#------------------------------------------------------------------------------
#$Date: 2016-02-16 02:10:39 +0100 (mar 16 de feb de 2016) $
#$Revision: 176453 $
#$URL: svn://www.crystallography.net/cod/cif/7/20/46/7204615.cif $
#------------------------------------------------------------------------------
#
# This file is available in the Crystallography Open Database (COD),
# http://www.crystallography.net/
#
# All data on this site have been placed in the public domain by the
# contributors.
#
data_7204615
loop_
_publ_author_name
'Christopher D. Johnson'
'Janet M. S. Skakle'
'Magnus G. Johnston'
'Jörg Feldmann'
'Donald E. Macphee'
_publ_section_title
;
 Hydrothermal synthesis, crystal structure and aqueous stability of two
 cadmium arsenate phases, CdNH4(HAsO4)OH and Cd5H2(AsO4)4·4H2O
;
_journal_issue                   6
_journal_name_full               'J. Mater. Chem.'
_journal_page_first              1429
_journal_page_last               1432
_journal_paper_doi               10.1039/b302154h
_journal_volume                  13
_journal_year                    2003
_chemical_formula_moiety         'H10 As4 Cd5 O20'
_chemical_formula_sum            'As4 Cd5 H10 O20'
_chemical_formula_weight         1191.76
_chemical_name_systematic
; 
? 
;
_space_group_IT_number           15
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-C 2yc'
_symmetry_space_group_name_H-M   'C 1 2/c 1'
_atom_sites_solution_hydrogens   none
_atom_sites_solution_primary     heavy
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 96.369(3)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   18.382(2)
_cell_length_b                   9.7192(13)
_cell_length_c                   9.9791(13)
_cell_measurement_reflns_used    5723
_cell_measurement_temperature    120(2)
_cell_measurement_theta_max      29.44
_cell_measurement_theta_min      2.31
_cell_volume                     1771.8(4)
_computing_cell_refinement       'SAINT (Bruker, 2001)'
_computing_data_collection       'SMART (Bruker, 2001)'
_computing_data_reduction        'SAINT (Bruker, 2001)'
_computing_molecular_graphics
;
Ortex in OSCAIL (McArdle, 1994, 2000)
ATOMS (Dowty, 1999)
ORTEP-III for Windows (Farrugia, 1999)
;
_computing_publication_material  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-86 (Sheldrick, 1990)'
_diffrn_ambient_temperature      120(2)
_diffrn_detector_area_resol_mean 8.192
_diffrn_measured_fraction_theta_full 0.402
_diffrn_measured_fraction_theta_max 0.402
_diffrn_measurement_device_type  'Bruker SMART 1K CCD diffractometer'
_diffrn_measurement_method       'ω rotation with narrow frames'
_diffrn_radiation_monochromator  'silicon 111'
_diffrn_radiation_source         'Daresbury SRS station 9.8'
_diffrn_radiation_type           synchrotron
_diffrn_radiation_wavelength     0.6928
_diffrn_reflns_av_R_equivalents  0.0326
_diffrn_reflns_av_sigmaI/netI    0.0396
_diffrn_reflns_limit_h_max       22
_diffrn_reflns_limit_h_min       -25
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       12
_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_number            5553
_diffrn_reflns_theta_full        29.44
_diffrn_reflns_theta_max         29.44
_diffrn_reflns_theta_min         2.17
_diffrn_standards_decay_%        15
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    13.418
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   '(SADABS; Bruker, 2000)'
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    4.467
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             2168
_exptl_crystal_size_max          0.10
_exptl_crystal_size_mid          0.06
_exptl_crystal_size_min          0.01
_refine_diff_density_max         3.302
_refine_diff_density_min         -1.899
_refine_diff_density_rms         0.664
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.212
_refine_ls_hydrogen_treatment    none
_refine_ls_matrix_type           full
_refine_ls_number_parameters     132
_refine_ls_number_reflns         2246
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.212
_refine_ls_R_factor_all          0.0401
_refine_ls_R_factor_gt           0.0398
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
;
w=1/[σ²(Fo²)+(0.0582P)²+9.4738P] where P=(Fo²+2Fc²)/3
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0984
_refine_ls_wR_factor_ref         0.0988
_reflns_number_gt                2206
_reflns_number_total             2246
_reflns_threshold_expression     >2σ(I)
_cod_data_source_file            b302154h.txt
_cod_data_source_block           revision
_cod_original_cell_volume        1771.9(4)
_cod_original_sg_symbol_H-M      C2/c
_cod_original_formula_sum        'H10 As4 Cd5 O20'
_cod_database_code               7204615
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, y, -z+1/2'
'x+1/2, y+1/2, z'
'-x+1/2, y+1/2, -z+1/2'
'-x, -y, -z'
'x, -y, z-1/2'
'-x+1/2, -y+1/2, -z'
'x+1/2, -y+1/2, z-1/2'
loop_
_atom_site_label
_atom_site_type_symbol
_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_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
Cd1 Cd 0.0000 0.10421(5) -0.2500 0.00620(13) Uani 1 d S . .
