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_Veszelyite_173K
 
_chemical_name_common             ?
_chemical_melting_point           ?
_chemical_formula_moiety          ?
_chemical_formula_sum		  'Cu1.75 H7 O9 P Zn1.25'
_chemical_formula_weight          374.93
#----------------------------------------------------------------------------#
#                   UNIT CELL INFORMATION                                    #
#----------------------------------------------------------------------------#
_symmetry_cell_setting            monoclinic
_symmetry_space_group_name_H-M    'P 1 21/c 1'
_symmetry_space_group_name_Hall   '-P 2ycb'
_symmetry_Int_Tables_number       14

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                    7.4863(4)
_cell_length_b                    10.1933(4)
_cell_length_c                    9.7895(4)
_cell_angle_alpha                 90.00
_cell_angle_beta                  103.180(4)
_cell_angle_gamma                 90.00
_cell_volume                      727.36(6)
_cell_formula_units_Z             4
_cell_measurement_temperature     173(2)
_cell_measurement_reflns_used     7674
_cell_measurement_theta_min       2.79
_cell_measurement_theta_max       29.14
#----------------------------------------------------------------------------#
#                   CRYSTAL INFORMATION                                      #
#----------------------------------------------------------------------------#
_exptl_crystal_description        irregular
_exptl_crystal_colour             'green-blue'
_exptl_crystal_size_max           0.120
_exptl_crystal_size_mid           0.087
_exptl_crystal_size_min           0.040
_exptl_crystal_density_meas       ?
_exptl_crystal_density_diffrn     3.424
_exptl_crystal_density_method     'not measured'
_exptl_crystal_F_000              729
_exptl_absorpt_coefficient_mu     9.402
_exptl_absorpt_correction_type    integration
_exptl_absorpt_correction_T_min   0.4858
_exptl_absorpt_correction_T_max   0.7713
_exptl_absorpt_process_details    
'Empirical absorption correction based on 21 faces'
loop_
    _exptl_crystal_face_index_h
    _exptl_crystal_face_index_k
    _exptl_crystal_face_index_l
    _exptl_crystal_face_perp_dist
  -3  11   6  0.0450
   2 -11  -5  0.0470
  -5  -7   8  0.0500
  11  -4  -6  0.0240
  14  -4   1  0.0280
   3  11  -4  0.0530
  -1  13   3  0.0380
  -4   1  -1  0.0150
  -3   1   1  0.0150
  -5   7   2  0.0200
   2   4 -11  0.0540
 -15  -1   0  0.0160
  -3  -2   8  0.0540
   3  -6  -2  0.0390
  -1  -4   8  0.0530
   5  -5  -7  0.0390
   1  -2   3  0.0470
   9  -1  -4  0.0210
   6   1  -3  0.0260
  -8  -5  -3  0.0260
   8   4   1  0.0350
#----------------------------------------------------------------------------#
#                   DATA COLLECTION                                          #
#----------------------------------------------------------------------------#
_diffrn_measurement_device         '2-circle goniometer'
_diffrn_measurement_device_type    'STOE IPDS 2'
_diffrn_detector                   'image plate (34 cm diameter)'
_diffrn_detector_type              'STOE'
_diffrn_detector_area_resol_mean    6.67
_diffrn_source             'sealed X-ray tube, 12 x 0.4 mm long-fine focus'
_diffrn_source_voltage             50
_diffrn_source_current             40
_diffrn_source_power               2.00
_diffrn_radiation_type             'Mo K\a'
_diffrn_radiation_wavelength       0.71073
_diffrn_radiation_monochromator    'plane graphite'
_diffrn_radiation_polarisn_norm    0
_diffrn_radiation_collimation      '0.5 mm diameter, multiple pinhole'
_diffrn_ambient_temperature        0
_diffrn_measurement_method         'rotation method'
_diffrn_measurement_details
 '180 frames, detector distance = 100 mm'
_diffrn_reflns_number             6701
_diffrn_reflns_theta_min          2.79
_diffrn_reflns_theta_max          29.13
_diffrn_reflns_av_unetI/netI      0.0177
_diffrn_reflns_limit_h_min        -10
_diffrn_reflns_limit_h_max        10
_diffrn_reflns_limit_k_min        -13
_diffrn_reflns_limit_k_max        13
_diffrn_reflns_limit_l_min        -13
_diffrn_reflns_limit_l_max        13


_reflns_number_total              1946
_reflns_number_gt                 1829
_reflns_threshold_expression      >2sigma(I)'
_reflns_limit_h_min               -10
_reflns_limit_h_max               10
_reflns_limit_k_min               -13
_reflns_limit_k_max               13
_reflns_limit_l_min               -13
_reflns_limit_l_max               13
#----------------------------------------------------------------------------#
#                   COMPUTER PROGRAMS USED                                   #
#----------------------------------------------------------------------------# 
_computing_data_collection        'STOE X-AREA'
_computing_cell_refinement        'STOE X-AREA'
_computing_data_reduction         'STOE X-RED'
_computing_structure_solution     'SIR97 (Altomare et al)'
_computing_structure_refinement   'SHELXL-97 (Sheldrick, 1997)'
_computing_molecular_graphics     ?
