#------------------------------------------------------------------------------
#$Date: 2022-05-05 23:50:32 +0300 (Thu, 05 May 2022) $
#$Revision: 275047 $
#$URL: file:///home/coder/svn-repositories/cod/cif/7/06/12/7061269.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_7061269
loop_
_publ_author_name
'Ibrahim, Mukaila A.'
'Boeré, René T.'
_publ_section_title
;
 The copper sulfate hydration cycle. Crystal structures of CuSO4
 (Chalcocyanite), CuSO4·H2O (Poitevinite), CuSO4·3H2O
 (Bonattite) and CuSO4·5H2O (Chalcanthite) at low temperature using
 non-spherical atomic scattering factors
;
_journal_issue                   12
_journal_name_full               'New Journal of Chemistry'
_journal_page_first              5479
_journal_page_last               5488
_journal_paper_doi               10.1039/D2NJ00169A
_journal_volume                  46
_journal_year                    2022
_chemical_formula_moiety         'Cu O4 S'
_chemical_formula_sum            'Cu O4 S'
_chemical_formula_weight         159.609
_space_group_crystal_system      orthorhombic
_space_group_IT_number           62
_space_group_name_Hall           '-P 2ac 2n'
_space_group_name_H-M_alt        'P n m a'
_symmetry_Int_Tables_number      62
_atom_sites_solution_primary     heavy
_audit_creation_date             2022-01-07
_audit_creation_method
;
Olex2 1.5
(compiled 2021.12.09 svn.r5202d8cf for OlexSys, GUI svn.r6439)
;
_audit_update_record
;
2022-01-10 deposited with the CCDC.	2022-02-02 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   8.3958(6)
_cell_length_b                   6.6760(4)
_cell_length_c                   4.8270(3)
_cell_measurement_reflns_used    2493
_cell_measurement_temperature    100.0(3)
_cell_measurement_theta_max      38.1800
_cell_measurement_theta_min      4.8190
_cell_volume                     270.56(3)
_computing_cell_refinement       'CrysAlisPro 1.171.41.116a (Rigaku OD, 2021)'
_computing_data_collection       'CrysAlisPro 1.171.41.116a (Rigaku OD, 2021)'
_computing_data_reduction        'CrysAlisPro 1.171.41.116a (Rigaku OD, 2021)'
_computing_molecular_graphics    'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_structure_refinement  'olex2.refine 1.5 (Bourhis et al., 2015)'
_computing_structure_solution    'SHELXS  (Sheldrick, 2008)'
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      100.0(3)
_diffrn_detector                 'Hybrid Pixel Array Detector'
_diffrn_detector_area_resol_mean 5.8140
_diffrn_detector_type            'Pilatus 200K'
_diffrn_measured_fraction_theta_full 1.0000
_diffrn_measured_fraction_theta_max 0.9295
_diffrn_measurement_details
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  tₑₓₚ   ω     θ     κ     φ   Frames
#--------------------------------------------------------------------------
  1  ω     37.00  91.00   0.50    5.73    --   22.41-178.00   0.00  108
  2  ω    -44.00  26.00   0.50    5.73    --   22.41 -38.00-180.00  140
  3  ω     39.00  91.00   0.50    5.73    --   22.41 178.00 150.00  104
  4  ω    -92.00 -22.00   0.50    5.73    --  -25.54 -38.00-150.00  140
  5  ω    -92.00 -22.00   0.50    5.73    --  -25.54 -38.00 -60.00  140
  6  ω    -89.00 -14.00   0.50    5.73    --  -25.54 -57.00  90.00  150
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type
'SuperNova, Dual, Cu at home/near, Pilatus 200K'
_diffrn_measurement_method       'ω scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      -0.0433904000
_diffrn_orient_matrix_UB_12      0.0470898000
_diffrn_orient_matrix_UB_13      -0.1078525000
_diffrn_orient_matrix_UB_21      -0.0187158000
_diffrn_orient_matrix_UB_22      0.0804924000
_diffrn_orient_matrix_UB_23      0.0899959000
_diffrn_orient_matrix_UB_31      0.0700919000
_diffrn_orient_matrix_UB_32      0.0508926000
_diffrn_orient_matrix_UB_33      -0.0428774000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0344
_diffrn_reflns_av_unetI/netI     0.0251
_diffrn_reflns_Laue_measured_fraction_full 1.0000
_diffrn_reflns_Laue_measured_fraction_max 0.9295
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_k_min       -10
_diffrn_reflns_limit_l_max       8
_diffrn_reflns_limit_l_min       -7
_diffrn_reflns_number            3682
_diffrn_reflns_point_group_measured_fraction_full 1.0000
_diffrn_reflns_point_group_measured_fraction_max 0.9295
_diffrn_reflns_theta_full        25.2417
_diffrn_reflns_theta_max         38.09
_diffrn_reflns_theta_min         4.86
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    8.637