Cd2 Cd 0.321527(18) 0.08535(3) -0.31358(3) 0.00682(12) Uani 1 d . . .
Cd3 Cd 0.177759(18) -0.02813(3) -0.13440(3) 0.00632(12) Uani 1 d . . .
As1 As 0.08373(3) -0.17680(5) -0.41298(5) 0.00546(14) Uani 1 d . . .
As2 As 0.16141(3) 0.25870(4) -0.37582(5) 0.00466(13) Uani 1 d . . .
O1 O 0.1583(2) -0.2751(4) -0.3736(4) 0.0111(7) Uani 1 d . . .
O2 O 0.0101(2) -0.2870(4) -0.4248(4) 0.0148(8) Uani 1 d . . .
O3 O 0.0790(2) -0.0645(4) -0.2892(4) 0.0101(7) Uani 1 d . . .
O4 O 0.0848(2) -0.1021(4) -0.5633(4) 0.0100(7) Uani 1 d . . .
O5 O 0.1658(2) 0.2337(3) -0.5426(3) 0.0068(6) Uani 1 d . . .
O6 O 0.07228(19) 0.2635(3) -0.3486(4) 0.0075(6) Uani 1 d . . .
O7 O 0.20288(19) 0.4084(3) -0.3317(4) 0.0086(7) Uani 1 d . . .
O8 O 0.20526(19) 0.1286(4) -0.2889(4) 0.0098(7) Uani 1 d . . .
O9 O 0.4240(3) -0.0165(5) -0.3600(6) 0.0247(10) Uani 1 d . . .
O10 O 0.2581(2) 0.0885(3) 0.0322(4) 0.0094(7) Uani 1 d . . .
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
O O 0.0106 0.0060 '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'
As As 0.0499 2.0058 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Cd Cd -0.8075 1.2024 '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
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
O3 Cd1 O3 86.6(2) 2_554 . ?
O3 Cd1 O4 75.00(12) 2_554 5_554 ?
O3 Cd1 O4 104.21(13) . 5_554 ?
O3 Cd1 O4 104.21(13) 2_554 6_556 ?
O3 Cd1 O4 75.00(12) . 6_556 ?
O4 Cd1 O4 178.96(18) 5_554 6_556 ?
O3 Cd1 O6 165.11(12) 2_554 . ?
O3 Cd1 O6 90.08(13) . . ?
O4 Cd1 O6 91.79(12) 5_554 . ?
O4 Cd1 O6 88.90(13) 6_556 . ?
O3 Cd1 O6 90.08(13) 2_554 2_554 ?
O3 Cd1 O6 165.11(12) . 2_554 ?
O4 Cd1 O6 88.90(13) 5_554 2_554 ?
O4 Cd1 O6 91.79(12) 6_556 2_554 ?
O6 Cd1 O6 96.61(17) . 2_554 ?
O8 Cd2 O9 163.16(16) . . ?
O8 Cd2 O5 95.15(13) . 7_554 ?
O9 Cd2 O5 93.64(16) . 7_554 ?
O8 Cd2 O1 82.45(14) . 4_554 ?
O9 Cd2 O1 111.56(17) . 4_554 ?
O5 Cd2 O1 92.15(12) 7_554 4_554 ?
O8 Cd2 O7 79.41(12) . 4_544 ?
O9 Cd2 O7 91.57(15) . 4_544 ?
O5 Cd2 O7 174.56(12) 7_554 4_544 ?
O1 Cd2 O7 87.39(13) 4_554 4_544 ?
O8 Cd2 O10 78.81(13) . 6 ?
O9 Cd2 O10 85.34(15) . 6 ?
O5 Cd2 O10 101.92(11) 7_554 6 ?
O1 Cd2 O10 157.42(13) 4_554 6 ?
