loop_
_publ_author_name
‘Danisi et al.’
_publ_title
;In situ dehydration behavior of veszelyite (Cu,Zn)2Zn(PO4)(OH)3⋅2H2O: A single-crystal X-ray study
_journal_name_full 'American Mineralogist'
_journal_year 2013
_journal_volume 98
_journal_issue 7
_journal_paper_doi 10.2138/am.2013.4465

data_vesz200
 
_audit_creation_method            SHELXL-97
_chemical_name_mineral            'veszelyite'
_chemical_melting_point           ?
_chemical_formula_moiety          ?
_chemical_formula_sum             'H7 Cu2 O9 P Zn'
_chemical_formula_weight          374.48
 
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'
 'Zn'  'Zn'   0.2839   1.4301
 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
 
_symmetry_cell_setting            monoclinic
_symmetry_space_group_name_H-M    P2(1)/c
 
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'
 
_cell_length_a                    7.252(4)
_cell_length_b                    9.233(5)
_cell_length_c                    10.520(5)
_cell_angle_alpha                 90.00
_cell_angle_beta                  102.076(15)
_cell_angle_gamma                 90.00
_cell_volume                      688.8(6)
_cell_formula_units_Z             4
_cell_measurement_temperature     473
_cell_measurement_reflns_used     ?
_cell_measurement_theta_min       ?
_cell_measurement_theta_max       ?
 
_exptl_crystal_description        ?
_exptl_crystal_colour             ?
_exptl_crystal_size_max           ?
_exptl_crystal_size_mid           ?
_exptl_crystal_size_min           ?
_exptl_crystal_density_meas       ?
_exptl_crystal_density_diffrn     2.121
_exptl_crystal_density_method     'not measured'
_exptl_crystal_F_000              424
_exptl_absorpt_coefficient_mu     6.616
_exptl_absorpt_correction_type    ?
_exptl_absorpt_correction_T_min   ?
_exptl_absorpt_correction_T_max   ?
_exptl_absorpt_process_details    ?
 
_exptl_special_details
;
 ?
;
 
_diffrn_ambient_temperature       296(2)
_diffrn_radiation_wavelength      0.71073
_diffrn_radiation_type            MoK\a
_diffrn_radiation_source          'fine-focus sealed tube'
_diffrn_radiation_monochromator   graphite
_diffrn_measurement_device_type   ?
_diffrn_measurement_method        ?
_diffrn_detector_area_resol_mean  ?
_diffrn_standards_number          ?
_diffrn_standards_interval_count  ?
_diffrn_standards_interval_time   ?
_diffrn_standards_decay_%         ?
_diffrn_reflns_number             4483
_diffrn_reflns_av_R_equivalents   0.1027
_diffrn_reflns_av_sigmaI/netI     0.1190
_diffrn_reflns_limit_h_min        -7
_diffrn_reflns_limit_h_max        9
_diffrn_reflns_limit_k_min        -11
_diffrn_reflns_limit_k_max        12
_diffrn_reflns_limit_l_min        -12
_diffrn_reflns_limit_l_max        12
_diffrn_reflns_theta_min          2.87
_diffrn_reflns_theta_max          27.92
_reflns_number_total              1575
_reflns_number_gt                 922
_reflns_threshold_expression      >2\s(I)
 
_computing_data_collection        ?
_computing_cell_refinement        ?
_computing_data_reduction         ?
_computing_structure_solution     ?
_computing_structure_refinement   'SHELXL-97 (Sheldrick, 2008)'
_computing_molecular_graphics     ?
_computing_publication_material   ?
 
_refine_special_details
;
 Refinement of F^2^ against ALL reflections.  The weighted R-factor wR and
 goodness of fit S are based on F^2^, conventional R-factors R are based
 on F, with F set to zero for negative F^2^. The threshold expression of
 F^2^ > 2\s(F^2^) is used only for calculating R-factors(gt) etc. and is
 not relevant to the choice of reflections for refinement.  R-factors based
 on F^2^ are statistically about twice as large as those based on F, and R-
 factors based on ALL data will be even larger.
;
 
_refine_ls_structure_factor_coef  Fsqd
_refine_ls_matrix_type            full
_refine_ls_weighting_scheme       calc
_refine_ls_weighting_details
 'calc w=1/[\s^2^(Fo^2^)+(0.0844P)^2^+0.9221P] where P=(Fo^2^+2Fc^2^)/3'
_atom_sites_solution_primary      direct
_atom_sites_solution_secondary    difmap
_atom_sites_solution_hydrogens    geom
_refine_ls_hydrogen_treatment     mixed
_refine_ls_extinction_method      SHELXL
_refine_ls_extinction_coef        0.0000(12)
_refine_ls_extinction_expression
 'Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^'
_refine_ls_number_reflns          1575
_refine_ls_number_parameters      111
_refine_ls_number_restraints      0
_refine_ls_R_factor_all           0.1315
_refine_ls_R_factor_gt            0.0716
_refine_ls_wR_factor_ref          0.1930
_refine_ls_wR_factor_gt           0.1610
_refine_ls_goodness_of_fit_ref    1.036
_refine_ls_restrained_S_all       1.036
_refine_ls_shift/su_max           5.294
_refine_ls_shift/su_mean          0.062
 
