#------------------------------------------------------------------------------
#$Date: 2016-02-14 06:40:26 +0200 (Sun, 14 Feb 2016) $
#$Revision: 176432 $
#$URL: svn://www.crystallography.net/cod/cif/2/21/33/2213397.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_2213397
loop_
_publ_author_name
'Xu-Sheng Gao'
'Yong-Min Wan'
'Qin Zhou'
'Yuan-Xiang Shi'
'Jin-Tang Wang'
_publ_section_title
;
 Aqua(salicylidene-β-alaninato-κ²O,O')potassium(I)
;
_journal_coeditor_code           HK2219
_journal_issue                   5
_journal_name_full               'Acta Crystallographica Section E'
_journal_page_first              m1417
_journal_page_last               m1418
_journal_paper_doi               10.1107/S1600536807017199
_journal_volume                  63
_journal_year                    2007
_chemical_formula_iupac          '[K (C10 H9 N O3) (H2 O1)]'
_chemical_formula_moiety         'C10 H11 K N O4'
_chemical_formula_sum            'C10 H11 K N O4'
_chemical_formula_weight         248.30
_chemical_name_systematic
;
Aqua(salicylidene-β-alaninato-κ²O,O')potassium(I)
;
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/c 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                 100.29(3)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   17.792(4)
_cell_length_b                   7.9920(16)
_cell_length_c                   8.3590(17)
_cell_measurement_reflns_used    25
_cell_measurement_temperature    294(2)
_cell_measurement_theta_max      12
_cell_measurement_theta_min      9
_cell_volume                     1169.5(4)
_computing_cell_refinement       'CAD-4 Software'
_computing_data_collection       'CAD-4 Software (Enraf--Nonius, 1989)'
_computing_data_reduction        'XCAD4 (Harms & Wocadlo, 1995)'
_computing_molecular_graphics    'SHELXTL (Bruker, 2000)'
_computing_publication_material  SHELXTL
_computing_structure_refinement  'SHELXL97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS97 (Sheldrick, 1997)'
_diffrn_ambient_temperature      294(2)
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device_type  'Nonius CAD-4'
_diffrn_measurement_method       ω/2θ
_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  0.0000
_diffrn_reflns_av_sigmaI/netI    0.0601
_diffrn_reflns_limit_h_max       21
_diffrn_reflns_limit_h_min       -21
_diffrn_reflns_limit_k_max       9
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       10
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_number            2289
_diffrn_reflns_theta_full        25.97
_diffrn_reflns_theta_max         25.97
_diffrn_reflns_theta_min         1.16
_diffrn_standards_decay_%        0
_diffrn_standards_interval_time  120
_diffrn_standards_number         3
_exptl_absorpt_coefficient_mu    0.452
_exptl_absorpt_correction_T_max  0.9562
_exptl_absorpt_correction_T_min  0.8763
_exptl_absorpt_correction_type   psi-scan
_exptl_absorpt_process_details   '(North et al.,  1968)'
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.410
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       Block
_exptl_crystal_F_000             516
_exptl_crystal_size_max          0.30
_exptl_crystal_size_mid          0.30
_exptl_crystal_size_min          0.10
_refine_diff_density_max         0.402
_refine_diff_density_min         -0.400
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.029
