#------------------------------------------------------------------------------
#$Date: 2016-02-20 04:06:23 +0100 (Sat 20 de Feb de 2016) $
#$Revision: 176774 $
#$URL: svn://www.crystallography.net/cod/cif/2/20/91/2209158.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_2209158
loop_
_publ_author_name
'Belombe M., Michel'
'Nenwa, Justin'
'Fokwa T., Boniface P.'
'Dronskowski, Richard'
_publ_section_title
;
 Potassium
 trans-diaquabis[oxalato(2--)-κ²O,O']chromate(III)
;
_journal_coeditor_code           FI2001
_journal_issue                   6
_journal_name_full               'Acta Crystallographica Section E'
_journal_page_first              m1400
_journal_page_last               m1402
_journal_paper_doi               10.1107/S1600536806018344
_journal_volume                  62
_journal_year                    2006
_chemical_formula_iupac          'K [Cr (C2 O4)2 (H2 O)2]'
_chemical_formula_moiety         'K +, C4 H4 Cr O10 -'
_chemical_formula_sum            'C4 H4 Cr K O10'
_chemical_formula_weight         303.17
_chemical_name_systematic
;
Potassium trans-diaquabis[oxalato(2-)-κ²O,O']chromate(III)
;
_space_group_IT_number           12
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-C 2y'
_symmetry_space_group_name_H-M   'C 1 2/m 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                 92.228(3)
_cell_angle_gamma                90.00
_cell_formula_units_Z            2
_cell_length_a                   6.6012(10)
_cell_length_b                   7.2585(11)
_cell_length_c                   9.8539(16)
_cell_measurement_reflns_used    3283
_cell_measurement_temperature    298
_cell_measurement_theta_max      28.3
_cell_measurement_theta_min      2.1
_cell_volume                     471.79(13)
_computing_cell_refinement       SMART
_computing_data_collection       'SMART (Bruker, 1998)'
_computing_data_reduction        'SAINT (Bruker, 2000)'
_computing_molecular_graphics    'DIAMOND (Brandenburg, 1999)'
_computing_publication_material  'WinGX publication routines (Farrugia, 1999)'
_computing_structure_refinement  'SHELXL97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS97 (Sheldrick, 1997)'
_diffrn_ambient_temperature      298
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device_type  'Bruker APEX CCD area-detector'
_diffrn_measurement_method       'integration method'
_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  0.064
_diffrn_reflns_av_sigmaI/netI    0.033
_diffrn_reflns_limit_h_max       8
_diffrn_reflns_limit_h_min       -8
_diffrn_reflns_limit_k_max       9
_diffrn_reflns_limit_k_min       -9
_diffrn_reflns_limit_l_max       13
_diffrn_reflns_limit_l_min       -13
_diffrn_reflns_number            3283
_diffrn_reflns_theta_full        28.28
_diffrn_reflns_theta_max         28.3
_diffrn_reflns_theta_min         2.1
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    1.70
