 
data_shelx
 
_audit_creation_method            'SHELXL-2018/1'
_shelx_SHELXL_version_number      '2018/1'
_chemical_name_mineral            'zincolivenite'
_chemical_compound_source         'Tripi mine, Alì, Sicily, Italy'
_chemical_formula_analytical
;      
As1.01 Cu0.73 H1.01 O5.01 Zn1.25
; 
_chemical_formula_sum
 'As Cu H O5 Zn' 
_chemical_formula_weight          284.87

loop_
 _atom_type_symbol
 _atom_type_description
 _atom_type_scat_dispersion_real
 _atom_type_scat_dispersion_imag
 _atom_type_scat_source
 'As'  'As'   0.0499   2.0058
 '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'
 'O'  'O'   0.0106   0.0060
 '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'
 'H'  'H'   0.0000   0.0000
 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
 
_space_group_crystal_system       orthorhombic
_space_group_IT_number            58
_space_group_name_H-M_alt         'P n n m'
_space_group_name_Hall            '-P 2 2n'
 
_shelx_space_group_comment
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;
 
loop_
 _space_group_symop_operation_xyz
 'x, y, z'
 '-x, -y, z'
 'x+1/2, -y+1/2, -z+1/2'
 '-x+1/2, y+1/2, -z+1/2'
 '-x, -y, -z'
 'x, y, -z'
 '-x-1/2, y-1/2, z-1/2'
 'x-1/2, -y-1/2, z-1/2'
 
_cell_length_a                    8.4594(9)
_cell_length_b                    8.5324(8)
_cell_length_c                    5.9893(6)
_cell_angle_alpha                 90
_cell_angle_beta                  90
_cell_angle_gamma                 90
_cell_volume                      432.30(8)
_cell_formula_units_Z             4
_cell_measurement_temperature     293(2)
_cell_measurement_reflns_used     2993
_cell_measurement_theta_min       3.391
_cell_measurement_theta_max       28.245
 
_exptl_crystal_description        'prismatic'
_exptl_crystal_colour             'light green'
_exptl_crystal_density_meas       'not measured'
_exptl_crystal_density_method     ?
_exptl_crystal_density_diffrn     4.377          
_exptl_crystal_F_000              532
_exptl_transmission_factor_min    0.354
_exptl_transmission_factor_max    0.488
_exptl_crystal_size_max           0.070
_exptl_crystal_size_mid           0.050
_exptl_crystal_size_min           0.040
_exptl_absorpt_coefficient_mu     17.972
_shelx_estimated_absorpt_T_min    ?
_shelx_estimated_absorpt_T_max    ?
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min   ?
_exptl_absorpt_correction_T_max   ?
_exptl_absorpt_process_details    
;
 SADABS 2016/2: Krause, L., Herbst-Irmer, R., Sheldrick G.M. & Stalke D.,
 J. Appl. Cryst. 48 (2015) 3-10
;
_exptl_absorpt_special_details    ?
_diffrn_ambient_temperature       293(2)
_diffrn_radiation_wavelength      0.71073
_diffrn_radiation_type            MoK\a
_diffrn_source                    'micro-focus'
_diffrn_measurement_device_type   'Bruker D8 Venture'
_diffrn_reflns_number             4860
_diffrn_reflns_av_unetI/netI      0.0260
_diffrn_reflns_av_R_equivalents   0.0393
_diffrn_reflns_limit_h_min        -11
_diffrn_reflns_limit_h_max        10
_diffrn_reflns_limit_k_min        -11
_diffrn_reflns_limit_k_max        11
_diffrn_reflns_limit_l_min        -7
_diffrn_reflns_limit_l_max        7
_diffrn_reflns_theta_min          3.391
_diffrn_reflns_theta_max          28.367
_diffrn_reflns_theta_full         25.242
_diffrn_measured_fraction_theta_max   0.998
_diffrn_measured_fraction_theta_full  1.000
_diffrn_reflns_Laue_measured_fraction_max    0.998
_diffrn_reflns_Laue_measured_fraction_full   1.000
_diffrn_reflns_point_group_measured_fraction_max   0.998
_diffrn_reflns_point_group_measured_fraction_full  1.000
_reflns_number_total              586
_reflns_number_gt                 523
_reflns_threshold_expression      'I > 2σ(I)'
_reflns_Friedel_coverage          0.000
_reflns_Friedel_fraction_max      .
_reflns_Friedel_fraction_full     .
 