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     136
_refine_ls_number_reflns         2289
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.029
_refine_ls_R_factor_all          0.1001
_refine_ls_R_factor_gt           0.0597
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[σ²(Fo²)+(0.0497P)²+0.8368P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1274
_refine_ls_wR_factor_ref         0.1416
_reflns_number_gt                1477
_reflns_number_total             2289
_reflns_threshold_expression     I>2σ(I)
_cod_data_source_file            hk2219.cif
_cod_data_source_block           I
_cod_original_sg_symbol_Hall     '-P 2yc'
_cod_original_sg_symbol_H-M      'P 21/c'
_cod_database_code               2213397
_cod_database_fobs_code          2213397
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, y+1/2, -z+1/2'
'-x, -y, -z'
'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_refinement_flags
_atom_site_occupancy
K K1 0.09787(5) 0.29832(11) 0.46274(10) 0.0450(3) Uani d . 1
O O1 0.24818(16) 0.3775(4) 0.5024(3) 0.0613(8) Uani d . 1
O O2 0.11341(15) 0.4556(3) 0.1794(3) 0.0444(7) Uani d . 1
O O3 0.05205(16) 0.6977(4) 0.1716(4) 0.0617(8) Uani d . 1
O O1W 0.06474(10) 0.4638(2) 0.7220(2) 0.0593(8) Uani d . 1
H H4B 0.0116 0.4980 0.7058 0.071 Uiso calc R 1
H H4A 0.0974 0.5605 0.7495 0.071 Uiso calc R 1
N N1 0.27039(10) 0.5358(2) 0.2451(2) 0.0485(8) Uani d R 1
C C1 0.31233(10) 0.4326(2) 0.5746(2) 0.0507(10) Uani d R 1
C C2 0.34179(10) 0.3983(2) 0.7406(2) 0.0665(13) Uani d R 1
H H2 0.3131 0.3329 0.7994 0.080 Uiso calc R 1
C C3 0.4114(3) 0.4586(7) 0.8173(6) 0.0765(15) Uani d . 1
H H3 0.4286 0.4325 0.9261 0.092 Uiso calc R 1
C C4 0.4568(3) 0.5579(7) 0.7361(6) 0.0733(14) Uani d . 1
H H4 0.5037 0.5977 0.7896 0.088 Uiso calc R 1
C C5 0.4312(2) 0.5953(6) 0.5775(6) 0.0643(13) Uani d . 1
H H5 0.4615 0.6613 0.5228 0.077 Uiso calc R 1
C C6 0.3602(2) 0.5373(5) 0.4926(5) 0.0488(10) Uani d . 1
C C7 0.3354(2) 0.5822(5) 0.3285(5) 0.0524(11) Uani d . 1
H H7 0.3672 0.6483 0.2780 0.063 Uiso calc R 1
C C8 0.2400(2) 0.5883(6) 0.0790(5) 0.0551(11) Uani d . 1
H H8A 0.2270 0.4906 0.0108 0.066 Uiso calc R 1
H H8B 0.2783 0.6517 0.0359 0.066 Uiso calc R 1
C C9 0.1697(2) 0.6948(5) 0.0771(5) 0.0495(10) Uani d . 1
H H9A 0.1498 0.7274 -0.0342 0.059 Uiso calc R 1
H H9B 0.1843 0.7960 0.1389 0.059 Uiso calc R 1
C C10 0.1065(2) 0.6081(5) 0.1470(4) 0.0391(9) Uani 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'
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
O1W K1 O2 . 4_566 80.81(7) yes
O1W K1 O1 . . 98.05(8) yes
O2 K1 O1 4_566 . 96.48(9) yes
O1W K1 O2 . . 122.77(7) yes
O2 K1 O2 4_566 . 155.59(8) yes
O1 K1 O2 . . 75.45(9) yes
O1W K1 O3 . 2_545 97.66(8) yes
O2 K1 O3 4_566 2_545 91.66(9) yes
O1 K1 O3 . 2_545 163.28(9) yes
O2 K1 O3 . 2_545 91.19(9) yes
O1W K1 O1W . 4_565 150.37(7) yes
O2 K1 O1W 4_566 4_565 84.61(7) yes
O1 K1 O1W . 4_565 109.16(8) yes
O2 K1 O1W . 4_565 76.71(7) yes
O3 K1 O1W 2_545 4_565 57.00(7) yes
O1W K1 K1 . 4_566 42.21(4) ?
O2 K1 K1 4_566 4_566 38.94(5) ?
O1 K1 K1 . 4_566 95.48(7) ?
O2 K1 K1 . 4_566 162.10(6) ?
O3 K1 K1 2_545 4_566 100.00(7) ?
O1W K1 K1 4_565 4_566 121.13(5) ?
O1W K1 K1 . 4_565 156.81(5) ?
O2 K1 K1 4_566 4_565 120.32(7) ?
O1 K1 K1 . 4_565 89.39(7) ?
O2 K1 K1 . 4_565 38.30(5) ?
O3 K1 K1 2_545 4_565 73.90(7) ?
