#------------------------------------------------------------------------------
#$Date: 2016-02-20 00:18:51 +0200 (Sat, 20 Feb 2016) $
#$Revision: 176760 $
#$URL: svn://www.crystallography.net/cod/cif/2/01/81/2018143.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_2018143
loop_
_publ_author_name
'Krawczyk, Monika K.'
'Lis, Tadeusz'
_publ_section_title
;
 New coordination modes in potassium edta salts:
 K₂[H₂edta]·2H₂O, K₃[Hedta]·2H₂O and
 K₄[edta]·3.92H₂O
;
_journal_coeditor_code           GD3395
_journal_issue                   7
_journal_name_full               'Acta Crystallographica Section C'
_journal_page_first              m266
_journal_page_last               m274
_journal_paper_doi               10.1107/S010827011102244X
_journal_volume                  67
_journal_year                    2011
_chemical_formula_iupac          '3K +, C10 H13 N2 O8 3-, 2H2 O'
_chemical_formula_moiety         '3(K +), C10 H13 N2 O8 3-, 2(H2 O)'
_chemical_formula_sum            'C10 H17 K3 N2 O10'
_chemical_formula_weight         442.56
_chemical_name_common
'tripotassium ethylenediaminetetraacetate dihydrate'
_chemical_name_systematic
;
tripotassium
2-({2-[bis(carboxylatomethyl)amino]ethyl}(carboxylatomethyl)azaniumyl)acetate
dihydrate
;
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                101.68(3)
_cell_angle_beta                 102.19(3)
_cell_angle_gamma                96.85(3)
_cell_formula_units_Z            2
_cell_length_a                   8.074(3)
_cell_length_b                   9.987(3)
_cell_length_c                   11.045(3)
_cell_measurement_reflns_used    15331
_cell_measurement_temperature    110(2)
_cell_measurement_theta_max      38.52
_cell_measurement_theta_min      4.58
_cell_volume                     840.2(5)
_computing_cell_refinement       'CrysAlis RED (Oxford Diffraction, 2008)'
_computing_data_collection       'CrysAlis CCD (Oxford Diffraction, 2008)'
_computing_data_reduction        'CrysAlis RED (Oxford Diffraction, 2008)'
_computing_molecular_graphics    'XP in SHELXTL (Bruker, 1997)'
_computing_publication_material
'SHELXL97 (Sheldrick, 2008) and publCIF (Westrip, 2010)'
_computing_structure_refinement  'SHELXL97 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      110(2)
_diffrn_measured_fraction_theta_full 0.995
_diffrn_measured_fraction_theta_max 0.950
_diffrn_measurement_device_type  'Oxford Diffraction Xcalibur PX KM-4-CCD'
_diffrn_measurement_method       'φ and ω'
_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  0.0221
_diffrn_reflns_av_sigmaI/netI    0.0311
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            24301
_diffrn_reflns_theta_full        27.00
_diffrn_reflns_theta_max         38.52
_diffrn_reflns_theta_min         4.58
_exptl_absorpt_coefficient_mu    0.866
_exptl_absorpt_correction_T_max  0.886
_exptl_absorpt_correction_T_min  0.808
_exptl_absorpt_correction_type   analytical
_exptl_absorpt_process_details
;
(CrysAlis RED; Oxford Diffraction, 2008)
;
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.749
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             456
_exptl_crystal_size_max          0.27
_exptl_crystal_size_mid          0.19
_exptl_crystal_size_min          0.19
_refine_diff_density_max         0.44
_refine_diff_density_min         -0.34
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.008
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     226
_refine_ls_number_reflns         9029
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.008
_refine_ls_R_factor_all          0.0351
_refine_ls_R_factor_gt           0.0242
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[σ²(Fo²)+(0.0360P)²+0.0000P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0628
_refine_ls_wR_factor_ref         0.0647
_reflns_number_gt                7083
_reflns_number_total             9029
_reflns_threshold_expression     I>2σ(I)
_cod_data_source_file            gd3395.cif
_cod_data_source_block           II
_cod_database_code               2018143
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, -y, -z'
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_refinement_flags
_atom_site_occupancy
_atom_site_symmetry_multiplicity
_atom_site_disorder_assembly
_atom_site_disorder_group
K K1 0.29419(2) 0.897638(16) 0.399042(15) 0.01204(3) Uani d . 1 1 . .
