#------------------------------------------------------------------------------
#$Date: 2016-02-20 00:18:51 +0200 (Sat, 20 Feb 2016) $
#$Revision: 176760 $
#$URL: svn://www.crystallography.net/cod/cif/2/01/81/2018142.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_2018142
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          '2K +, C10 H14 N2 O8 2-, 2H2 O'
_chemical_formula_moiety         '2(K +), C10 H14 N2 O8 2-, 2(H2 O)'
_chemical_formula_sum            'C10 H18 K2 N2 O10'
_chemical_formula_weight         404.46
_chemical_name_common
'dipotassium ethylenediaminetetraacetate dihydrate'
_chemical_name_systematic
;
dipotassium 2-({2-[bis(carboxylatomethyl)azaniumyl]ethyl}(carboxylatomethyl)\
azaniumyl)acetate dihydrate
;
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 94.56(3)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   8.869(3)
_cell_length_b                   18.653(5)
_cell_length_c                   9.613(3)
_cell_measurement_reflns_used    16880
_cell_measurement_temperature    110(2)
_cell_measurement_theta_max      38.55
_cell_measurement_theta_min      4.25
_cell_volume                     1585.3(8)
_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 0.996
_diffrn_measured_fraction_theta_max 0.981
_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  0.0335
_diffrn_reflns_av_sigmaI/netI    0.0436
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       32
_diffrn_reflns_limit_k_min       -32
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       -12
_diffrn_reflns_number            30091
_diffrn_reflns_theta_full        27.00
_diffrn_reflns_theta_max         38.55
_diffrn_reflns_theta_min         4.25
_exptl_absorpt_coefficient_mu    0.654
_exptl_absorpt_correction_T_max  0.959
_exptl_absorpt_correction_T_min  0.879
_exptl_absorpt_correction_type   analytical
_exptl_absorpt_process_details
;
(CrysAlis RED; Oxford Diffraction, 2008)
;
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.695
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             840
_exptl_crystal_size_max          0.31
_exptl_crystal_size_mid          0.12
_exptl_crystal_size_min          0.08
_refine_diff_density_max         0.55
_refine_diff_density_min         -0.43
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.019
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     217
_refine_ls_number_reflns         8782
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.019
_refine_ls_R_factor_all          0.0539
_refine_ls_R_factor_gt           0.0303
_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)+(0.0320P)²+0.0000P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0671
_refine_ls_wR_factor_ref         0.0716
_reflns_number_gt                6388
_reflns_number_total             8782
_reflns_threshold_expression     I>2σ(I)
_cod_data_source_file            gd3395.cif
_cod_data_source_block           I
_cod_original_sg_symbol_H-M      'P 21/n'
_cod_database_code               2018142
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x+1/2, y+1/2, -z+1/2'
'-x, -y, -z'
'x-1/2, -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_refinement_flags
_atom_site_occupancy
_atom_site_symmetry_multiplicity
_atom_site_disorder_assembly
_atom_site_disorder_group
K K1 0.57928(2) 0.655529(9) 0.589830(18) 0.01163(4) Uani d . 1 1 . .
K K2 0.44431(2) 0.432278(11) 0.75620(2) 0.01597(4) Uani d . 1 1 . .
O O11 0.39078(7) 0.67095(3) 0.36045(6) 0.01317(11) Uani d . 1 1 . .
O O12 0.27573(7) 0.73966(3) 0.19097(6) 0.01392(11) Uani d . 1 1 . .
O O21 0.32992(7) 0.55632(3) 0.62596(6) 0.01241(11) Uani d . 1 1 . .
O O22 0.25824(8) 0.46147(3) 0.49239(7) 0.01610(12) Uani d . 1 1 . .
O O31 0.25343(7) 0.81123(3) 0.82693(6) 0.01322(11) Uani d . 1 1 . .
O O32 0.32438(7) 0.71948(3) 0.69470(6) 0.01323(11) Uani d . 1 1 . .
O O41 0.25913(8) 0.53198(4) 1.13856(6) 0.01757(13) Uani d . 1 1 . .
O O42 0.39042(8) 0.58474(5) 0.97715(7) 0.02619(17) Uani d . 1 1 . .
N N1 0.13838(7) 0.64856(3) 0.48919(7) 0.00789(11) Uani d . 1 1 . .
