#------------------------------------------------------------------------------
#$Date: 2016-02-14 16:26:36 +0200 (Sun, 14 Feb 2016) $
#$Revision: 176435 $
#$URL: svn://www.crystallography.net/cod/cif/2/01/76/2017687.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_2017687
loop_
_publ_author_name
'Martin, Lee'
'Christian, Anthony'
'Akutsu, Hiroki'
_publ_section_title
;
 Tricaesium tris(oxalato-κ²O¹,O²)chromate(III)
 dihydrate
;
_journal_coeditor_code           SQ3237
_journal_issue                   6
_journal_name_full               'Acta Crystallographica Section C'
_journal_page_first              m157
_journal_page_last               m159
_journal_paper_doi               10.1107/S0108270110014861
_journal_volume                  66
_journal_year                    2010
_chemical_formula_iupac          'Cs3 [Cr (C2 O4)3] , 2H2 O'
_chemical_formula_moiety         '3Cs + , C6 Cr1 O12 3- , 2H2 O'
_chemical_formula_sum            'C6 H4 Cr Cs3 O14'
_chemical_formula_weight         750.80
_chemical_name_systematic
;
Tricaesium tris(oxalato-κ²O¹,O²)chromate(III) 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
_cell_angle_alpha                63.662(5)
_cell_angle_beta                 89.775(4)
_cell_angle_gamma                77.221(5)
_cell_formula_units_Z            2
_cell_length_a                   8.2299(5)
_cell_length_b                   10.2956(6)
_cell_length_c                   10.9902(5)
_cell_measurement_reflns_used    4324
_cell_measurement_temperature    120
_cell_measurement_theta_max      29.0060
_cell_measurement_theta_min      2.9696
_cell_volume                     809.14(9)
_computing_cell_refinement       'CrysAlisPro (Oxford Diffraction, 2009)'
_computing_data_collection       'CrysAlisPro (Oxford Diffraction, 2009)'
_computing_data_reduction        'CrysAlisPro (Oxford Diffraction, 2009)'
_computing_molecular_graphics    'CAMERON (Watkin et al.,  1996)'
_computing_publication_material  'CRYSTALS (Betteridge et al.,  2003)'
_computing_structure_refinement  'CRYSTALS (Betteridge et al.,  2003)'
_computing_structure_solution    'SIR92 (Altomare et al.,  1994)'
_diffrn_ambient_temperature      120
_diffrn_measured_fraction_theta_full 0.993
_diffrn_measured_fraction_theta_max 0.840
_diffrn_measurement_device       Unknown
_diffrn_measurement_device_type  'Xcalibur, Sapphire3'
_diffrn_measurement_method       ω/2θ
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.018
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -8
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       14
_diffrn_reflns_limit_l_min       -11
_diffrn_reflns_number            5562
_diffrn_reflns_theta_full        25.010
_diffrn_reflns_theta_max         29.082
_diffrn_reflns_theta_min         2.976
_diffrn_standards_decay_%        0.00(10)
_diffrn_standards_interval_count 0
_diffrn_standards_interval_time  0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    7.427
_exptl_absorpt_correction_T_max  1.0000
_exptl_absorpt_correction_T_min  0.74247
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
[CrysAlisPro (Oxford Diffraction, 2009). Empirical absorption correction
using
spherical harmonics, implemented in SCALE3 ABSPACK scaling algorithm]
;
_exptl_crystal_colour            blue
_exptl_crystal_density_diffrn    3.081
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             682
_exptl_crystal_size_max          0.22
_exptl_crystal_size_mid          0.15
_exptl_crystal_size_min          0.13
_refine_diff_density_max         0.91
_refine_diff_density_min         -1.62
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.9844
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     217
_refine_ls_number_reflns         3621
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0275
_refine_ls_R_factor_gt           0.0247
_refine_ls_shift/su_max          0.0018967
_refine_ls_shift/su_mean         1.5938258
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w = 1/[σ²(F²) + ( 0.03P)² + 4.43P],where P=(max(Fo²,0) + 2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.0589
_refine_ls_wR_factor_gt          0.0580
_refine_ls_wR_factor_ref         0.0589
_reflns_number_gt                3326
_reflns_number_total             3631
_reflns_threshold_expression     I>2σ(I)
_cod_data_source_file            sq3237.cif
_cod_data_source_block           I
_cod_original_formula_sum        'C6 H4 Cr1 Cs3 O14'
_cod_database_code               2017687
_cod_database_fobs_code          2017687
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_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
Cs Cs1 0.24540(3) 1.40826(3) -0.37553(3) 0.0105 Uani 1.0000 . .