_computing_publication_material   ?
#----------------------------------------------------------------------------#
#                   REFINEMENT INFORMATION                                   #
#----------------------------------------------------------------------------#
_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^ > 2sigma(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^)+(0.0376P)^2^+1.5554P] 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        0.0046(9)
_refine_ls_extinction_expression
 'Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^'
_refine_ls_number_reflns          1946
_refine_ls_number_parameters      147
_refine_ls_number_restraints      9
_refine_ls_R_factor_all           0.0287
_refine_ls_R_factor_gt            0.0261
_refine_ls_wR_factor_ref          0.0685
_refine_ls_wR_factor_gt           0.0675
_refine_ls_goodness_of_fit_ref    1.101
_refine_ls_restrained_S_all       1.099
_refine_ls_shift/su_max           0.029
_refine_ls_shift/su_mean          0.003
#----------------------------------------------------------------------------#
#                   ATOMIC TYPES, COORDINATES AND THERMAL PARAMETERS         #
#----------------------------------------------------------------------------#
loop_
 _atom_type_symbol
 _atom_type_scat_dispersion_real
 _atom_type_scat_dispersion_imag
 _atom_type_scat_source
 Cu  0.3201  1.2651
 'International Tables Vol C tables 4.2.6.8 and 6.1.1.1'
 H   0.0000  0.0000
 'International Tables Vol C tables 4.2.6.8 and 6.1.1.1'
 O   0.0106  0.0060
 'International Tables Vol C tables 4.2.6.8 and 6.1.1.1'
 P   0.1023  0.0942
 'International Tables Vol C tables 4.2.6.8 and 6.1.1.1'
 Zn  0.2839  1.4301
 'International Tables Vol C tables 4.2.6.8 and 6.1.1.1'

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 0.49198(5) 0.07238(3) 0.13093(4) 0.01181(11) Uani 0.875 1 d P . .
Zn1 Zn 0.49198(5) 0.07238(3) 0.13093(4) 0.01181(11) Uani 0.125 1 d P . .
Cu2 Cu 0.46096(5) 0.25245(3) 0.35993(3) 0.01138(11) Uani 0.875 1 d P . .
Zn2 Zn 0.46096(5) 0.25245(3) 0.35993(3) 0.01138(11) Uani 0.125 1 d P . .
Zn3 Zn 0.06992(5) 0.07500(3) 0.21193(3) 0.01153(11) Uani 1 1 d . . .
P P 0.06580(10) 0.29795(7) 0.41612(7) 0.01046(15) Uani 1 1 d . . .
O1 O 0.9742(3) 0.1587(2) 0.0333(2) 0.0143(4) Uani 1 1 d . . .
O2 O 0.9831(3) 0.1641(2) 0.3609(2) 0.0132(4) Uani 1 1 d . . .
