Ferrocenecarboxylic anhydride: a redetermination
McAdam, C. John; Simpson, Jim; IUCrData 1 (2016) x161769–; doi:10.1107/S2414314616017697

data_1544543
_publ_section_title
;
 Ferrocenecarboxylic anhydride: a redetermination
;
_journal_coeditor_code           HB4093
_journal_issue                   11
_journal_name_full               IUCrData
_journal_page_first              x161769
_journal_paper_doi               10.1107/S2414314616017697
_journal_volume                  1
_journal_year                    2016
_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      orthorhombic
_space_group_IT_number           61
_space_group_name_Hall           '-P 2ac 2ab'
_space_group_name_H-M_alt        'P b c a'
_symmetry_space_group_name_Hall  '-P 2ac 2ab'
_symmetry_space_group_name_H-M   'P b c a'
_atom_sites_solution_hydrogens   geom
_audit_creation_method           SHELXL-2014/7
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   14.8773(2)
_cell_length_b                   12.2499(2)
_cell_length_c                   19.3288(3)
_cell_measurement_reflns_used    7707
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      73.5310
_cell_measurement_theta_min      4.5690
_cell_volume                     3522.59(9)
_computing_cell_refinement
;
CrysAlis PRO (Agilent, 2014)
;
_computing_data_collection
;
CrysAlis PRO (Agilent, 2014)
;
_computing_data_reduction
;
CrysAlis PRO (Agilent, 2014)
;
_computing_molecular_graphics
;
Mercury (Macrae <i>et al.</i>, 2008)
;
_computing_publication_material
;
SHELXL2014 (Sheldrick, 2015), enCIFer (Allen <i>et al.</i>,
2004),
PLATON (Spek, 2009), publCIF (Westrip, 2010) and WinGX
(Farrugia, 2012)
;
_computing_structure_refinement
;
SHELXL2014 (Sheldrick, 2015) and <i>TITAN2000</i> (Hunter & Simpson,
1999)
;
_computing_structure_solution
;
SHELXS2013 (Sheldrick, 2008)
;
_diffrn_ambient_temperature      100(2)
_diffrn_detector_area_resol_mean 5.1725
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.980
_diffrn_measurement_device_type  'Agilent SuperNova, Dual, Cu at zero, Atlas'
_diffrn_measurement_method       '\w scans'
_diffrn_radiation_source         'SuperNova (Cu) X-ray Source'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0396
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       8
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            13584
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         73.292
_diffrn_reflns_theta_min         4.575
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    13.377
_exptl_absorpt_correction_T_max  0.456
_exptl_absorpt_correction_T_min  0.267
_exptl_absorpt_correction_type   gaussian
_exptl_absorpt_process_details
;
(CrysAlis PRO; Agilent, 2014)
;
_exptl_crystal_colour            orange
_exptl_crystal_density_diffrn    1.667
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             1808
_exptl_crystal_size_max          0.16
_exptl_crystal_size_mid          0.13
_exptl_crystal_size_min          0.11
_refine_diff_density_max         0.312
_refine_diff_density_min         -0.681
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.843
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     244
_refine_ls_number_reflns         3468
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.843
_refine_ls_R_factor_all          0.0313
_refine_ls_R_factor_gt           0.0295
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0890P)^2^+0.2107P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0879
_refine_ls_wR_factor_ref         0.0904
_reflns_number_gt                3262
_reflns_number_total             3468
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            hb4093sup1.cif
_cod_data_source_block           I
_cod_database_code               1544543
_shelx_estimated_absorpt_t_min   0.223
_shelx_estimated_absorpt_t_max   0.321
_shelx_hkl_checksum              54425
_shelx_res_checksum              78506
_cod_database_fobs_code 1544543