#------------------------------------------------------------------------------
#$Date: 2016-02-20 05:06:23 +0200 (Sat, 20 Feb 2016) $
#$Revision: 176774 $
#$URL: svn://www.crystallography.net/cod/cif/2/20/11/2201129.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_2201129
loop_
_publ_author_name
'El Bali, Brahim'
'Massa, Werner '
_publ_section_title
;
 Redetermination of copper(II) hydrogenphosphite dihydrate
;
_journal_issue                   4
_journal_name_full               'Acta Crystallographica Section E'
_journal_page_first              i29
_journal_page_last               i31
_journal_paper_doi               10.1107/S1600536802003574
_journal_volume                  58
_journal_year                    2002
_chemical_formula_iupac          'Cu H P1 O3, 2H2 O'
_chemical_formula_moiety         'Cu H O3 P1, 2H2 O'
_chemical_formula_sum            'Cu H5 O5 P'
_chemical_formula_weight         179.55
_chemical_name_common            'copper(II) hydrogenphosphite dihydrate'
_chemical_name_systematic
;
 ?
;
_space_group_IT_number           19
_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_Hall  'P 2ac 2ab'
_symmetry_space_group_name_H-M   'P 21 21 21'
_atom_sites_solution_hydrogens   difmap
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   6.6906(5)
_cell_length_b                   7.3727(5)
_cell_length_c                   8.9552(5)
_cell_measurement_reflns_used    8000
_cell_measurement_temperature    193(2)
_cell_measurement_theta_max      32.8
_cell_measurement_theta_min      3.6
_cell_volume                     441.74(5)
_computing_cell_refinement       XAREA
_computing_data_collection       'XAREA (Stoe & Cie, 2001)'
_computing_data_reduction        XAREA
_computing_molecular_graphics    'DIAMOND (Brandenburg, 1999)'
_computing_structure_refinement  'SHELXL97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS97 (Sheldrick, 1997)'
_diffrn_ambient_temperature      193(2)
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measurement_device_type  'Stoe IPDS-II image-plate'
_diffrn_measurement_method       'D=90 mm, Δω = 1°, 5 min/rec'
_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  0.0865
_diffrn_reflns_av_sigmaI/netI    0.0357
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_l_max       14
_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_number            11632
_diffrn_reflns_theta_full        33.98
_diffrn_reflns_theta_max         33.98
_diffrn_reflns_theta_min         3.58
_diffrn_standards_decay_%        0
_diffrn_standards_interval_time  0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    5.212
_exptl_absorpt_correction_T_max  0.710
_exptl_absorpt_correction_T_min  0.406
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   '(SHELXTL; Sheldrick, 1996)'
_exptl_crystal_colour            'light blue'
_exptl_crystal_density_diffrn    2.700
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             356
_exptl_crystal_size_max          0.08
_exptl_crystal_size_mid          0.06
_exptl_crystal_size_min          0.05
_refine_diff_density_max         0.660
_refine_diff_density_min         -0.617
_refine_ls_abs_structure_details 'Flack (1983)'
_refine_ls_abs_structure_Flack   0.010(8)
_refine_ls_extinction_coef       0.019(3)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4^
_refine_ls_extinction_method     SHELXL
_refine_ls_goodness_of_fit_ref   1.104
_refine_ls_hydrogen_treatment    refall
_refine_ls_matrix_type           full
_refine_ls_number_parameters     84
_refine_ls_number_reflns         1798
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.104
