_a                   5.9758(5)
_cell_length_b                   36.456(3)
_cell_length_c                   24.363(2)
_cell_measurement_reflns_used    9522
_cell_measurement_temperature    150
_cell_measurement_theta_max      27.46
_cell_measurement_theta_min      2.23
_cell_volume                     5304.3(8)
_computing_cell_refinement
;
APEX2 (Bruker, 2014)
;
_computing_data_collection
;
APEX2 (Bruker, 2014)
;
_computing_data_reduction
;
APEX2 (Bruker, 2014)
;
_computing_molecular_graphics
;
SXGRAPH (Farrugia, 1999) and Mercury (Macrae <i>et al.</i>,
2008)
;
_computing_publication_material
;
CRYSCALC (T. Roisnel, local program)
;
_computing_structure_refinement
;
SHELXL2016 (Sheldrick, 2015b)
;
_computing_structure_solution
;
SHELXT (Sheldrick, 2015a)
;
_diffrn_ambient_temperature      150
_diffrn_measured_fraction_theta_full 0.994
_diffrn_measured_fraction_theta_max 0.992
_diffrn_measurement_device_type  'Bruker APEXII'
_diffrn_measurement_method       'CCD rotation images, thin slices'
_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  0.0234
_diffrn_reflns_limit_h_max       7
_diffrn_reflns_limit_h_min       -6
_diffrn_reflns_limit_k_max       41
_diffrn_reflns_limit_k_min       -46
_diffrn_reflns_limit_l_max       31
_diffrn_reflns_limit_l_min       -31
_diffrn_reflns_number            16323
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.485
_diffrn_reflns_theta_min         3.347
_exptl_absorpt_coefficient_mu    1.661
_exptl_absorpt_correction_T_max  0.608
_exptl_absorpt_correction_T_min  0.466
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
(SADABS; Sheldrick, 2014)
;
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    1.661
_exptl_crystal_description       prism
_exptl_crystal_F_000             2712
_exptl_crystal_size_max          0.560
_exptl_crystal_size_mid          0.360
_exptl_crystal_size_min          0.300
_refine_diff_density_max         0.968
_refine_diff_density_min         -0.863
_refine_ls_abs_structure_details
;
 Refined as an inversion twin.
;
_refine_ls_abs_structure_Flack   0.21(3)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.106
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     731
_refine_ls_number_reflns         10804
_refine_ls_number_restraints     32
_refine_ls_restrained_S_all      1.106
_refine_ls_R_factor_all          0.0509
_refine_ls_R_factor_gt           0.0490
_refine_ls_shift/su_max          0.004
_refine_ls_shift/su_mean         0.001
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0346P)^2^+44.5361P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1181
_refine_ls_wR_factor_ref         0.1189
_reflns_number_gt                10350
_reflns_number_total             10804
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            yf3122sup1.cif
_cod_data_source_block           I
_cod_original_cell_volume        5304.4(8)
_cod_original_sg_symbol_H-M      'C c'
_cod_database_code               2311899
_shelx_hkl_checksum              30032
_shelx_res_checksum              13098