Cs Cs2 0.69122(3) 1.03653(3) 0.33926(3) 0.0124 Uani 1.0000 . .
Cs Cs3 0.17374(3) 1.72892(3) 0.10003(3) 0.0115 Uani 1.0000 . .
Cr Cr4 0.22095(8) 1.09160(7) 0.23561(7) 0.0072 Uani 1.0000 . .
O O5 0.0406(4) 1.2776(3) 0.1568(3) 0.0109 Uani 1.0000 . .
C C6 0.0508(5) 1.3697(5) 0.2030(4) 0.0095 Uani 1.0000 . .
O O7 -0.0465(4) 1.4936(3) 0.1676(3) 0.0127 Uani 1.0000 . .
C C8 0.2044(5) 1.3157(5) 0.3112(4) 0.0101 Uani 1.0000 . .
O O9 0.2811(4) 1.1766(3) 0.3532(3) 0.0113 Uani 1.0000 . .
O O10 0.2451(4) 1.4022(4) 0.3465(3) 0.0159 Uani 1.0000 . .
O O11 0.1677(4) 1.0415(3) 0.0895(3) 0.0099 Uani 1.0000 . .
C C12 0.2503(5) 1.0898(5) -0.0156(4) 0.0108 Uani 1.0000 . .
O O13 0.2270(4) 1.0800(4) -0.1212(3) 0.0167 Uani 1.0000 . .
C C14 0.3837(5) 1.1697(5) -0.0008(4) 0.0112 Uani 1.0000 . .
O O15 0.3835(4) 1.1824(3) 0.1113(3) 0.0102 Uani 1.0000 . .
O O16 0.4730(4) 1.2176(4) -0.0911(3) 0.0184 Uani 1.0000 . .
O O17 0.0684(4) 0.9793(3) 0.3519(3) 0.0115 Uani 1.0000 . .
C C18 0.1220(5) 0.8372(5) 0.3934(4) 0.0114 Uani 1.0000 . .
O O19 0.0362(4) 0.7456(4) 0.4400(4) 0.0179 Uani 1.0000 . .
C C20 0.3115(5) 0.7886(5) 0.3772(4) 0.0098 Uani 1.0000 . .
O O21 0.3855(4) 0.8979(3) 0.3349(3) 0.0112 Uani 1.0000 . .
O O22 0.3753(4) 0.6587(4) 0.4026(3) 0.0164 Uani 1.0000 . .
O O23 0.3219(4) 1.5124(4) -0.0218(4) 0.0214 Uani 1.0000 . .
O O24 0.6059(5) 1.3623(4) 0.3025(4) 0.0243 Uani 1.0000 . .
H H232 0.3810 1.4263 0.0196 0.0321 Uiso 1.0000 . .
H H242 0.5066 1.3760 0.3194 0.0365 Uiso 1.0000 . .
H H231 0.2406 1.5125 -0.0641 0.0321 Uiso 1.0000 . .
H H241 0.6028 1.4155 0.2190 0.0365 Uiso 1.0000 . .