O3 O 0.2755(3) 0.2848(2) 0.4716(2) 0.0127(4) Uani 1 1 d . . .
O4 O 0.0241(3) 0.3981(2) 0.2950(2) 0.0142(4) Uani 1 1 d . . .
OH1 O 0.3385(3) 0.0858(2) 0.2706(2) 0.0113(4) Uani 1 1 d D . .
H1 H 0.357(6) 0.024(3) 0.344(3) 0.027(11) Uiso 1 1 d D . .
OH2 O 0.6236(3) 0.2176(2) 0.2349(2) 0.0123(4) Uani 1 1 d D . .
H2 H 0.741(4) 0.185(5) 0.279(5) 0.047(15) Uiso 1 1 d D . .
OH3 O 0.6002(3) 0.40763(19) 0.4638(2) 0.0113(4) Uani 1 1 d D . .
H3 H 0.727(3) 0.387(7) 0.483(7) 0.07(2) Uiso 1 1 d D . .
H2O1 O 0.6558(3) 0.3839(2) 0.0381(2) 0.0193(4) Uani 1 1 d D . .
H4 H 0.766(4) 0.376(5) 0.007(5) 0.046(15) Uiso 1 1 d D . .
H5 H 0.653(6) 0.323(4) 0.110(4) 0.033(13) Uiso 1 1 d D . .
H2O2 O 0.3211(3) 0.4065(2) 0.1931(2) 0.0184(4) Uani 1 1 d D . .
H6 H 0.317(8) 0.364(5) 0.106(3) 0.055(17) Uiso 1 1 d D . .
H7 H 0.209(5) 0.396(8) 0.222(7) 0.10(3) Uiso 1 1 d 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 0.01297(18) 0.01154(18) 0.01180(18) -0.00213(11) 0.00469(13) -0.00167(11)
Zn1 0.01297(18) 0.01154(18) 0.01180(18) -0.00213(11) 0.00469(13) -0.00167(11)
Cu2 0.01200(18) 0.01090(18) 0.01196(17) -0.00158(12) 0.00420(12) -0.00092(11)
Zn2 0.01200(18) 0.01090(18) 0.01196(17) -0.00158(12) 0.00420(12) -0.00092(11)
Zn3 0.01203(17) 0.01120(18) 0.01152(17) -0.00063(11) 0.00300(12) -0.00074(11)
P 0.0108(3) 0.0099(3) 0.0109(3) -0.0007(2) 0.0029(2) -0.0001(2)
O1 0.0129(9) 0.0163(10) 0.0141(9) 0.0031(8) 0.0040(7) 0.0003(8)
O2 0.0145(9) 0.0117(9) 0.0140(9) -0.0022(7) 0.0048(7) -0.0003(7)
O3 0.0117(9) 0.0152(10) 0.0118(9) -0.0019(7) 0.0038(7) -0.0010(7)
O4 0.0169(10) 0.0113(9) 0.0149(9) 0.0011(8) 0.0046(7) 0.0033(8)
OH1 0.0111(9) 0.0123(9) 0.0107(9) 0.0001(7) 0.0027(7) -0.0007(7)
OH2 0.0115(9) 0.0132(9) 0.0123(9) -0.0016(7) 0.0031(7) -0.0010(7)
OH3 0.0129(9) 0.0107(9) 0.0112(9) 0.0007(7) 0.0046(7) -0.0005(7)
H2O1 0.0230(11) 0.0178(10) 0.0175(10) 0.0014(8) 0.0052(8) 0.0003(9)
H2O2 0.0151(10) 0.0227(11) 0.0177(10) -0.0006(8) 0.0047(8) -0.0013(8)
 
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 1.934(2) . ?
Cu1 OH3 1.966(2) 2_645 ?
Cu1 OH1 1.981(2) . ?
Cu1 OH3 1.995(2) 4_565 ?
Cu1 Cu2 2.9472(5) . ?
Cu1 Cu1 2.9839(7) 3_655 ?
Cu1 Zn1 2.9839(7) 3_655 ?
Cu2 OH2 1.946(2) . ?