H H1 0.2286 0.6562 0.5433 0.009 Uiso calc R 1 1 . .
N N2 0.14064(8) 0.62336(3) 0.81555(7) 0.00866(11) Uani d . 1 1 . .
H H2 0.2295 0.6127 0.7746 0.010 Uiso calc R 1 1 . .
C C1 0.01165(9) 0.66241(4) 0.58071(8) 0.00948(13) Uani d . 1 1 . .
H H1A -0.0857 0.6568 0.5238 0.011 Uiso calc R 1 1 . .
H H1B 0.0184 0.7128 0.6132 0.011 Uiso calc R 1 1 . .
C C2 0.01047(9) 0.61382(4) 0.70708(8) 0.00990(13) Uani d . 1 1 . .
H H2A -0.0848 0.6220 0.7518 0.012 Uiso calc R 1 1 . .
H H2B 0.0098 0.5634 0.6747 0.012 Uiso calc R 1 1 . .
C C11 0.27998(9) 0.70379(4) 0.30110(8) 0.00979(13) Uani d . 1 1 . .
C C12 0.13176(9) 0.70201(4) 0.37285(8) 0.01051(13) Uani d . 1 1 . .
H H12A 0.1115 0.7502 0.4103 0.013 Uiso calc R 1 1 . .
H H12B 0.0474 0.6896 0.3034 0.013 Uiso calc R 1 1 . .
C C21 0.25256(9) 0.52601(4) 0.52646(8) 0.01022(13) Uani d . 1 1 . .
C C22 0.14114(9) 0.57280(4) 0.43680(8) 0.00986(13) Uani d . 1 1 . .
H H22A 0.1700 0.5728 0.3394 0.012 Uiso calc R 1 1 . .
H H22B 0.0384 0.5520 0.4369 0.012 Uiso calc R 1 1 . .
C C31 0.25209(9) 0.74667(4) 0.78901(8) 0.01004(13) Uani d . 1 1 . .
C C32 0.15280(9) 0.69829(4) 0.87130(8) 0.01054(13) Uani d . 1 1 . .
H H32A 0.1949 0.6967 0.9698 0.013 Uiso calc R 1 1 . .
H H32B 0.0502 0.7194 0.8696 0.013 Uiso calc R 1 1 . .
C C41 0.27168(10) 0.56253(5) 1.02329(8) 0.01405(15) Uani d . 1 1 . .
C C42 0.12428(9) 0.57083(4) 0.93155(8) 0.01151(14) Uani d . 1 1 . .
H H42A 0.0937 0.5237 0.8914 0.014 Uiso calc R 1 1 . .
H H42B 0.0436 0.5874 0.9894 0.014 Uiso calc R 1 1 . .
O O1W 0.65494(8) 0.60818(4) 0.85551(7) 0.01817(13) Uani d . 1 1 . .
H H11W 0.6829 0.5647 0.8440 0.027 Uiso d R 1 1 . .
H H12W 0.5653 0.6051 0.8824 0.027 Uiso d R 1 1 . .
O O2W 0.17125(8) 0.40097(4) 0.88160(8) 0.02328(15) Uani d . 1 1 . .
H H22W 0.1813 0.3675 0.8214 0.035 Uiso d R 1 1 . .
H H21W 0.2139 0.3841 0.9580 0.035 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
O11 K1 O1W . . 153.56(2) ?
O11 K1 O12 . 4_676 123.57(3) ?
O1W K1 O12 . 4_676 78.32(3) ?
O11 K1 O22 . 3_666 98.92(3) ?
O1W K1 O22 . 3_666 85.26(3) ?
O12 K1 O22 4_676 3_666 109.44(3) ?
O11 K1 O32 . . 77.43(3) ?
O1W K1 O32 . . 86.95(3) ?
O12 K1 O32 4_676 . 94.39(3) ?
O22 K1 O32 3_666 . 152.77(2) ?
O11 K1 O21 . . 74.75(3) ?
O1W K1 O21 . . 79.43(3) ?
O12 K1 O21 4_676 . 150.82(2) ?
O22 K1 O21 3_666 . 87.18(3) ?
O32 K1 O21 . . 65.73(3) ?
O11 K1 O31 . 4_675 68.22(3) ?
O1W K1 O31 . 4_675 135.93(3) ?
O12 K1 O31 4_676 4_675 78.73(3) ?
O22 K1 O31 3_666 4_675 67.87(2) ?