_refine_ls_R_factor_all          0.0226
_refine_ls_R_factor_gt           0.0220
_refine_ls_shift/su_max          <0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w = 1/[σ²(Fo²)+(0.02P)²+0.05P] where P = (Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0468
_refine_ls_wR_factor_ref         0.0472
_reflns_number_gt                1765
_reflns_number_total             1798
_reflns_threshold_expression     I>2σ(I)
_cod_data_source_file            mg6003.cif
_cod_data_source_block           I
_cod_database_code               2201129
_cod_database_fobs_code          2201129
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x+1/2, -y, z+1/2'
'-x, y+1/2, -z+1/2'
'x+1/2, -y+1/2, -z'
loop_
_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_disorder_assembly
_atom_site_disorder_group
_atom_site_type_symbol
Cu 0.26767(2) 0.02867(2) 0.095756(17) 0.00937(6) Uani d . 1 . . Cu
P 0.01075(5) -0.31863(5) 0.14769(4) 0.00821(7) Uani d . 1 . . P
O1 -0.02312(17) -0.38942(15) 0.30688(11) 0.01191(18) Uani d . 1 . . O
O2 0.21498(17) -0.22526(14) 0.14162(12) 0.01153(17) Uani d . 1 . . O
O3 -0.00358(16) -0.47100(16) 0.03114(11) 0.01178(16) Uani d . 1 . . O
O4 0.29938(18) 0.28458(16) 0.03218(12) 0.0144(2) Uani d . 1 . . O
H41 0.184(5) 0.350(5) 0.033(4) 0.031(6) Uiso d . 1 . . H
H42 0.353(5) 0.304(5) -0.054(4) 0.031(6) Uiso d . 1 . . H
O5 0.45467(19) 0.05250(18) 0.31261(14) 0.0181(2) Uani d . 1 . . O
H51 0.512(5) -0.042(5) 0.324(3) 0.021(4) Uiso d . 1 . . H
H52 0.549(5) 0.123(4) 0.325(3) 0.021(4) Uiso d . 1 . . H
H1 -0.113(4) -0.208(3) 0.119(3) 0.008(5) Uiso d . 1 . . H
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
Cu 0.01033(8) 0.00762(8) 0.01016(8) 0.00021(5) 0.00246(5) -0.00008(5)
P 0.00875(14) 0.00723(13) 0.00863(13) -0.00020(10) 0.00000(10) -0.0002(2)
O1 0.0116(4) 0.0139(4) 0.0102(4) -0.0028(4) 0.0016(3) 0.0008(3)
O2 0.0114(4) 0.0094(4) 0.0137(4) -0.0020(4) 0.0002(3) 0.0007(3)
O3 0.0123(4) 0.0106(3) 0.0124(4) 0.0006(4) -0.0028(3) -0.0027(4)
O4 0.0162(5) 0.0105(4) 0.0166(4) 0.0023(4) 0.0051(4) 0.0023(4)
O5 0.0161(5) 0.0167(5) 0.0217(5) -0.0009(4) -0.0053(4) -0.0010(4)
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'
P P 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Cu Cu 0.3201 1.2651 '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
O2 Cu O1 . 3_555 92.95(5) yes
O2 Cu O3 . 4_545 93.17(5) yes
O1 Cu O3 3_555 4_545 170.12(4) yes
O2 Cu O4 . . 173.88(5) yes
O1 Cu O4 3_555 . 85.61(5) yes
O3 Cu O4 4_545 . 87.49(5) yes
O2 Cu O5 . . 89.65(5) yes
O1 Cu O5 3_555 . 93.14(5) yes
O3 Cu O5 4_545 . 94.65(5) yes
O4 Cu O5 . . 96.36(5) yes
O2 Cu O5 . 2_554 84.08(4) yes
O1 Cu O5 3_555 2_554 91.36(4) yes
O3 Cu O5 4_545 2_554 81.57(4) yes
O4 Cu O5 . 2_554 90.01(4) yes
O5 Cu O5 . 2_554 172.461(11) yes
O2 P O1 . . 108.52(6) yes
O2 P O3 . . 111.12(6) yes
O1 P O3 . . 111.91(6) yes
O2 P H1 . . 107.8(12) yes
O1 P H1 . . 109.1(12) yes
O3 P H1 . . 108.3(12) yes
P O1 Cu . 3_545 130.13(7) yes
P O2 Cu . . 126.93(7) yes
P O3 Cu . 4_445 127.11(7) yes
Cu O4 H41 . . 114(2) yes
Cu O4 H42 . . 117(2) yes
H41 O4 H42 . . 106(3) yes
Cu O5 H51 . . 108(2) yes
Cu O5 H52 . . 125(2) yes
H51 O5 H52 . . 100(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
Cu O2 . 1.9488(10) yes
Cu O1 3_555 1.9499(11) yes
Cu O3 4_545 1.9531(10) yes
Cu O4 . 1.9822(12) yes
Cu O5 . 2.3168(12) yes
Cu O5 2_554 3.0001(13) yes
P O2 . 1.5310(12) yes
P O1 . 1.5349(11) yes
P O3 . 1.5364(11) yes
P H1 . 1.19(2) yes
O1 Cu 3_545 1.9499(11) no
O3 Cu 4_445 1.9531(10) no
O4 H41 . 0.91(3) yes
O4 H42 . 0.86(4) yes
O5 H51 . 0.80(3) yes
O5 H52 . 0.82(3) yes