loop_
_atom_type_symbol
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C 0.0033 0.0016 'International Tables Vol C 4.2.6.8 and 6.1.1.4'
H 0.0000 0.0000 'International Tables Vol C 4.2.6.8 and 6.1.1.4'
O 0.0106 0.0060 'International Tables Vol C 4.2.6.8 and 6.1.1.4'
Cr 0.3209 0.6236 'International Tables Vol C 4.2.6.8 and 6.1.1.4'
Cs -0.3680 2.1192 'International Tables Vol C 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_2
_geom_angle_site_symmetry_3
_geom_angle
_geom_angle_publ_flag
O5 Cr4 O9 . . . 82.68(13) no
O5 Cr4 O11 . . . 91.74(13) no
O9 Cr4 O11 . . . 169.10(13) no
O5 Cr4 O15 . . . 93.94(13) no
O9 Cr4 O15 . . . 88.75(13) no
O11 Cr4 O15 . . . 82.29(12) no
O5 Cr4 O17 . . . 91.23(13) no
O9 Cr4 O17 . . . 97.77(13) no
O11 Cr4 O17 . . . 91.68(13) no
O15 Cr4 O17 . . . 172.15(13) no
O5 Cr4 O21 . . . 172.73(13) no
O9 Cr4 O21 . . . 94.89(13) no
O11 Cr4 O21 . . . 91.73(13) no
O15 Cr4 O21 . . . 92.85(13) no
O17 Cr4 O21 . . . 82.29(13) no
Cr4 O5 C6 . . . 114.4(3) no
O5 C6 O7 . . . 125.8(4) no
O5 C6 C8 . . . 114.2(4) no
O7 C6 C8 . . . 120.0(4) no
C6 C8 O9 . . . 113.4(4) no
C6 C8 O10 . . . 120.7(4) no
O9 C8 O10 . . . 125.9(4) no
Cr4 O9 C8 . . . 113.4(3) no
Cr4 O11 C12 . . . 115.1(3) no
O11 C12 O13 . . . 125.2(4) no
O11 C12 C14 . . . 114.1(4) no
O13 C12 C14 . . . 120.7(4) no
C12 C14 O15 . . . 113.4(4) no
C12 C14 O16 . . . 120.9(4) no
O15 C14 O16 . . . 125.7(4) no
Cr4 O15 C14 . . . 115.1(3) no
Cr4 O17 C18 . . . 112.0(3) no
O17 C18 O19 . . . 125.2(4) no
O17 C18 C20 . . . 113.4(4) no
O19 C18 C20 . . . 121.4(4) no
C18 C20 O21 . . . 113.2(4) no
C18 C20 O22 . . . 120.2(4) no
O21 C20 O22 . . . 126.6(4) no
Cr4 O21 C20 . . . 110.6(3) no
H232 O23 H231 . . . 109.5 no
H242 O24 H241 . . . 105.2 no
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_site_symmetry_1
_geom_bond_site_symmetry_2
_geom_bond_distance
_geom_bond_publ_flag
Cr4 O5 . . 1.975(3) no
Cr4 O9 . . 1.970(3) no
Cr4 O11 . . 1.969(3) no
Cr4 O15 . . 1.984(3) no
Cr4 O17 . . 1.966(3) no
Cr4 O21 . . 1.972(3) no
O5 C6 . . 1.275(5) no
C6 O7 . . 1.237(5) no
C6 C8 . . 1.560(6) no
C8 O9 . . 1.295(5) no
C8 O10 . . 1.223(5) no
O11 C12 . . 1.294(5) no
C12 O13 . . 1.229(5) no
C12 C14 . . 1.558(6) no
C14 O15 . . 1.296(5) no
C14 O16 . . 1.219(5) no
O17 C18 . . 1.291(5) no
C18 O19 . . 1.230(5) no
C18 C20 . . 1.564(6) no
C20 O21 . . 1.300(5) no
C20 O22 . . 1.225(5) no
O23 H232 . . 0.826 no
O23 H231 . . 0.816 no
O24 H242 . . 0.833 no
O24 H241 . . 0.831 no
loop_
_geom_hbond_atom_site_label_D
_geom_hbond_atom_site_label_H
_geom_hbond_atom_site_label_A
_geom_hbond_site_symmetry_D
_geom_hbond_site_symmetry_H
_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
O23 H232 O15 . . . 0.83 2.25 2.963(7) 145 yes
O24 H242 O10 . . . 0.83 2.15 2.974(7) 173 yes
O23 H231 C6 . . 2_585 0.82 2.58 3.333(7) 154 yes
O23 H231 O7 . . 2_585 0.82 1.99 2.809(7) 178 yes
O24 H241 O23 . . 2_685 0.83 2.10 2.886(7) 158 yes