K K2 0.44262(2) 0.858824(16) 0.776214(15) 0.01304(3) Uani d . 1 1 . .
K K3 0.04772(2) 1.175392(17) 0.197522(16) 0.01501(4) Uani d . 1 1 . .
O O11 0.19850(8) 0.62235(6) 0.37444(5) 0.01568(11) Uani d . 1 1 . .
O O12 -0.00447(8) 0.45612(6) 0.23735(6) 0.01919(12) Uani d . 1 1 . .
O O21 0.24837(8) 0.93201(6) 0.16198(5) 0.01876(12) Uani d . 1 1 . .
O O22 0.27947(7) 0.91022(6) -0.03641(5) 0.01477(10) Uani d . 1 1 . .
O O31 0.63291(7) 0.68285(6) 0.67029(5) 0.01262(10) Uani d . 1 1 . .
O O32 0.56755(7) 0.83383(5) 0.55001(5) 0.01175(9) Uani d . 1 1 . .
O O41 0.98013(7) 0.97410(6) 0.32934(6) 0.01934(12) Uani d . 1 1 . .
O O42 0.69826(7) 0.95450(6) 0.32534(6) 0.01763(11) Uani d . 1 1 . .
N N1 0.34185(8) 0.66795(6) 0.16978(6) 0.01018(10) Uani d . 1 1 . .
N N2 0.67292(8) 0.69855(6) 0.35625(6) 0.00924(10) Uani d . 1 1 . .
H H2 0.5962 0.7610 0.3542 0.011 Uiso calc R 1 1 . .
C C1 0.44530(9) 0.55601(7) 0.17190(7) 0.01126(12) Uani d . 1 1 . .
H H1A 0.4254 0.4986 0.0842 0.014 Uiso calc R 1 1 . .
H H1B 0.4062 0.4957 0.2249 0.014 Uiso calc R 1 1 . .
C C2 0.63588(9) 0.60959(8) 0.22374(7) 0.01151(12) Uani d . 1 1 . .
H H2A 0.6984 0.5302 0.2243 0.014 Uiso calc R 1 1 . .
H H2B 0.6775 0.6643 0.1675 0.014 Uiso calc R 1 1 . .
C C11 0.11830(9) 0.55599(8) 0.26489(7) 0.01243(12) Uani d . 1 1 . .
C C12 0.16162(9) 0.60412(8) 0.15001(7) 0.01358(13) Uani d . 1 1 . .
H H12A 0.1336 0.5232 0.0762 0.016 Uiso calc R 1 1 . .
H H12B 0.0872 0.6719 0.1280 0.016 Uiso calc R 1 1 . .
C C21 0.28766(9) 0.86909(8) 0.06529(7) 0.01100(12) Uani d . 1 1 . .
C C22 0.35924(10) 0.73331(8) 0.06427(7) 0.01230(12) Uani d . 1 1 . .
H H22A 0.3004 0.6660 -0.0168 0.015 Uiso calc R 1 1 . .
H H22B 0.4828 0.7519 0.0652 0.015 Uiso calc R 1 1 . .
C C31 0.61234(9) 0.72172(7) 0.56826(6) 0.00932(11) Uani d . 1 1 . .
C C32 0.64230(10) 0.62151(7) 0.45385(7) 0.01175(12) Uani d . 1 1 . .
H H32A 0.7430 0.5777 0.4814 0.014 Uiso calc R 1 1 . .