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_symmetry_multiplicity
 _atom_site_calc_flag
 _atom_site_refinement_flags
 _atom_site_disorder_assembly
 _atom_site_disorder_group
Cu1 Cu 0.4798(2) 0.08719(14) 0.11512(13) 0.0290(4) Uani 1 1 d . . .
Cu2 Cu 0.4742(2) 0.22291(15) 0.36711(14) 0.0315(5) Uani 1 1 d . . .
Zn1 Zn 0.0541(2) 0.07741(14) 0.19716(14) 0.0317(5) Uani 1 1 d . . .
P4 P 0.0902(5) 0.2150(3) -0.0771(3) 0.0282(8) Uani 1 1 d . . .
OH1 O 0.3324(13) 0.0610(8) 0.2501(8) 0.034(2) Uani 1 1 d . . .
OH2 O 0.6023(13) 0.2449(8) 0.2223(9) 0.037(2) Uani 1 1 d . . .
OH3 O 0.6005(11) 0.1039(7) -0.0372(8) 0.0282(18) Uani 1 1 d . . .
O1 O -0.0130(12) 0.1742(9) 0.0301(8) 0.035(2) Uani 1 1 d . . .
O2 O -0.0201(12) 0.1634(10) 0.3432(8) 0.038(2) Uani 1 1 d . . .
O3 O 0.2947(12) 0.2645(8) -0.0172(8) 0.0302(19) Uani 1 1 d . . .
O4 O -0.1070(15) -0.0902(9) 0.1639(10) 0.051(3) Uani 1 1 d . . .
H201 O 0.6902(17) 0.0653(11) 0.4712(13) 0.067(5) Uani 1.00(3) 1 d . . .
 
loop_
 _atom_site_aniso_label
 _atom_site_aniso_U_11
 _atom_site_aniso_U_22
 _atom_site_aniso_U_33
 _atom_site_aniso_U_23
 _atom_site_aniso_U_13
 _atom_site_aniso_U_12
Cu1 0.0366(9) 0.0255(7) 0.0274(9) -0.0030(5) 0.0125(7) -0.0023(6)
Cu2 0.0373(10) 0.0261(7) 0.0335(10) -0.0075(6) 0.0129(7) -0.0041(6)
Zn1 0.0377(9) 0.0271(7) 0.0313(9) -0.0030(5) 0.0095(7) -0.0037(6)
P4 0.0295(18) 0.0237(14) 0.0314(18) 0.0032(11) 0.0064(15) -0.0041(12)
OH1 0.043(5) 0.026(4) 0.038(5) -0.003(3) 0.021(4) 0.003(4)
OH2 0.040(6) 0.032(4) 0.041(5) -0.001(4) 0.014(4) -0.007(4)
OH3 0.031(5) 0.023(4) 0.033(5) 0.000(3) 0.013(4) 0.006(3)
O1 0.036(5) 0.035(4) 0.035(5) 0.011(4) 0.009(4) -0.001(4)
O2 0.033(5) 0.051(5) 0.038(5) -0.017(4) 0.020(4) -0.003(4)
O3 0.036(5) 0.029(4) 0.027(5) 0.004(3) 0.011(4) -0.005(3)
O4 0.061(7) 0.041(5) 0.056(6) -0.015(4) 0.022(6) -0.022(5)
H201 0.062(8) 0.049(7) 0.091(10) 0.023(6) 0.019(7) 0.016(5)
 
_geom_special_details
;
 All s.u.'s (except the s.u. in the dihedral angle between two l.s. planes)
 are estimated using the full covariance matrix.  The cell s.u.'s are taken
 into account individually in the estimation of s.u.'s in distances, angles
 and torsion angles; correlations between s.u.'s in cell parameters are only
 used when they are defined by crystal symmetry.  An approximate (isotropic)
 treatment of cell s.u.'s is used for estimating s.u.'s involving l.s. planes.
;
 
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
Cu1 OH2 1.940(8) . ?
Cu1 OH1 1.962(9) . ?
Cu1 OH3 1.981(7) 3_655 ?
Cu1 OH3 1.986(8) . ?
Cu1 O3 2.375(8) . ?
Cu1 Cu2 2.940(2) . ?
Cu1 Cu1 2.974(3) 3_655 ?
Cu2 OH2 1.954(9) . ?
Cu2 O3 1.962(8) 4_566 ?
Cu2 OH3 2.006(7) 4_566 ?
Cu2 OH1 2.068(8) . ?
Cu2 H201 2.248(10) . ?
Zn1 O2 1.905(8) . ?
Zn1 O4 1.926(9) . ?
Zn1 O1 1.941(8) . ?
Zn1 OH1 1.984(9) . ?
P4 O4 1.491(9) 3 ?
P4 O2 1.524(9) 4_565 ?
P4 O1 1.525(9) . ?
P4 O3 1.554(9) . ?
OH3 Cu1 1.981(7) 3_655 ?
OH3 Cu2 2.006(7) 4_565 ?
O2 P4 1.524(9) 4_566 ?
O3 Cu2 1.962(8) 4_565 ?
O4 P4 1.491(9) 3 ?
 