O32 K1 O31 . 4_675 131.93(2) ?
O21 K1 O31 . 4_675 130.39(2) ?
O11 K2 O21 3_666 . 126.37(3) ?
O11 K2 O41 3_666 3_667 78.36(3) ?
O21 K2 O41 . 3_667 105.12(3) ?
O11 K2 O2W 3_666 . 122.23(3) ?
O21 K2 O2W . . 93.95(3) ?
O41 K2 O2W 3_667 . 134.10(3) ?
O11 K2 O42 3_666 3_667 92.11(3) ?
O21 K2 O42 . 3_667 129.51(2) ?
O41 K2 O42 3_667 3_667 46.37(3) ?
O2W K2 O42 . 3_667 89.45(3) ?
O11 K2 O31 3_666 2_546 70.80(3) ?
O21 K2 O31 . 2_546 109.20(3) ?
O41 K2 O31 3_667 2_546 143.16(2) ?
O2W K2 O31 . 2_546 56.45(2) ?
O42 K2 O31 3_667 2_546 114.25(3) ?
O11 K2 O22 3_666 . 93.35(3) ?
O21 K2 O22 . . 45.913(19) ?
O41 K2 O22 3_667 . 134.67(3) ?
O2W K2 O22 . . 88.02(3) ?
O42 K2 O22 3_667 . 174.52(2) ?
O31 K2 O22 2_546 . 68.15(3) ?
C11 O11 K1 . . 147.37(6) ?
C11 O11 K2 . 3_666 125.89(5) ?
K1 O11 K2 . 3_666 86.69(3) ?
C11 O12 K1 . 4_575 131.04(6) ?
C21 O21 K2 . . 97.18(5) ?
C21 O21 K1 . . 124.23(5) ?
K2 O21 K1 . . 109.10(3) ?
C21 O22 K1 . 3_666 150.23(6) ?
C21 O22 K2 . . 89.08(5) ?
K1 O22 K2 3_666 . 80.34(2) ?
C31 O31 K2 . 2_556 131.82(5) ?
C31 O31 K1 . 4_576 115.48(5) ?
K2 O31 K1 2_556 4_576 75.18(2) ?
C31 O32 K1 . . 154.08(5) ?
C41 O41 K2 . 3_667 93.64(6) ?
C41 O42 K2 . 3_667 91.80(6) ?
C12 N1 C22 . . 112.17(6) ?
C12 N1 C1 . . 109.65(6) ?
C22 N1 C1 . . 113.01(6) ?
C32 N2 C42 . . 110.61(6) ?
C32 N2 C2 . . 112.83(6) ?
C42 N2 C2 . . 108.90(6) ?
N1 C1 C2 . . 114.78(7) ?
N2 C2 C1 . . 115.54(7) ?
O12 C11 O11 . . 127.98(8) ?
O12 C11 C12 . . 115.05(7) ?
O11 C11 C12 . . 116.95(7) ?
N1 C12 C11 . . 111.52(7) ?
O22 C21 O21 . . 126.72(8) ?
O22 C21 C22 . . 116.05(7) ?
O21 C21 C22 . . 117.24(7) ?
N1 C22 C21 . . 112.00(6) ?
O32 C31 O31 . . 126.95(8) ?
O32 C31 C32 . . 118.93(7) ?
O31 C31 C32 . . 114.11(7) ?
N2 C32 C31 . . 113.24(7) ?
O42 C41 O41 . . 126.90(9) ?
O42 C41 C42 . . 118.05(8) ?
O41 C41 C42 . . 115.03(8) ?
N2 C42 C41 . . 111.53(7) ?
H11W O1W H12W . . 105.1 ?
H22W O2W H21W . . 104.3 ?
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 O11 . 2.6746(11) ?
K1 O1W . 2.7350(11) ?
K1 O12 4_676 2.7447(9) ?
K1 O22 3_666 2.7650(9) ?
K1 O32 . 2.8129(10) ?
K1 O21 . 2.9255(9) ?
K1 O31 4_675 3.1269(12) ?
K1 K2 3_666 3.6987(10) ?
K1 K2 . 4.6515(11) ?
K2 O11 3_666 2.7138(9) ?
K2 O21 . 2.7836(9) ?
K2 O41 3_667 2.8218(12) ?
K2 O2W . 2.8502(12) ?