Cu2 O3 1.981(2) . ?
Cu2 OH1 2.031(2) . ?
Cu2 OH3 2.035(2) . ?
Cu2 H2O2 2.334(2) . ?
Cu2 H2O1 2.438(2) 4_566 ?
Zn3 O1 1.931(2) 1_455 ?
Zn3 O4 1.931(2) 2_545 ?
Zn3 O2 1.951(2) 1_455 ?
Zn3 OH1 1.964(2) . ?
P O1 1.530(2) 4_466 ?
P O4 1.541(2) . ?
P O2 1.544(2) 1_455 ?
P O3 1.545(2) . ?
O1 P 1.530(2) 4_665 ?
O1 Zn3 1.931(2) 1_655 ?
O2 P 1.544(2) 1_655 ?
O2 Zn3 1.951(2) 1_655 ?
O3 Zn1 2.455(2) 4_566 ?
O4 Zn3 1.931(2) 2 ?
OH1 H1 0.943(10) . ?
OH2 H2 0.945(10) . ?
OH3 Zn1 1.966(2) 2_655 ?
OH3 Cu1 1.966(2) 2_655 ?
OH3 Zn1 1.995(2) 4_566 ?
OH3 Cu1 1.995(2) 4_566 ?
OH3 H3 0.947(10) . ?
H2O1 Zn2 2.438(2) 4_565 ?
H2O1 Cu2 2.438(2) 4_565 ?
H2O1 H4 0.945(10) . ?
H2O1 H5 0.947(10) . ?
H2O2 H6 0.947(10) . ?
H2O2 H7 0.948(10) . ?
 
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 OH3 169.73(9) . 2_645 ?
OH2 Cu1 OH1 83.68(8) . . ?
OH3 Cu1 OH1 100.84(8) 2_645 . ?
OH2 Cu1 OH3 95.74(8) . 4_565 ?
OH3 Cu1 OH3 82.24(9) 2_645 4_565 ?
OH1 Cu1 OH3 165.23(8) . 4_565 ?
OH2 Cu1 Cu2 40.72(6) . . ?
OH3 Cu1 Cu2 144.18(6) 2_645 . ?
OH1 Cu1 Cu2 43.40(6) . . ?
OH3 Cu1 Cu2 132.64(6) 4_565 . ?
OH2 Cu1 Cu1 135.66(6) . 3_655 ?
OH3 Cu1 Cu1 41.48(6) 2_645 3_655 ?
OH1 Cu1 Cu1 140.38(6) . 3_655 ?
OH3 Cu1 Cu1 40.76(6) 4_565 3_655 ?
Cu2 Cu1 Cu1 170.77(2) . 3_655 ?
OH2 Cu1 Zn1 135.66(6) . 3_655 ?
OH3 Cu1 Zn1 41.48(6) 2_645 3_655 ?
OH1 Cu1 Zn1 140.38(6) . 3_655 ?
OH3 Cu1 Zn1 40.76(6) 4_565 3_655 ?
Cu2 Cu1 Zn1 170.77(2) . 3_655 ?
Cu1 Cu1 Zn1 0.000(13) 3_655 3_655 ?
OH2 Cu2 O3 174.50(8) . . ?
OH2 Cu2 OH1 82.09(8) . . ?
O3 Cu2 OH1 94.14(8) . . ?
OH2 Cu2 OH3 97.68(8) . . ?
O3 Cu2 OH3 86.48(8) . . ?
OH1 Cu2 OH3 174.25(8) . . ?
OH2 Cu2 H2O2 85.88(8) . . ?
O3 Cu2 H2O2 90.86(8) . . ?
OH1 Cu2 H2O2 100.07(8) . . ?
OH3 Cu2 H2O2 85.63(8) . . ?
OH2 Cu2 H2O1 89.29(8) . 4_566 ?
O3 Cu2 H2O1 94.61(8) . 4_566 ?
OH1 Cu2 H2O1 88.22(8) . 4_566 ?
OH3 Cu2 H2O1 86.03(8) . 4_566 ?
