Crystal structure of 4-(dimethylamino)pyridinium <i>cis</i>-diaquabis(oxalato-κ^2^<i>O</i>,<i>O</i>')ferrate(III) hemihydrate
Djomo, Edith Dimitri; Capet, Frédéric; Nenwa, Justin; Bélombé, Michel M.; Foulon, Michel; Acta Crystallographica Section E 71 (2015) 934–936; doi:10.1107/S2056989015013213

data_2240930
_publ_section_title
;
 Crystal structure of 4-(dimethylamino)pyridinium
 <i>cis</i>-diaquabis(oxalato-\k^2^<i>O</i>,<i>O</i>')ferrate(III)
 hemihydrate
;
_journal_coeditor_code           VN2095
_journal_issue                   8
_journal_name_full               'Acta Crystallographica Section E'
_journal_page_first              934
_journal_page_last               936
_journal_paper_doi               10.1107/S2056989015013213
_journal_volume                  71
_journal_year                    2015
_chemical_formula_iupac          '(C7 H11 N2) [Fe (C2 O4)2 (H2 O)2], 0.5H2 O'
_chemical_formula_moiety         'C7 H11 N2 +, C4 H4 Fe O10 -, 0.5(H2 O) '
_chemical_formula_sum            'C11 H16 Fe N2 O10.5'
_chemical_formula_weight         400.11
_chemical_name_systematic
;
4-(Dimethylamino)pyridinium
<i>cis</i>-diaquabis(oxalato-\k^2^<i>O</i>,<i>O</i>')ferrate(III)
hemihydrate
;
_space_group_crystal_system      monoclinic
_space_group_IT_number           15
_space_group_name_Hall           '-I 2ya'
_space_group_name_H-M_alt        'I 1 2/a 1'
_symmetry_space_group_name_Hall  '-I 2ya'
_symmetry_space_group_name_H-M   'I 1 2/a 1'
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method
;
Olex2 1.2
(compiled 2015.01.19 svn.r3143 for OlexSys, GUI svn.r4992)
;
_cell_angle_alpha                90
_cell_angle_beta                 108.352(3)
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   14.7960(7)
_cell_length_b                   10.4422(4)
_cell_length_c                   21.7751(10)
_cell_measurement_reflns_used    9923
_cell_measurement_temperature    296(2)
_cell_measurement_theta_max      27.34
_cell_measurement_theta_min      2.19
_cell_volume                     3193.2(2)
_computing_cell_refinement
;
SAINT (Bruker, 2014)
;
_computing_data_collection
;
APEX2 (Bruker, 2014)
;
_computing_data_reduction
;
SAINT (Bruker, 2014)
;
_computing_molecular_graphics
;
OLEX2 (Dolomanov <i>et al.</i>,  2009)
;
_computing_publication_material
;
OLEX2 (Dolomanov <i>et al.</i>,  2009), publCIF (Westrip, 2010)
and
PLATON (Spek, 2009)
;
_computing_structure_refinement
;
SHELXL2014 (Sheldrick, 2015)
;
_computing_structure_solution
;
SHELXS97 (Sheldrick, 2008)
;
_diffrn_ambient_temperature      296.15
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.996
_diffrn_measurement_device_type  'Bruker APEXII CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0443
_diffrn_reflns_limit_h_max       21
_diffrn_reflns_limit_h_min       -21
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       31
_diffrn_reflns_limit_l_min       -31
_diffrn_reflns_number            48070
_diffrn_reflns_theta_full        26.000
_diffrn_reflns_theta_max         30.549
_diffrn_reflns_theta_min         2.827
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    1.004
_exptl_absorpt_correction_T_max  0.7461
_exptl_absorpt_correction_T_min  0.6785
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
(SADABS2014; Bruker, 2014)
;
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.665
_exptl_crystal_description       irregular
_exptl_crystal_F_000             1648
_exptl_crystal_size_max          0.26
_exptl_crystal_size_mid          0.22
_exptl_crystal_size_min          0.13
_refine_diff_density_max         0.851
_refine_diff_density_min         -0.576
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.055
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     239
_refine_ls_number_reflns         4880
_refine_ls_number_restraints     8
_refine_ls_restrained_S_all      1.164
_refine_ls_R_factor_all          0.0669
_refine_ls_R_factor_gt           0.0422
_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^)+(0.0528P)^2^+5.0524P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1077
_refine_ls_wR_factor_ref         0.1230
_reflns_number_gt                3435
_reflns_number_total             4880
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            vn2095sup1.cf
_cod_data_source_block           I
_cod_depositor_comments
;

2017-04-08
Z value and formula fixed to values more according to usual
chemical conventions.                 miguel
;
_cod_original_formula_moiety     '2(C7 H11 N2 +), 2(C4 H4 Fe O10 -), H2 O '
_cod_original_formula_sum        'C22 H32 Fe2 N4 O21'
_cod_original_formula_units_Z    4
_cod_original_formula_weight     800.22
_cod_database_code               2240930
_cod_database_fobs_code          2240930