_exptl_absorpt_correction_T_max  0.873
_exptl_absorpt_correction_T_min  0.772
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   '(SADABS; Bruker, 2001)'
_exptl_crystal_colour            pink
_exptl_crystal_density_diffrn    2.134
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       Needle
_exptl_crystal_F_000             302
_exptl_crystal_size_max          0.32
_exptl_crystal_size_mid          0.10
_exptl_crystal_size_min          0.08
_refine_diff_density_max         0.432
_refine_diff_density_min         -1.511
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.15
_refine_ls_hydrogen_treatment    refall
_refine_ls_matrix_type           full
_refine_ls_number_parameters     46
_refine_ls_number_reflns         636
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.15
_refine_ls_R_factor_all          0.044
_refine_ls_R_factor_gt           0.044
_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)+(0.0805P)²+1.7264P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.136
_refine_ls_wR_factor_ref         0.137
_reflns_number_gt                625
_reflns_number_total             636
_reflns_threshold_expression     I>2σ(I)
_cod_data_source_file            fi2001.cif
_cod_data_source_block           I
_cod_original_sg_symbol_H-M      'C 2/m'
_cod_database_code               2209158
_cod_database_fobs_code          2209158
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, y, -z'
'x+1/2, y+1/2, z'
'-x+1/2, y+1/2, -z'
'-x, -y, -z'
'x, -y, z'
'-x+1/2, -y+1/2, -z'
'x+1/2, -y+1/2, 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
Cr Cr 0.0000 0.5000 0.5000 0.0133(3) Uani d S 1
K K 0.0000 0.0000 0.0000 0.0443(5) Uani d S 1
O O1 0.0638(3) 0.3215(3) 0.3590(2) 0.0195(5) Uani d . 1
O O2 0.1862(4) 0.3070(4) 0.1521(2) 0.0341(6) Uani d . 1
C C 0.1285(4) 0.3925(4) 0.2473(3) 0.0203(6) Uani d . 1
O O3 -0.2885(5) 0.5000 0.4385(3) 0.0235(7) Uani d S 1
H H -0.334(6) 0.585(6) 0.400(4) 0.026(10) Uiso d . 1
loop_
_atom_site_aniso_label
_atom_site_aniso_U_11
_atom_site_aniso_U_22
_atom_site_aniso_U_33
_atom_site_aniso_U_12
_atom_site_aniso_U_13
_atom_site_aniso_U_23
Cr 0.0153(5) 0.0094(4) 0.0156(5) 0.000 0.0045(3) 0.000
K 0.0533(11) 0.0412(10) 0.0391(9) 0.000 0.0120(8) 0.000
O1 0.0261(10) 0.0134(9) 0.0194(9) 0.0009(7) 0.0057(8) -0.0014(7)
O2 0.0473(14) 0.0315(13) 0.0245(11) 0.0020(11) 0.0132(10) -0.0082(9)
C 0.0216(13) 0.0189(14) 0.0205(12) 0.0008(10) 0.0034(10) -0.0020(10)
O3 0.0189(14) 0.0137(14) 0.0377(17) 0.000 -0.0022(12) 0.000
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'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Cr Cr 0.3209 0.6236 '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'
H H 0.0000 0.0000 '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
O1 Cr O1 . 5_566 180 y
O1 Cr O1 . 2_556 97.13(12) y
O1 Cr O1 5_566 2_556 82.87(12) n
O1 Cr O1 . 6_565 82.87(12) y
O1 Cr O1 5_566 6_565 97.13(12) n