K2 O42 3_667 2.8675(12) ?
K2 O31 2_546 2.9309(9) ?
K2 O22 . 2.9641(12) ?
O11 C11 . 1.2560(10) ?
O12 C11 . 1.2505(10) ?
O21 C21 . 1.2652(10) ?
O22 C21 . 1.2498(10) ?
O31 C31 . 1.2580(10) ?
O32 C31 . 1.2579(10) ?
O41 C41 . 1.2588(11) ?
O42 C41 . 1.2457(12) ?
N1 C12 . 1.4959(10) ?
N1 C22 . 1.5010(11) ?
N1 C1 . 1.5038(11) ?
N1 H1 . 0.9300 ?
N2 C32 . 1.4978(11) ?
N2 C42 . 1.5001(10) ?
N2 C2 . 1.5035(11) ?
N2 H2 . 0.9300 ?
C1 C2 . 1.5163(11) ?
C1 H1A . 0.9900 ?
C1 H1B . 0.9900 ?
C2 H2A . 0.9900 ?
C2 H2B . 0.9900 ?
C11 C12 . 1.5326(12) ?
C12 H12A . 0.9900 ?
C12 H12B . 0.9900 ?
C21 C22 . 1.5316(12) ?
C22 H22A . 0.9900 ?
C22 H22B . 0.9900 ?
C31 C32 . 1.5252(12) ?
C32 H32A . 0.9900 ?
C32 H32B . 0.9900 ?
C41 C42 . 1.5256(13) ?
C42 H42A . 0.9900 ?
C42 H42B . 0.9900 ?
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
N1 H1 O32 . 0.93 2.01 2.8029(12) 142.3
N1 H1 O21 . 0.93 2.19 2.6869(11) 112.4
N2 H2 O21 . 0.93 2.04 2.8617(12) 147.2
N2 H2 O32 . 0.93 2.32 2.7425(11) 107.4
N2 H2 O42 . 0.93 2.38 2.7004(13) 100.0
O1W H12W O42 . 0.86 1.90 2.7384(13) 166.1
O1W H11W O41 3_667 0.86 1.88 2.7226(12) 167.3
O2W H21W O1W 3_667 0.86 2.06 2.8588(14) 153.9
O2W H22W O31 2_546 0.86 1.90 2.7350(11) 163.8
C1 H1A O31 4_575 0.99 2.35 3.2480(15) 149.7
C2 H2A O1W 1_455 0.99 2.60 3.5644(16) 165.0
C1 H1B O12 4_576 0.99 2.50 3.0316(12) 113.6
C22 H22A O41 1_554 0.99 2.28 3.2205(14) 159.3
C32 H32A O12 1_556 0.99 2.33 3.2703(14) 157.9
C32 H32B O11 4_576 0.99 2.48 3.3647(12) 147.9
C42 H42A O2W . 0.99 2.39 3.2365(14) 142.6
C42 H42B O2W 3_567 0.99 2.36 3.3349(15) 166.3
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
C12 N1 C1 C2 . . . . -177.17(6) ?
C22 N1 C1 C2 . . . . 56.90(9) ?
C32 N2 C2 C1 . . . . 57.78(9) ?
C42 N2 C2 C1 . . . . -178.99(6) ?
N1 C1 C2 N2 . . . . 66.78(9) ?
C22 N1 C12 C11 . . . . -69.17(8) ?
C1 N1 C12 C11 . . . . 164.42(6) ?
O12 C11 C12 N1 . . . . 170.42(7) ?
O11 C11 C12 N1 . . . . -11.14(10) ?
C12 N1 C22 C21 . . . . 138.63(7) ?
C1 N1 C22 C21 . . . . -96.80(8) ?
O22 C21 C22 N1 . . . . 177.84(7) ?
O21 C21 C22 N1 . . . . -2.74(10) ?
C42 N2 C32 C31 . . . . 147.71(7) ?
C2 N2 C32 C31 . . . . -90.02(8) ?
O32 C31 C32 N2 . . . . -6.78(10) ?
O31 C31 C32 N2 . . . . 174.33(7) ?
C32 N2 C42 C41 . . . . -71.56(8) ?
C2 N2 C42 C41 . . . . 163.89(6) ?
O42 C41 C42 N2 . . . . -16.05(11) ?
O41 C41 C42 N2 . . . . 165.31(7) ?
