#------------------------------------------------------------------------------
#$Date: 2017-05-05 08:49:52 +0300 (Fri, 05 May 2017) $
#$Revision: 196234 $
#$URL: file:///home/coder/svn-repositories/cod/cif/2/24/09/2240930.cif $
#------------------------------------------------------------------------------
#
# This file is available in the Crystallography Open Database (COD),
# http://www.crystallography.net/. The original data for this entry
# were provided by IUCr Journals, http://journals.iucr.org/.
#
# The file may be used within the scientific community so long as
# proper attribution is given to the journal article from which the
# data were obtained.
#
data_2240930
loop_
_publ_author_name
'Djomo, Edith Dimitri'
'Capet, Frédéric'
'Nenwa, Justin'
'Bélombé, Michel M.'
'Foulon, Michel'
_publ_section_title
;
 Crystal structure of 4-(dimethylamino)pyridinium
 cis-diaquabis(oxalato-κ²O,O')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
cis-diaquabis(oxalato-κ²O,O')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 et al.,  2009)
;
_computing_publication_material
;
OLEX2 (Dolomanov et al.,  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       'φ and ω 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/[σ²(Fo²)+(0.0528P)²+5.0524P] where P=(Fo²+2Fc²)/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 > 2σ(I)'
_cod_depositor_comments
;

2017-04-08
Z value and formula fixed to values more according to usual
chemical conventions.                 miguel
;
_cod_original_formula_sum            'C22 H32 Fe2 N4 O21'
_cod_original_formula_weight         800.22
_cod_original_formula_moiety         '2(C7 H11 N2 +), 2(C4 H4 Fe O10 -), H2 O '
_cod_original_formula_units_Z            4
_cod_data_source_file            vn2095sup1.cf
_cod_data_source_block           I
_cod_database_code               2240930
_shelx_space_group_comment
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x+1/2, y, -z'
'x+1/2, y+1/2, z+1/2'
'-x+1, y+1/2, -z+1/2'
'-x, -y, -z'
'x-1/2, -y, z'
'-x+1/2, -y+1/2, -z+1/2'
'x, -y+1/2, z+1/2'
loop_
_atom_site_type_symbol
_atom_site_label
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_calc_flag
_atom_site_occupancy
Fe Fe1 0.33846(2) 0.99760(3) 0.33390(2) 0.02994(10) Uani d 1
O O1 0.27198(13) 0.84143(16) 0.15711(7) 0.0393(4) Uani d 1
O O1W 0.31148(18) 1.14895(18) 0.38270(9) 0.0511(5) Uani d 1
H H1WA 0.287(3) 1.216(2) 0.3669(16) 0.077 Uiso d 1
H H1WB 0.321(3) 1.132(4) 0.4186(10) 0.077 Uiso d 1
O O2 0.23808(16) 1.10293(17) 0.14845(8) 0.0524(5) Uani d 1
O O2W 0.21255(12) 0.91604(16) 0.33264(9) 0.0381(4) Uani d 1
H H2WA 0.187(2) 0.941(3) 0.3590(13) 0.057 Uiso d 1