H H32B 0.5406 0.5474 0.4169 0.014 Uiso calc R 1 1 . .
C C41 0.84165(10) 0.91617(8) 0.34322(7) 0.01214(12) Uani d . 1 1 . .
C C42 0.84879(9) 0.78345(7) 0.39235(7) 0.01150(12) Uani d . 1 1 . .
H H42A 0.9284 0.7294 0.3550 0.014 Uiso calc R 1 1 . .
H H42B 0.8921 0.8077 0.4862 0.014 Uiso calc R 1 1 . .
O O2W 0.15351(9) 0.68563(6) 0.62234(6) 0.02288(13) Uani d . 1 1 . .
H H21W 0.1025 0.6215 0.6490 0.034 Uiso d R 1 1 . .
H H22W 0.1484 0.6523 0.5435 0.034 Uiso d R 1 1 . .
O O3W 0.15902(9) 1.16026(7) -0.02942(6) 0.02384(13) Uani d . 1 1 . .
H H31W 0.2025 1.0854 -0.0317 0.036 Uiso d R 1 1 . .
H H32W 0.0774 1.1427 -0.0973 0.036 Uiso d R 1 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'
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'
K K 0.2009 0.2494 '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_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle
_geom_angle_publ_flag
O21 K1 O32 . 2_676 80.71(4) ?
O21 K1 O32 . . 130.07(3) ?
O32 K1 O32 2_676 . 93.30(4) ?
O21 K1 O11 . . 105.46(4) ?
O32 K1 O11 2_676 . 171.021(19) ?
O32 K1 O11 . . 77.74(4) ?
O21 K1 O41 . 1_455 71.18(3) ?
O32 K1 O41 2_676 1_455 87.59(4) ?
O32 K1 O41 . 1_455 158.60(2) ?
O11 K1 O41 . 1_455 100.50(4) ?
O21 K1 O42 . 2_676 143.15(2) ?
O32 K1 O42 2_676 2_676 68.87(3) ?
O32 K1 O42 . 2_676 73.68(3) ?
O11 K1 O42 . 2_676 107.42(3) ?
O41 K1 O42 1_455 2_676 86.81(4) ?
O21 K1 N1 . . 57.41(3) ?
O32 K1 N1 2_676 . 124.19(3) ?
O32 K1 N1 . . 88.57(4) ?
O11 K1 N1 . . 56.99(3) ?
O41 K1 N1 1_455 . 108.56(4) ?
O42 K1 N1 2_676 . 159.182(19) ?
O42 K2 O22 2_676 1_556 89.86(3) ?
O42 K2 O31 2_676 . 125.88(3) ?
O22 K2 O31 1_556 . 143.60(2) ?
O42 K2 O2W 2_676 . 82.71(4) ?
O22 K2 O2W 1_556 . 90.08(4) ?
O31 K2 O2W . . 88.23(4) ?
O42 K2 O32 2_676 . 78.78(3) ?
O22 K2 O32 1_556 . 168.208(18) ?
O31 K2 O32 . . 47.26(2) ?
O2W K2 O32 . . 85.38(4) ?
O42 K2 O21 2_676 2_676 82.54(3) ?
O22 K2 O21 1_556 2_676 108.46(4) ?
O31 K2 O21 . 2_676 85.40(3) ?
O2W K2 O21 . 2_676 156.19(2) ?
O32 K2 O21 . 2_676 73.48(4) ?
O31 K3 O41 2_676 1_455 104.20(3) ?
O31 K3 O22 2_676 2_575 165.409(19) ?
O41 K3 O22 1_455 2_575 89.89(3) ?
O31 K3 O3W 2_676 . 88.59(4) ?
O41 K3 O3W 1_455 . 131.33(3) ?
O22 K3 O3W 2_575 . 84.80(4) ?
O31 K3 O12 2_676 1_565 77.61(4) ?
O41 K3 O12 1_455 1_565 130.68(3) ?