H2O2 Cu2 H2O1 169.72(8) . 4_566 ?
OH2 Cu2 Cu1 40.42(6) . . ?
O3 Cu2 Cu1 135.24(6) . . ?
OH1 Cu2 Cu1 42.09(6) . . ?
OH3 Cu2 Cu1 138.09(6) . . ?
H2O2 Cu2 Cu1 89.27(6) . . ?
H2O1 Cu2 Cu1 92.93(6) 4_566 . ?
O1 Zn3 O4 108.88(9) 1_455 2_545 ?
O1 Zn3 O2 110.66(9) 1_455 1_455 ?
O4 Zn3 O2 106.27(9) 2_545 1_455 ?
O1 Zn3 OH1 112.58(9) 1_455 . ?
O4 Zn3 OH1 113.78(9) 2_545 . ?
O2 Zn3 OH1 104.40(8) 1_455 . ?
O1 P O4 109.80(12) 4_466 . ?
O1 P O2 107.74(12) 4_466 1_455 ?
O4 P O2 108.74(12) . 1_455 ?
O1 P O3 110.79(11) 4_466 . ?
O4 P O3 109.82(12) . . ?
O2 P O3 109.91(12) 1_455 . ?
P O1 Zn3 132.01(13) 4_665 1_655 ?
P O2 Zn3 119.83(12) 1_655 1_655 ?
P O3 Cu2 127.18(12) . . ?
P O3 Zn1 129.97(12) . 4_566 ?
Cu2 O3 Zn1 90.29(8) . 4_566 ?
P O4 Zn3 130.84(13) . 2 ?
Zn3 OH1 Cu1 120.69(10) . . ?
Zn3 OH1 Cu2 120.29(10) . . ?
Cu1 OH1 Cu2 94.52(8) . . ?
Zn3 OH1 H1 99(3) . . ?
Cu1 OH1 H1 118(3) . . ?
Cu2 OH1 H1 105(3) . . ?
Cu1 OH2 Cu2 98.86(9) . . ?
Cu1 OH2 H2 106(3) . . ?
Cu2 OH2 H2 115(3) . . ?
Zn1 OH3 Cu1 0.00(3) 2_655 2_655 ?
Zn1 OH3 Zn1 97.76(9) 2_655 4_566 ?
Cu1 OH3 Zn1 97.76(9) 2_655 4_566 ?
Zn1 OH3 Cu1 97.76(9) 2_655 4_566 ?
Cu1 OH3 Cu1 97.76(9) 2_655 4_566 ?
Zn1 OH3 Cu1 0.000(17) 4_566 4_566 ?
Zn1 OH3 Cu2 110.08(10) 2_655 . ?
Cu1 OH3 Cu2 110.08(10) 2_655 . ?
Zn1 OH3 Cu2 103.40(9) 4_566 . ?
Cu1 OH3 Cu2 103.40(9) 4_566 . ?
Zn1 OH3 H3 121(4) 2_655 . ?
Cu1 OH3 H3 121(4) 2_655 . ?
Zn1 OH3 H3 116(4) 4_566 . ?
Cu1 OH3 H3 116(4) 4_566 . ?
Cu2 OH3 H3 108(4) . . ?
Zn2 H2O1 Cu2 0.00(3) 4_565 4_565 ?
Zn2 H2O1 H4 99(3) 4_565 . ?
Cu2 H2O1 H4 99(3) 4_565 . ?
Zn2 H2O1 H5 93(3) 4_565 . ?
Cu2 H2O1 H5 93(3) 4_565 . ?
H4 H2O1 H5 111(4) . . ?
Cu2 H2O2 H6 104(4) . . ?
Cu2 H2O2 H7 90(5) . . ?
H6 H2O2 H7 111(4) . . ?
 
_diffrn_measured_fraction_theta_max    0.993
_diffrn_reflns_theta_full              29.13
_diffrn_measured_fraction_theta_full   0.993
_refine_diff_density_max    0.517
_refine_diff_density_min   -0.507
_refine_diff_density_rms    0.134