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
OH2 Cu1 OH1 85.7(4) . . ?
OH2 Cu1 OH3 165.6(3) . 3_655 ?
OH1 Cu1 OH3 91.9(3) . 3_655 ?
OH2 Cu1 OH3 100.7(3) . . ?
OH1 Cu1 OH3 172.7(4) . . ?
OH3 Cu1 OH3 82.9(3) 3_655 . ?
OH2 Cu1 O3 87.5(3) . . ?
OH1 Cu1 O3 100.5(3) . . ?
OH3 Cu1 O3 106.9(3) 3_655 . ?
OH3 Cu1 O3 76.3(3) . . ?
OH2 Cu1 Cu2 41.1(3) . . ?
OH1 Cu1 Cu2 44.6(2) . . ?
OH3 Cu1 Cu2 134.0(3) 3_655 . ?
OH3 Cu1 Cu2 141.8(2) . . ?
O3 Cu1 Cu2 97.0(2) . . ?
OH2 Cu1 Cu1 140.3(3) . 3_655 ?
OH1 Cu1 Cu1 133.2(2) . 3_655 ?
OH3 Cu1 Cu1 41.5(2) 3_655 3_655 ?
OH3 Cu1 Cu1 41.4(2) . 3_655 ?
O3 Cu1 Cu1 92.0(2) . 3_655 ?
Cu2 Cu1 Cu1 170.94(9) . 3_655 ?
OH2 Cu2 O3 164.3(4) . 4_566 ?
OH2 Cu2 OH3 93.8(3) . 4_566 ?
O3 Cu2 OH3 86.2(3) 4_566 4_566 ?
OH2 Cu2 OH1 82.5(3) . . ?
O3 Cu2 OH1 95.8(3) 4_566 . ?
OH3 Cu2 OH1 173.1(3) 4_566 . ?
OH2 Cu2 H201 92.9(4) . . ?
O3 Cu2 H201 102.8(4) 4_566 . ?
OH3 Cu2 H201 94.2(4) 4_566 . ?
OH1 Cu2 H201 91.8(4) . . ?
OH2 Cu2 Cu1 40.8(2) . . ?
O3 Cu2 Cu1 136.1(2) 4_566 . ?
OH3 Cu2 Cu1 134.5(2) 4_566 . ?
OH1 Cu2 Cu1 41.8(2) . . ?
H201 Cu2 Cu1 91.4(3) . . ?
O2 Zn1 O4 102.6(4) . . ?
O2 Zn1 O1 118.6(4) . . ?
O4 Zn1 O1 100.2(4) . . ?
O2 Zn1 OH1 104.4(4) . . ?
O4 Zn1 OH1 122.2(4) . . ?
O1 Zn1 OH1 109.7(4) . . ?
O4 P4 O2 109.5(6) 3 4_565 ?
O4 P4 O1 112.2(5) 3 . ?
O2 P4 O1 107.8(5) 4_565 . ?
O4 P4 O3 106.4(5) 3 . ?
O2 P4 O3 110.6(5) 4_565 . ?
O1 P4 O3 110.3(5) . . ?
Cu1 OH1 Zn1 117.6(4) . . ?
Cu1 OH1 Cu2 93.6(4) . . ?
Zn1 OH1 Cu2 117.5(4) . . ?
Cu1 OH2 Cu2 98.1(4) . . ?
Cu1 OH3 Cu1 97.1(3) 3_655 . ?
Cu1 OH3 Cu2 116.0(4) 3_655 4_565 ?
Cu1 OH3 Cu2 103.6(3) . 4_565 ?
P4 O1 Zn1 135.6(5) . . ?
P4 O2 Zn1 123.1(5) 4_566 . ?
P4 O3 Cu2 117.8(5) . 4_565 ?
P4 O3 Cu1 114.1(4) . . ?
Cu2 O3 Cu1 92.1(3) 4_565 . ?
P4 O4 Zn1 127.5(6) 3 . ?
 
_diffrn_measured_fraction_theta_max    0.952
_diffrn_reflns_theta_full              27.92
_diffrn_measured_fraction_theta_full   0.952
_refine_diff_density_max    1.887
_refine_diff_density_min   -1.721
_refine_diff_density_rms    0.331