H H2WB 0.223(2) 0.8379(17) 0.3394(15) 0.057 Uiso d 1
O O3 0.33473(12) 0.86776(14) 0.26407(7) 0.0343(3) Uani d 1
O O4 0.29136(13) 1.10922(15) 0.25610(7) 0.0389(4) Uani d 1
O O5 0.39926(12) 0.89364(16) 0.41206(8) 0.0398(4) Uani d 1
O O6 0.47565(13) 1.04452(18) 0.34780(8) 0.0408(4) Uani d 1
O O7 0.53967(14) 0.85689(19) 0.48747(9) 0.0504(5) Uani d 1
O O8 0.62163(14) 1.0053(2) 0.41370(12) 0.0625(6) Uani d 1
C C1 0.29387(15) 0.9073(2) 0.20675(10) 0.0293(4) Uani d 1
C C2 0.27184(17) 1.0531(2) 0.20161(10) 0.0338(5) Uani d 1
C C3 0.49036(17) 0.9055(2) 0.43727(11) 0.0335(5) Uani d 1
C C4 0.53485(18) 0.9927(2) 0.39683(12) 0.0377(5) Uani d 1
N N1 0.34280(18) 0.5649(3) 0.47049(11) 0.0564(6) Uani d 1
H H1 0.3107 0.5735 0.4302 0.068 Uiso calc 1
N N2 0.49507(17) 0.5221(2) 0.66339(10) 0.0442(5) Uani d 1
C C5 0.44607(18) 0.5376(2) 0.60033(11) 0.0371(5) Uani d 1
C C6 0.4118(3) 0.4314(3) 0.55903(14) 0.0609(9) Uani d 1
H H6 0.4241 0.3488 0.5756 0.073 Uiso calc 1
C C7 0.3617(3) 0.4484(4) 0.49606(15) 0.0683(10) Uani d 1
H H7 0.3400 0.3771 0.4700 0.082 Uiso calc 1
C C8 0.3735(2) 0.6686(3) 0.50711(14) 0.0518(7) Uani d 1
H H8 0.3599 0.7493 0.4885 0.062 Uiso calc 1
C C9 0.42434(19) 0.6587(3) 0.57107(13) 0.0438(6) Uani d 1
H H9 0.4448 0.7324 0.5955 0.053 Uiso calc 1
C C10 0.5313(2) 0.6307(3) 0.70562(14) 0.0521(7) Uani d 1
H H10A 0.5788 0.6742 0.6919 0.078 Uiso calc 1
H H10B 0.5591 0.6011 0.7493 0.078 Uiso calc 1
H H10C 0.4801 0.6885 0.7036 0.078 Uiso calc 1
C C11 0.5175(3) 0.3955(3) 0.69141(16) 0.0704(10) Uani d 1
H H11A 0.4600 0.3467 0.6833 0.106 Uiso calc 1
H H11B 0.5480 0.4030 0.7372 0.106 Uiso calc 1
H H11C 0.5596 0.3530 0.6723 0.106 Uiso calc 1
O O3W 0.2500 0.1564(4) 0.5000 0.117(2) Uani d 1
H H3W 0.302(3) 0.115(5) 0.512(3) 0.176 Uiso d 1
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Fe Fe 0.3463 0.8444 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
O1W Fe1 O2W 90.16(8)
O1W Fe1 O3 163.51(8)
O1W Fe1 O6 95.03(9)
O3 Fe1 O2W 84.35(7)
O4 Fe1 O1W 85.14(7)
O4 Fe1 O2W 99.16(8)
O4 Fe1 O3 80.42(6)
O4 Fe1 O6 92.95(7)
O5 Fe1 O1W 95.09(8)
O5 Fe1 O2W 87.05(7)
O5 Fe1 O3 100.13(7)
O5 Fe1 O4 173.78(7)
O5 Fe1 O6 80.84(7)
O6 Fe1 O2W 167.19(7)
O6 Fe1 O3 93.64(7)
Fe1 O1W H1WA 126(3)
Fe1 O1W H1WB 110(3)
H1WA O1W H1WB 123(3)
Fe1 O2W H2WA 118(2)
Fe1 O2W H2WB 107(2)
H2WA O2W H2WB 107(3)
C1 O3 Fe1 114.30(13)
C2 O4 Fe1 116.08(14)
C3 O5 Fe1 116.33(14)
C4 O6 Fe1 114.72(15)
O1 C1 O3 126.2(2)
O1 C1 C2 119.43(19)
O3 C1 C2 114.39(17)
O2 C2 O4 126.3(2)
O2 C2 C1 119.91(19)
O4 C2 C1 113.77(18)
O5 C3 C4 112.84(19)
O7 C3 O5 126.3(2)
O7 C3 C4 120.9(2)
O6 C4 C3 115.1(2)
O8 C4 O6 125.9(2)
O8 C4 C3 119.0(2)