_reflns_special_details
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
;
 
_computing_data_collection      'Apex4 (Bruker AXS Inc., 2022)'
_computing_cell_refinement      'Apex4 (Bruker AXS Inc., 2022)'
_computing_data_reduction       'Apex4 (Bruker AXS Inc., 2022)'
_computing_structure_refinement 'SHELXL-2018/1 (Sheldrick, 2018)'
_computing_molecular_graphics     ?
_computing_publication_material   ?
_refine_special_details           ?
_refine_ls_structure_factor_coef  Fsqd
_refine_ls_matrix_type            full
_refine_ls_weighting_scheme       calc
_refine_ls_weighting_details
'w=1/[σ²(Fo²)+2.3444P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary      ?
_atom_sites_solution_secondary    ?
_atom_sites_solution_hydrogens    difmap
_refine_ls_hydrogen_treatment     refxyz
_refine_ls_extinction_method      none
_refine_ls_extinction_coef        .
_refine_ls_number_reflns          586
_refine_ls_number_parameters      47
_refine_ls_number_restraints      1
_refine_ls_R_factor_all           0.0273
_refine_ls_R_factor_gt            0.0230
_refine_ls_wR_factor_ref          0.0497
_refine_ls_wR_factor_gt           0.0485
_refine_ls_goodness_of_fit_ref    1.184
_refine_ls_restrained_S_all       1.184
_refine_ls_shift/su_max           0.000
_refine_ls_shift/su_mean          0.000
 
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_site_symmetry_order  
 _atom_site_calc_flag
 _atom_site_refinement_flags_posn
 _atom_site_refinement_flags_adp
 _atom_site_refinement_flags_occupancy
 _atom_site_disorder_assembly
 _atom_site_disorder_group
As1 As 0.24811(7) 0.23899(6) 0.500000 0.00861(14) Uani 1 2 d S T P . .
Zn1 Zn 0.12893(8) 0.36237(7) 0.000000 0.01140(15) Uani 1 2 d S T P . .
Cu1 Cu 0.000000 0.000000 0.24848(11) 0.01355(17) Uani 1 2 d S T P . .
O1 O 0.0776(5) 0.1350(4) 0.500000 0.0114(8) Uani 1 2 d S T P . .
O2 O 0.1013(5) 0.1220(4) 0.000000 0.0119(7) Uani 1 2 d DS T P . .
H H 0.191(5) 0.072(7) 0.000000 0.018 Uiso 1 2 d DS U P . .
O3 O 0.3944(5) 0.1054(4) 0.500000 0.0177(8) Uani 1 2 d S T P . .
O4 O 0.2629(4) 0.3554(3) 0.2749(5) 0.0166(6) Uani 1 1 d . . . . .
 