O1W K1 K1 4_565 4_565 38.72(4) ?
K1 K1 K1 4_566 4_565 159.06(5) ?
O1W K1 K1 . 3_566 46.14(4) ?
O2 K1 K1 4_566 3_566 113.69(6) ?
O1 K1 K1 . 3_566 122.87(8) ?
O2 K1 K1 . 3_566 89.53(6) ?
O3 K1 K1 2_545 3_566 65.94(6) ?
O1W K1 K1 4_565 3_566 120.49(5) ?
K1 K1 K1 4_566 3_566 82.46(3) ?
K1 K1 K1 4_565 3_566 111.84(3) ?
C1 O1 K1 . . 157.2(2) yes
C10 O2 K1 . 4_565 126.4(2) yes
C10 O2 K1 . . 127.9(2) yes
K1 O2 K1 4_565 . 102.77(8) yes
C10 O3 K1 . 2 143.4(3) yes
K1 O1W K1 . 4_566 99.07(6) yes
K1 O1W H4B . . 112.0 ?
K1 O1W H4B 4_566 . 112.0 ?
K1 O1W H4A . . 112.0 ?
K1 O1W H4A 4_566 . 112.0 ?
H4B O1W H4A . . 109.6 ?
C7 N1 C8 . . 125.1(3) yes
O1 C1 C2 . . 122.76(15) yes
O1 C1 C6 . . 121.9(2) yes
C2 C1 C6 . . 115.35(18) ?
C3 C2 C1 . . 122.1(2) ?
C3 C2 H2 . . 118.9 ?
C1 C2 H2 . . 118.9 ?
C2 C3 C4 . . 121.6(4) ?
C2 C3 H3 . . 119.2 ?
C4 C3 H3 . . 119.2 ?
C5 C4 C3 . . 118.7(5) ?
C5 C4 H4 . . 120.6 ?
C3 C4 H4 . . 120.6 ?
C4 C5 C6 . . 122.2(5) ?
C4 C5 H5 . . 118.9 ?
C6 C5 H5 . . 118.9 ?
C7 C6 C5 . . 120.1(4) ?
C7 C6 C1 . . 119.9(3) ?
C5 C6 C1 . . 120.0(4) ?
N1 C7 C6 . . 123.1(4) yes
N1 C7 H7 . . 118.4 ?
C6 C7 H7 . . 118.4 ?
N1 C8 C9 . . 109.7(3) yes
N1 C8 H8A . . 109.7 ?
C9 C8 H8A . . 109.7 ?
N1 C8 H8B . . 109.7 ?
C9 C8 H8B . . 109.7 ?
H8A C8 H8B . . 108.2 ?
C8 C9 C10 . . 113.9(3) ?
C8 C9 H9A . . 108.8 ?
C10 C9 H9A . . 108.8 ?
C8 C9 H9B . . 108.8 ?
C10 C9 H9B . . 108.8 ?
H9A C9 H9B . . 107.7 ?
O2 C10 O3 . . 124.8(4) yes
O2 C10 C9 . . 118.4(3) yes
O3 C10 C9 . . 116.7(3) yes
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 O1W . 2.692(2) yes
K1 O2 4_566 2.701(3) yes
K1 O1 . 2.710(3) yes
K1 O2 . 2.739(3) yes
K1 O3 2_545 2.820(3) yes
K1 O1W 4_565 2.891(2) yes
K1 K1 4_566 4.2503(9) ?
K1 K1 4_565 4.2503(9) ?
K1 K1 3_566 4.8665(19) ?
O1 C1 . 1.271(3) yes
O2 C10 . 1.250(4) ?
O2 K1 4_565 2.701(3) ?
O3 C10 . 1.251(4) yes
O3 K1 2 2.820(3) ?
O1W K1 4_566 2.891(2) yes
O1W H4B . 0.9700 ?
O1W H4A . 0.9700 ?
N1 C7 . 1.293(5) yes
N1 C8 . 1.458(4) yes
C1 C2 . 1.4192 ?
C1 C6 . 1.451(4) ?
C2 C3 . 1.377(5) ?
C2 H2 . 0.9300 ?