O7 Cd2 O10 76.92(12) 4_544 6 ?
O5 Cd3 O8 157.95(13) 6_556 . ?
O5 Cd3 O3 91.87(13) 6_556 . ?
O8 Cd3 O3 82.16(13) . . ?
O5 Cd3 O4 104.88(14) 6_556 6_556 ?
O8 Cd3 O4 93.98(13) . 6_556 ?
O3 Cd3 O4 74.40(13) . 6_556 ?
O5 Cd3 O7 87.71(13) 6_556 4_544 ?
O8 Cd3 O7 78.18(12) . 4_544 ?
O3 Cd3 O7 123.42(13) . 4_544 ?
O4 Cd3 O7 158.45(12) 6_556 4_544 ?
O5 Cd3 O10 102.84(12) 6_556 . ?
O8 Cd3 O10 89.26(13) . . ?
O3 Cd3 O10 158.79(12) . . ?
O4 Cd3 O10 86.97(12) 6_556 . ?
O7 Cd3 O10 73.02(13) 4_544 . ?
O3 As1 O4 112.94(18) . . ?
O3 As1 O1 107.98(17) . . ?
O4 As1 O1 111.49(19) . . ?
O3 As1 O2 110.8(2) . . ?
O4 As1 O2 107.28(17) . . ?
O1 As1 O2 106.12(19) . . ?
O7 As2 O8 109.74(17) . . ?
O7 As2 O6 110.71(17) . . ?
O8 As2 O6 110.76(17) . . ?
O7 As2 O5 108.22(18) . . ?
O8 As2 O5 109.00(17) . . ?
O6 As2 O5 108.34(17) . . ?
As1 O1 Cd2 125.2(2) . 4_544 ?
As1 O3 Cd1 134.15(18) . . ?
As1 O3 Cd3 120.27(19) . . ?
Cd1 O3 Cd3 104.48(14) . . ?
As1 O4 Cd1 130.7(2) . 5_554 ?
As1 O4 Cd3 126.85(19) . 6 ?
Cd1 O4 Cd3 102.47(14) 5_554 6 ?
As2 O5 Cd3 123.59(18) . 6 ?
As2 O5 Cd2 121.54(17) . 7_554 ?
Cd3 O5 Cd2 114.17(15) 6 7_554 ?
As2 O6 Cd1 131.14(18) . . ?
As2 O7 Cd2 133.7(2) . 4_554 ?
As2 O7 Cd3 126.62(19) . 4_554 ?
Cd2 O7 Cd3 98.29(12) 4_554 4_554 ?
As2 O8 Cd2 119.77(19) . . ?
As2 O8 Cd3 136.4(2) . . ?
Cd2 O8 Cd3 103.80(13) . . ?
Cd3 O10 Cd2 108.67(13) . 6_556 ?
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Cd1 O3 2.253(4) 2_554 ?
Cd1 O3 2.253(4) . ?
Cd1 O4 2.293(3) 5_554 ?
Cd1 O4 2.293(3) 6_556 ?
Cd1 O6 2.328(4) . ?
Cd1 O6 2.328(4) 2_554 ?
Cd2 O8 2.219(4) . ?
Cd2 O9 2.222(5) . ?
Cd2 O5 2.299(3) 7_554 ?
Cd2 O1 2.305(3) 4_554 ?
Cd2 O7 2.325(4) 4_544 ?
Cd2 O10 2.487(3) 6 ?
Cd3 O5 2.219(3) 6_556 ?
Cd3 O8 2.265(4) . ?
Cd3 O3 2.277(3) . ?
Cd3 O4 2.301(4) 6_556 ?
Cd3 O7 2.340(4) 4_544 ?
Cd3 O10 2.384(3) . ?
As1 O3 1.658(4) . ?
As1 O4 1.669(4) . ?
As1 O1 1.682(4) . ?
As1 O2 1.720(4) . ?
As2 O7 1.679(3) . ?
As2 O8 1.686(3) . ?
As2 O6 1.691(4) . ?
As2 O5 1.692(3) . ?
O1 Cd2 2.305(4) 4_544 ?
O4 Cd1 2.293(3) 5_554 ?
O4 Cd3 2.301(4) 6 ?
O5 Cd3 2.219(3) 6 ?
O5 Cd2 2.299(3) 7_554 ?
O7 Cd2 2.325(4) 4_554 ?
O7 Cd3 2.340(4) 4_554 ?
O10 Cd2 2.487(3) 6_556 ?