O22 K3 O12 2_575 1_565 90.39(4) ?
O3W K3 O12 . 1_565 97.77(3) ?
O31 K3 O2W 2_676 2_576 97.12(4) ?
O41 K3 O2W 1_455 2_576 77.58(3) ?
O22 K3 O2W 2_575 2_576 82.01(4) ?
O3W K3 O2W . 2_576 148.18(2) ?
O12 K3 O2W 1_565 2_576 53.69(3) ?
O31 K3 O21 2_676 . 81.94(4) ?
O41 K3 O21 1_455 . 64.60(3) ?
O22 K3 O21 2_575 . 108.05(4) ?
O3W K3 O21 . . 71.32(3) ?
O12 K3 O21 1_565 . 157.09(2) ?
O2W K3 O21 2_576 . 140.42(2) ?
K1 O21 K2 . 2_676 93.61(4) ?
K1 O21 K3 . . 96.82(3) ?
K2 O21 K3 2_676 . 86.76(3) ?
K2 O22 K3 1_554 2_575 94.53(3) ?
K2 O31 K3 . 2_676 98.23(4) ?
K1 O32 K1 2_676 . 86.70(4) ?
K1 O32 K2 2_676 . 94.60(3) ?
K1 O32 K2 . . 97.95(3) ?
K1 O41 K3 1_655 1_655 102.76(3) ?
K2 O42 K1 2_676 2_676 94.35(3) ?
C22 N1 C12 . . 109.34(6) ?
C22 N1 C1 . . 110.20(6) ?
C12 N1 C1 . . 107.16(6) ?
C22 N1 K1 . . 108.47(5) ?
C12 N1 K1 . . 88.75(5) ?
C1 N1 K1 . . 129.66(5) ?
C32 N2 C42 . . 112.28(6) ?
C32 N2 C2 . . 114.23(6) ?
C42 N2 C2 . . 110.77(6) ?
N1 C1 C2 . . 112.98(7) ?
N2 C2 C1 . . 111.15(7) ?
O11 C11 O12 . . 126.46(8) ?
O11 C11 C12 . . 118.57(7) ?
O12 C11 C12 . . 114.83(7) ?
N1 C12 C11 . . 114.75(6) ?
O21 C21 O22 . . 125.11(7) ?
O21 C21 C22 . . 120.74(7) ?
O22 C21 C22 . . 114.11(7) ?
N1 C22 C21 . . 116.01(6) ?
O31 C31 O32 . . 126.68(7) ?
O31 C31 C32 . . 116.41(6) ?
O32 C31 C32 . . 116.91(6) ?
N2 C32 C31 . . 109.49(6) ?
O41 C41 O42 . . 128.32(7) ?
O41 C41 C42 . . 116.12(7) ?
O42 C41 C42 . . 115.53(7) ?
N2 C42 C41 . . 109.40(6) ?
K2 O2W K3 . 2_576 87.49(4) ?
H31W O3W H32W . . 105.3 ?
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_site_symmetry_2
_geom_bond_distance
_geom_bond_publ_flag
K1 O21 . 2.6637(9) ?
K1 O32 2_676 2.6767(11) ?
K1 O32 . 2.6962(11) ?
K1 O11 . 2.7077(11) ?
K1 O41 1_455 2.7351(12) ?
K1 O42 2_676 3.0873(12) ?
K1 N1 . 3.1769(13) ?
K1 K1 2_676 3.6881(18) ?
K1 K2 2_676 4.0729(13) ?
K2 O42 2_676 2.6156(10) ?
K2 O22 1_556 2.6767(10) ?
K2 O31 . 2.7182(11) ?
K2 O2W . 2.7386(15) ?
K2 O32 . 2.8625(10) ?
K2 O21 2_676 2.9180(14) ?
K2 K3 2_576 4.0096(15) ?
K2 K3 2_676 4.1238(16) ?
K3 O31 2_676 2.7363(14) ?