C3 C4 . 1.391(7) ?
C3 H3 . 0.9300 ?
C4 C5 . 1.356(6) ?
C4 H4 . 0.9300 ?
C5 C6 . 1.413(6) ?
C5 H5 . 0.9300 ?
C6 C7 . 1.410(6) ?
C7 H7 . 0.9300 ?
C8 C9 . 1.510(6) ?
C8 H8A . 0.9700 ?
C8 H8B . 0.9700 ?
C9 C10 . 1.523(5) ?
C9 H9A . 0.9700 ?
C9 H9B . 0.9700 ?
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 H4B O2 3_566 0.97 2.60 3.475(3) 149.8
O1W H4A O3 4_576 0.97 2.15 2.741(3) 117.9
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_4
_geom_torsion
O1W K1 O1 C1 . . 12.6(5)
O2 K1 O1 C1 4_566 . -69.0(6)
O2 K1 O1 C1 . . 134.5(6)
O3 K1 O1 C1 2_545 . 172.4(4)
O1W K1 O1 C1 4_565 . -155.5(5)
K1 K1 O1 C1 4_566 . -29.8(6)
K1 K1 O1 C1 4_565 . 170.6(6)
K1 K1 O1 C1 3_566 . 54.7(6)
O1W K1 O2 C10 . . -0.4(3)
O2 K1 O2 C10 4_566 . -163.9(2)
O1 K1 O2 C10 . . -90.7(3)
O3 K1 O2 C10 2_545 . 99.5(3)
O1W K1 O2 C10 4_565 . 155.1(3)
K1 K1 O2 C10 4_566 . -29.6(4)
K1 K1 O2 C10 4_565 . 161.2(4)
K1 K1 O2 C10 3_566 . 33.5(3)
O1W K1 O2 K1 . 4_565 -161.60(6)
O2 K1 O2 K1 4_566 4_565 35.0(3)
O1 K1 O2 K1 . 4_565 108.12(10)
O3 K1 O2 K1 2_545 4_565 -61.70(10)
O1W K1 O2 K1 4_565 4_565 -6.08(7)
K1 K1 O2 K1 4_566 4_565 169.26(11)
K1 K1 O2 K1 3_566 4_565 -127.63(7)
O2 K1 O1W K1 4_566 4_566 6.02(7)
O1 K1 O1W K1 . 4_566 -89.29(8)
O2 K1 O1W K1 . 4_566 -167.13(7)
O3 K1 O1W K1 2_545 4_566 96.47(8)
O1W K1 O1W K1 4_565 4_566 67.52(17)
K1 K1 O1W K1 4_565 4_566 163.08(8)
K1 K1 O1W K1 3_566 4_566 142.08(8)
K1 O1 C1 C2 . . 42.5(6)
K1 O1 C1 C6 . . -136.7(5)
O1 C1 C2 C3 . . 179.9(4)
C6 C1 C2 C3 . . -0.8(3)
C1 C2 C3 C4 . . 0.4(6)
C2 C3 C4 C5 . . 0.0(7)
C3 C4 C5 C6 . . 0.2(7)
C4 C5 C6 C7 . . 178.8(4)
C4 C5 C6 C1 . . -0.7(6)
O1 C1 C6 C7 . . 0.8(5)
C2 C1 C6 C7 . . -178.5(3)
O1 C1 C6 C5 . . -179.8(3)
C2 C1 C6 C5 . . 0.9(4)
C8 N1 C7 C6 . . 175.6(4)
C5 C6 C7 N1 . . -178.7(4)
C1 C6 C7 N1 . . 0.8(6)
C7 N1 C8 C9 . . -113.6(4)
N1 C8 C9 C10 . . -57.8(4)
K1 O2 C10 O3 4_565 . 108.7(4)
K1 O2 C10 O3 . . -48.3(5)
K1 O2 C10 C9 4_565 . -73.3(4)
K1 O2 C10 C9 . . 129.7(3)
K1 O3 C10 O2 2 . -84.8(5)
K1 O3 C10 C9 2 . 97.3(4)
C8 C9 C10 O2 . . -8.8(5)
C8 C9 C10 O3 . . 169.4(3)