 
_geom_special_details
;
 All esds (except the esd in the dihedral angle between two l.s. planes)
 are estimated using the full covariance matrix.  The cell esds are taken
 into account individually in the estimation of esds in distances, angles
 and torsion angles; correlations between esds in cell parameters are only
 used when they are defined by crystal symmetry.  An approximate (isotropic)
 treatment of cell esds is used for estimating esds 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
As1 O4 1.679(3) 6_556 ?
As1 O4 1.679(3) . ?
As1 O3 1.682(4) . ?
As1 O1 1.694(4) . ?
Zn1 O4 1.999(3) . ?
Zn1 O4 1.999(3) 6 ?
Zn1 O3 2.003(4) 3_455 ?
Zn1 O2 2.064(4) . ?
Zn1 O3 2.083(4) 7_665 ?
Cu1 O1 2.006(3) 5_556 ?
Cu1 O1 2.006(3) . ?
Cu1 O2 2.008(3) . ?
Cu1 O2 2.008(3) 5 ?
Cu1 O4 2.359(3) 3_455 ?
Cu1 O4 2.359(3) 4_545 ?
Cu1 Cu1 2.9765(13) 5 ?
Cu1 Cu1 3.0128(13) 5_556 ?
O2 H 0.87(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
O4 As1 O4 106.83(19) 6_556 . ?
O4 As1 O3 110.24(13) 6_556 . ?
O4 As1 O3 110.24(13) . . ?
O4 As1 O1 111.91(12) 6_556 . ?
O4 As1 O1 111.91(12) . . ?
O3 As1 O1 105.74(19) . . ?
O4 Zn1 O4 110.85(18) . 6 ?
O4 Zn1 O3 124.43(9) . 3_455 ?
O4 Zn1 O3 124.43(9) 6 3_455 ?
O4 Zn1 O2 91.98(10) . . ?
O4 Zn1 O2 91.98(10) 6 . ?
O3 Zn1 O2 91.39(16) 3_455 . ?
O4 Zn1 O3 94.78(10) . 7_665 ?
O4 Zn1 O3 94.78(10) 6 7_665 ?
O3 Zn1 O3 76.68(18) 3_455 7_665 ?
O2 Zn1 O3 168.07(16) . 7_665 ?
O1 Cu1 O1 82.69(16) 5_556 . ?
O1 Cu1 O2 173.43(16) 5_556 . ?
O1 Cu1 O2 96.86(11) . . ?
O1 Cu1 O2 96.86(11) 5_556 5 ?
O1 Cu1 O2 173.43(16) . 5 ?
O2 Cu1 O2 84.34(16) . 5 ?
O1 Cu1 O4 93.82(13) 5_556 3_455 ?
O1 Cu1 O4 91.28(13) . 3_455 ?
O2 Cu1 O4 92.74(13) . 3_455 ?
O2 Cu1 O4 82.20(13) 5 3_455 ?
O1 Cu1 O4 91.28(13) 5_556 4_545 ?
O1 Cu1 O4 93.82(13) . 4_545 ?
O2 Cu1 O4 82.20(13) . 4_545 ?
O2 Cu1 O4 92.74(13) 5 4_545 ?
O4 Cu1 O4 173.20(14) 3_455 4_545 ?
O1 Cu1 Cu1 138.66(8) 5_556 5 ?
O1 Cu1 Cu1 138.66(8) . 5 ?
O2 Cu1 Cu1 42.17(8) . 5 ?
O2 Cu1 Cu1 42.17(8) 5 5 ?
O4 Cu1 Cu1 86.60(7) 3_455 5 ?
O4 Cu1 Cu1 86.60(7) 4_545 5 ?
O1 Cu1 Cu1 41.34(8) 5_556 5_556 ?
O1 Cu1 Cu1 41.34(8) . 5_556 ?
O2 Cu1 Cu1 137.83(8) . 5_556 ?
O2 Cu1 Cu1 137.83(8) 5 5_556 ?
O4 Cu1 Cu1 93.40(7) 3_455 5_556 ?
O4 Cu1 Cu1 93.40(7) 4_545 5_556 ?
Cu1 Cu1 Cu1 180.0 5 5_556 ?
As1 O1 Cu1 125.40(12) . 5_556 ?
As1 O1 Cu1 125.40(12) . . ?
Cu1 O1 Cu1 97.31(16) 5_556 . ?
Cu1 O2 Cu1 95.66(16) . 5 ?
Cu1 O2 Zn1 124.28(11) . . ?
Cu1 O2 Zn1 124.28(11) 5 . ?
Cu1 O2 H 97(3) . . ?
Cu1 O2 H 97(3) 5 . ?
Zn1 O2 H 113(5) . . ?
As1 O3 Zn1 129.5(2) . 3 ?
As1 O3 Zn1 127.2(2) . 7_656 ?
Zn1 O3 Zn1 103.32(18) 3 7_656 ?
As1 O4 Zn1 129.54(16) . . ?
As1 O4 Cu1 114.84(14) . 3 ?
Zn1 O4 Cu1 114.67(12) . 3 ?
 
loop_
 _geom_hbond_atom_site_label_D 
 _geom_hbond_atom_site_label_H 
 _geom_hbond_atom_site_label_A 
 _geom_hbond_distance_DH 
 _geom_hbond_distance_HA 
 _geom_hbond_distance_DA 
 _geom_hbond_angle_DHA 
 _geom_hbond_site_symmetry_A 
 _geom_hbond_publ_flag
O2 H O4  0.87(3) 2.32(4) 2.883(4) 123(4) 7_655 yes
O2 H O4  0.87(3) 2.32(4) 2.883(4) 123(4) 4_545 yes
 
_refine_diff_density_max    0.939
_refine_diff_density_min   -1.081
_refine_diff_density_rms    0.177



