Adducts of hexamethylenetetramine with ferrocenecarboxylic acid and ferrocene-1,1'-dicarboxylic acid: multiple disorder in space groups <i>Fmm</i>2 and <i>Cmcm</i>
Zakaria, Choudhury M.; Ferguson, George; Lough, Alan J.; Glidewell, Christopher; Acta Crystallographica Section C 59 (2003) m271–m274; doi:10.1107/S010827010301031X

data_2013502
_publ_section_title
;
 Adducts of hexamethylenetetramine with ferrocenecarboxylic acid and
 ferrocene-1,1'-dicarboxylic acid: multiple disorder in space groups
 <i>Fmm</i>2 and <i>Cmcm</i>
;
_journal_issue                   7
_journal_name_full               'Acta Crystallographica Section C'
_journal_page_first              m271
_journal_page_last               m274
_journal_paper_doi               10.1107/S010827010301031X
_journal_volume                  59
_journal_year                    2003
_chemical_formula_iupac          '(C6 H14 N4) [Fe (C5 H5) (C6 H4 O2)]2'
_chemical_formula_moiety         'C6 H14 N4 2+, 2C11 H9 Fe O2 1-'
_chemical_formula_sum            'C28 H32 Fe2 N4 O4'
_chemical_formula_weight         600.28
_chemical_name_systematic
;
Hexamethylenetetramine--ferrocenecarboxylic acid (1/2)
;
_space_group_IT_number           42
_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_Hall  'F 2 -2'
_symmetry_space_group_name_H-M   'F m m 2'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   9.9496(8)
_cell_length_b                   36.295(3)
_cell_length_c                   7.0643(6)
_cell_measurement_reflns_used    1351
_cell_measurement_temperature    150.0(10)
_cell_measurement_theta_max      27.40
_cell_measurement_theta_min      2.55
_cell_volume                     2551.1(4)
_computing_cell_refinement       'DENZO-SMN (Otwinowski & Minor, 1997)'
_computing_data_collection       'KappaCCD Server Software (Nonius, 1997)'
_computing_data_reduction        DENZO-SMN
_computing_molecular_graphics    'PLATON (Spek, 2003)'
_computing_publication_material  'SHELXL97 and PRPKAPPA (Ferguson, 1999)'
_computing_structure_refinement  'SHELXL97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS97 (Sheldrick, 1997)'
_diffrn_ambient_temperature      150.0(10)
_diffrn_measured_fraction_theta_full 0.990
_diffrn_measured_fraction_theta_max 0.970
_diffrn_measurement_device_type  'Nonius KappaCCD'
_diffrn_measurement_method       '\f scans, and \w scans with \k offsets'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed X-ray tube'
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.055
_diffrn_reflns_av_sigmaI/netI    0.0880
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       45
_diffrn_reflns_limit_k_min       -46
_diffrn_reflns_limit_l_max       8
_diffrn_reflns_limit_l_min       -8
_diffrn_reflns_number            2539
_diffrn_reflns_theta_full        27.00
_diffrn_reflns_theta_max         27.40
_diffrn_reflns_theta_min         2.55
_diffrn_standards_decay_%        0
_exptl_absorpt_coefficient_mu    1.181
_exptl_absorpt_correction_T_max  0.775
_exptl_absorpt_correction_T_min  0.709
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   '(DENZO-SMN; Otwinowski & Minor, 1997)'
_exptl_crystal_colour            orange
_exptl_crystal_density_diffrn    1.563
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             1248
_exptl_crystal_size_max          0.28
_exptl_crystal_size_mid          0.26
_exptl_crystal_size_min          0.22
_refine_diff_density_max         0.395
_refine_diff_density_min         -0.319
_refine_ls_abs_structure_details 'Flack (1983), 507 Friedel pairs'
_refine_ls_abs_structure_Flack   0.33(4)
_refine_ls_extinction_coef       0.0031(6)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     SHELXL97
_refine_ls_goodness_of_fit_ref   1.063
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     129
_refine_ls_number_reflns         1351
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.063
_refine_ls_R_factor_all          0.0540
_refine_ls_R_factor_gt           0.0442
_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^)^2^+2.01P] where P = (Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0948
_refine_ls_wR_factor_ref         0.0994
_reflns_number_gt                1197
_reflns_number_total             1351
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            sk1641.cif
_cod_data_source_block           I
_cod_database_code               2013502
_cod_database_fobs_code          2013502