C7 N1 H1 119.9
C7 N1 C8 120.2(2)
C8 N1 H1 119.9
C5 N2 C10 121.7(2)
C5 N2 C11 121.2(2)
C11 N2 C10 117.1(2)
N2 C5 C6 121.6(2)
N2 C5 C9 122.9(2)
C9 C5 C6 115.5(2)
C5 C6 H6 119.5
C7 C6 C5 121.0(3)
C7 C6 H6 119.5
N1 C7 C6 121.4(3)
N1 C7 H7 119.3
C6 C7 H7 119.3
N1 C8 H8 119.2
N1 C8 C9 121.5(3)
C9 C8 H8 119.2
C5 C9 H9 119.8
C8 C9 C5 120.3(3)
C8 C9 H9 119.8
N2 C10 H10A 109.5
N2 C10 H10B 109.5
N2 C10 H10C 109.5
H10A C10 H10B 109.5
H10A C10 H10C 109.5
H10B C10 H10C 109.5
N2 C11 H11A 109.5
N2 C11 H11B 109.5
N2 C11 H11C 109.5
H11A C11 H11B 109.5
H11A C11 H11C 109.5
H11B C11 H11C 109.5
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
Fe1 O1W 2.0133(18)
Fe1 O2W 2.0407(18)
Fe1 O3 2.0250(15)
Fe1 O4 1.9927(16)
Fe1 O5 1.9799(16)
Fe1 O6 2.0163(18)
O1 C1 1.235(3)
O1W H1WA 0.809(17)
O1W H1WB 0.771(17)
O2 C2 1.223(3)
O2W H2WA 0.824(17)
O2W H2WB 0.834(17)
O3 C1 1.272(3)
O4 C2 1.272(3)
O5 C3 1.291(3)
O6 C4 1.269(3)
O7 C3 1.218(3)
O8 C4 1.226(3)
C1 C2 1.554(3)
C3 C4 1.550(3)
N1 H1 0.8600
N1 C7 1.330(5)
N1 C8 1.337(4)
N2 C5 1.345(3)
N2 C10 1.452(3)
N2 C11 1.450(4)
C5 C6 1.417(4)
C5 C9 1.407(3)
C6 H6 0.9300
C6 C7 1.349(4)
C7 H7 0.9300
C8 H8 0.9300
C8 C9 1.363(4)
C9 H9 0.9300
C10 H10A 0.9600
C10 H10B 0.9600
C10 H10C 0.9600
C11 H11A 0.9600
C11 H11B 0.9600
C11 H11C 0.9600
O3W H3W 0.842(19)
loop_
_geom_hbond_atom_site_label_D
_geom_hbond_atom_site_label_H
_geom_hbond_atom_site_label_A
_geom_hbond_site_symmetry_A
_geom_hbond_distance_DH
_geom_hbond_distance_HA
_geom_hbond_distance_DA
_geom_hbond_angle_DHA
O1W H1WA O2 7_575 0.809(17) 1.94(2) 2.720(3) 162(4)
O1W H1WB O7 5_676 0.771(17) 2.40(3) 2.988(3) 134(4)
O1W H1WB O3W 1_565 0.771(17) 2.34(3) 2.9699(19) 139(4)
O2W H2WA O8 6_575 0.824(17) 1.841(18) 2.664(3) 176(3)
O2W H2WB O1 7_565 0.834(17) 1.875(18) 2.702(2) 171(3)
N1 H1 O1 7_565 0.86 2.11 2.931(3) 160.3
N1 H1 O2 7_565 0.86 2.46 3.043(3) 125.3
O3W H3W O7 5_666 0.842(19) 2.36(5) 3.040(2) 138(6)
O3W H3W O8 5_666 0.842(19) 2.09(5) 2.782(3) 140(6)
loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
Fe1 O3 C1 O1 -170.06(19)
Fe1 O3 C1 C2 10.4(2)
Fe1 O4 C2 O2 176.4(2)
Fe1 O4 C2 C1 -3.0(3)
Fe1 O5 C3 O7 174.7(2)
Fe1 O5 C3 C4 -4.7(3)
Fe1 O6 C4 O8 178.3(2)
Fe1 O6 C4 C3 -1.1(3)
O1 C1 C2 O2 -4.1(4)
O1 C1 C2 O4 175.3(2)
O3 C1 C2 O2 175.4(2)
O3 C1 C2 O4 -5.2(3)
O5 C3 C4 O6 3.8(3)
O5 C3 C4 O8 -175.6(2)
O7 C3 C4 O6 -175.6(2)
O7 C3 C4 O8 5.0(4)
N1 C8 C9 C5 0.1(4)
N2 C5 C6 C7 179.1(3)
N2 C5 C9 C8 -179.2(3)
C5 C6 C7 N1 0.1(6)
C6 C5 C9 C8 0.0(4)
C7 N1 C8 C9 -0.2(5)
C8 N1 C7 C6 0.1(5)
C9 C5 C6 C7 -0.2(5)
C10 N2 C5 C6 179.2(3)
C10 N2 C5 C9 -1.6(4)
C11 N2 C5 C6 1.9(5)
C11 N2 C5 C9 -178.8(3)

_cod_database_fobs_code 2240930