K3 O41 1_455 2.7781(10) ?
K3 O22 2_575 2.7814(14) ?
K3 O3W . 2.8185(10) ?
K3 O12 1_565 2.8447(11) ?
K3 O2W 2_576 3.0512(12) ?
K3 O21 . 3.0836(12) ?
O11 C11 . 1.2508(11) ?
O12 C11 . 1.2585(11) ?
O21 C21 . 1.2471(10) ?
O22 C21 . 1.2636(9) ?
O31 C31 . 1.2496(9) ?
O32 C31 . 1.2579(9) ?
O41 C41 . 1.2499(10) ?
O42 C41 . 1.2512(10) ?
N1 C22 . 1.4694(10) ?
N1 C12 . 1.4696(11) ?
N1 C1 . 1.4741(11) ?
N2 C32 . 1.4894(10) ?
N2 C42 . 1.4937(11) ?
N2 C2 . 1.4987(11) ?
N2 H2 . 0.9300 ?
C1 C2 . 1.5131(12) ?
C1 H1A . 0.9900 ?
C1 H1B . 0.9900 ?
C2 H2A . 0.9900 ?
C2 H2B . 0.9900 ?
C11 C12 . 1.5354(11) ?
C12 H12A . 0.9900 ?
C12 H12B . 0.9900 ?
C21 C22 . 1.5350(11) ?
C22 H22A . 0.9900 ?
C22 H22B . 0.9900 ?
C31 C32 . 1.5270(11) ?
C32 H32A . 0.9900 ?
C32 H32B . 0.9900 ?
C41 C42 . 1.5333(11) ?
C42 H42A . 0.9900 ?
C42 H42B . 0.9900 ?
O2W H21W . 0.8547 ?
O2W H22W . 0.8577 ?
O3W H31W . 0.8609 ?
O3W H32W . 0.8589 ?
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
N2 H2 O42 . 0.93 2.12 2.6364(11) 113.8
N2 H2 N1 . 0.93 2.50 2.9505(15) 110.1
O2W H21W O12 2_566 0.85 1.86 2.6690(12) 156.5
O2W H22W O11 . 0.86 1.96 2.7933(12) 162.1
O3W H31W O22 . 0.86 1.92 2.7786(12) 174.8
O3W H32W O41 2_675 0.86 2.51 3.2101(16) 139.2
O3W H32W O21 2_575 0.86 2.55 3.2417(17) 138.1
C1 H1B O31 2_666 0.99 2.34 3.3040(13) 164.3
C2 H2A O12 1_655 0.99 2.58 3.4313(15) 144.4
C32 H32B O31 2_666 0.99 2.44 3.3870(18) 160.5
C42 H42A O11 1_655 0.99 2.53 3.4338(15) 151.9
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_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion
_geom_torsion_publ_flag
N1 C1 C2 N2 . . . . 58.12(8) ?
C22 N1 C12 C11 . . . . -169.06(6) ?
C1 N1 C12 C11 . . . . 71.51(8) ?
O11 C11 C12 N1 . . . . 31.84(10) ?
O12 C11 C12 N1 . . . . -152.21(7) ?
C12 N1 C22 C21 . . . . 73.87(9) ?
C1 N1 C22 C21 . . . . -168.59(6) ?
O21 C21 C22 N1 . . . . 13.17(10) ?
O22 C21 C22 N1 . . . . -169.15(6) ?
C42 N2 C32 C31 . . . . 75.56(8) ?
C2 N2 C32 C31 . . . . -157.23(6) ?
O31 C31 C32 N2 . . . . -160.49(6) ?
O32 C31 C32 N2 . . . . 20.36(9) ?
C32 N2 C42 C41 . . . . -146.30(6) ?
C2 N2 C42 C41 . . . . 84.66(7) ?
O41 C41 C42 N2 . . . . -157.85(7) ?
O42 C41 C42 N2 . . . . 23.95(9) ?