O1 Cr O1 2_556 6_565 180 n
O1 Cr O3 . . 90.80(10) n
O1 Cr O3 5_566 . 89.20(10) n
O1 Cr O3 2_556 . 89.20(10) n
O1 Cr O3 6_565 . 90.80(10) n
O1 Cr O3 . 5_566 89.20(10) n
O1 Cr O3 5_566 5_566 90.80(10) n
O1 Cr O3 2_556 5_566 90.80(10) n
O1 Cr O3 6_565 5_566 89.20(10) n
O3 Cr O3 . 5_566 180 n
O2 K O2 5 . 180 y
O2 K O2 5 2 99.07(11) n
O2 K O2 . 2 80.93(11) n
O2 K O2 5 6 80.93(11) y
O2 K O2 . 6 99.07(11) y
O2 K O2 2 6 180.00(7) n
O2 K O2 5 3_445 67.07(7) n
O2 K O2 . 3_445 112.93(7) n
O2 K O2 2 3_445 109.36(4) n
O2 K O2 6 3_445 70.64(4) n
O2 K O2 5 8_455 109.36(4) n
O2 K O2 . 8_455 70.64(4) n
O2 K O2 2 8_455 67.07(7) n
O2 K O2 6 8_455 112.93(7) n
O2 K O2 3_445 8_455 56.58(10) n
O2 K O2 5 7 112.93(7) y
O2 K O2 . 7 67.07(7) y
O2 K O2 2 7 70.64(4) y
O2 K O2 6 7 109.36(4) y
O2 K O2 3_445 7 180.00(9) n
O2 K O2 8_455 7 123.42(10) n
O2 K O2 5 4_545 70.64(4) n
O2 K O2 . 4_545 109.36(4) n
O2 K O2 2 4_545 112.93(7) n
O2 K O2 6 4_545 67.07(7) n
O2 K O2 3_445 4_545 123.42(10) n
O2 K O2 8_455 4_545 180.0 n
O2 K O2 7 4_545 56.58(10) n
O2 K K 5 3 146.29(5) n
O2 K K . 3 33.71(5) n
O2 K K 2 3 72.91(5) n
O2 K K 6 3 107.09(5) n
O2 K K 3_445 3 146.64(5) n
O2 K K 8_455 3 97.70(5) n
O2 K K 7 3 33.36(5) n
O2 K K 4_545 3 82.30(5) n
O2 K K 5 3_445 33.71(5) n
O2 K K . 3_445 146.29(5) n
O2 K K 2 3_445 107.09(5) n
O2 K K 6 3_445 72.91(5) n
O2 K K 3_445 3_445 33.36(5) n
O2 K K 8_455 3_445 82.30(5) n
O2 K K 7 3_445 146.64(5) n
O2 K K 4_545 3_445 97.70(5) n
K K K 3 3_445 180.0 n
O2 K K 5 3_545 72.91(5) n
O2 K K . 3_545 107.09(5) n
O2 K K 2 3_545 146.29(5) n
O2 K K 6 3_545 33.71(5) n
O2 K K 3_445 3_545 97.70(5) n
O2 K K 8_455 3_545 146.64(5) n
O2 K K 7 3_545 82.30(5) n
O2 K K 4_545 3_545 33.36(5) n
K K K 3 3_545 95.430(12) n
K K K 3_445 3_545 84.570(12) n
O2 K K 5 3_455 107.09(5) n
O2 K K . 3_455 72.91(5) n
O2 K K 2 3_455 33.71(5) n
O2 K K 6 3_455 146.29(5) n
O2 K K 3_445 3_455 82.30(5) n
O2 K K 8_455 3_455 33.36(5) n
O2 K K 7 3_455 97.70(5) n
O2 K K 4_545 3_455 146.64(5) n
K K K 3 3_455 84.570(12) n
K K K 3_445 3_455 95.430(12) n
K K K 3_545 3_455 180.0 n
C O1 Cr . . 115.14(17) n
C O2 K . . 130.9(2) n
C O2 K . 3 113.7(2) n
K O2 K . 3 112.93(7) n
O2 C O1 . . 125.5(3) y
O2 C C . 6_565 121.17(19) y
O1 C C . 6_565 113.31(15) y
Cr O3 H . . 120(3) n
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
Cr O1 . 1.9575(19) y
Cr O1 5_566 1.9575(19) n
Cr O1 2_556 1.9575(19) n
Cr O1 6_565 1.9575(19) n
Cr O3 . 1.976(3) y
Cr O3 5_566 1.976(3) n
K O2 5 2.929(3) n
K O2 . 2.929(3) y
K O2 2 2.929(3) n
K O2 6 2.929(3) n
K O2 3_445 2.956(3) y
K O2 8_455 2.956(3) n
K O2 7 2.956(3) n
K O2 4_545 2.956(3) n
K K 3 4.9057(5) n
K K 3_445 4.9057(5) n
K K 3_545 4.9057(5) n
K K 3_455 4.9057(5) n
O1 C . 1.302(3) y
O2 C . 1.200(4) y
O2 K 3 2.956(3) n
C C 6_565 1.561(6) y
O3 H . 0.78(4) n
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
_geom_hbond_publ_flag
O3 H O1 3_455 0.78(4) 1.88(4) 2.636(3) 163(4) y