_exptl_absorpt_correction_T_max  0.785
_exptl_absorpt_correction_T_min  0.524
_exptl_absorpt_correction_type   gaussian
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.41.116a (Rigaku Oxford Diffraction, 2021)
Numerical absorption correction based on gaussian integration over
a multifaceted crystal model
Empirical absorption correction using spherical harmonics,
implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            'clear colourless'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    3.918
_exptl_crystal_description       prism
_exptl_crystal_F_000             310.162
_exptl_crystal_size_max          0.09
_exptl_crystal_size_mid          0.05
_exptl_crystal_size_min          0.04
_refine_diff_density_max         0.6089
_refine_diff_density_min         -1.0296
_refine_diff_density_rms         0.1972
_refine_ls_d_res_high            0.5760
_refine_ls_d_res_low             4.1979
_refine_ls_goodness_of_fit_ref   1.0215
_refine_ls_hydrogen_treatment    undef
_refine_ls_matrix_type           full
_refine_ls_number_constraints    0
_refine_ls_number_parameters     34
_refine_ls_number_reflns         738
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.0215
_refine_ls_R_factor_all          0.0235
_refine_ls_R_factor_gt           0.0205
_refine_ls_shift/su_max          -0.0002
_refine_ls_shift/su_mean         0.0000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[σ²(Fo²)+(0.0296P)²+0.0357P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0520
_refine_ls_wR_factor_ref         0.0535
_reflns_Friedel_coverage         0.0
_reflns_limit_h_max              14
_reflns_limit_h_min              0
_reflns_limit_k_max              11
_reflns_limit_k_min              0
_reflns_limit_l_max              8
_reflns_limit_l_min              0
_reflns_number_gt                653
_reflns_number_total             738
_reflns_threshold_expression     I>=2u(I)
_cod_data_source_file            d2nj00169a2.cif
_cod_data_source_block           RB21097if
_cod_depositor_comments
'Adding full bibliography for 7061267--7061270.cif.'
_cod_database_code               7061269
_chemical_oxdiff_formula         'Cu S O4'
_chemical_oxdiff_usercomment
'Small  prism grown from (NH4)2SO4/H2SO4 X = 0.2'
_olex2_refinement_description
;
1. Rigid body (RIGU) restrains
 All non-hydrogen atoms
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
;
_olex2_submission_special_instructions 'No special instructions were received'
_oxdiff_exptl_absorpt_empirical_details
;
Empirical correction (ABSPACK) includes:
- Absorption correction using spherical harmonics
- Frame scaling
;
_oxdiff_exptl_absorpt_empirical_full_max 1.283
_oxdiff_exptl_absorpt_empirical_full_min 0.853
loop_
_space_group_symop_id
_space_group_symop_operation_xyz
1 x,y,z
2 x+1/2,-y+1/2,-z+1/2
3 -x,y+1/2,-z
4 -x+1/2,-y,z+1/2
5 -x,-y,-z
6 -x-1/2,y-1/2,z-1/2
7 x,-y-1/2,z
8 x-1/2,y,-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_site_symmetry_order
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
Cu Cu 0.0 0.0 0.0 0.00364(7) Uani 1.000000 2 S TU P
S S 0.18370(5) 0.25 0.45155(8) 0.00240(8) Uani 1.000000 2 S TU P
O1 O 0.13062(14) 0.25 0.7388(2) 0.0052(2) Uani 1.000000 2 S TU P
O2 O 0.36421(14) 0.25 0.4379(3) 0.0041(2) Uani 1.000000 2 S TU P
O3 O 0.13217(9) 0.06669(12) 0.31105(18) 0.00494(15) Uani 1.000000 1 . U .
loop_
_atom_type_symbol
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
_atom_type_scat_dispersion_source
Cu 0.34125 1.28947 'NoSpherA2: Chem.Sci. 2021, DOI:10.1039/D0SC05526C'
'Henke, Gullikson and Davis, At. Data and Nucl. Data Tables, 1993, 54, 2'
O 0.01158 0.00611 'NoSpherA2: Chem.Sci. 2021, DOI:10.1039/D0SC05526C'
'Henke, Gullikson and Davis, At. Data and Nucl. Data Tables, 1993, 54, 2'
S 0.12424 0.12443 'NoSpherA2: Chem.Sci. 2021, DOI:10.1039/D0SC05526C'
'Henke, Gullikson and Davis, At. Data and Nucl. Data Tables, 1993, 54, 2'
loop_
_exptl_crystal_face_index_h
_exptl_crystal_face_index_k
_exptl_crystal_face_index_l
_exptl_crystal_face_perp_dist
0 1 0 0.0355
0 -1 0 0.0505
-1 0 -1 0.0169
1 0 1 0.0201
1 0 -1 0.0170
-1 0 1 0.0233
1 0 0 0.0215
-1 0 0 0.0208
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
O1 Cu O1 180.0 3_546 1_554 ?
O2 Cu O1 76.13(3) 2_455 1_554 ?
O2 Cu O1 103.87(3) 2_455 3_546 ?
O2 Cu O1 103.87(3) 4_554 1_554 ?
O2 Cu O1 76.13(3) 4_554 3_546 ?
O2 Cu O2 180.0 4_554 2_455 ?
O3 Cu O1 90.84(4) . 3_546 ?
O3 Cu O1 89.16(4) . 1_554 ?
O3 Cu O1 89.16(4) 5 3_546 ?
O3 Cu O1 90.84(4) 5 1_554 ?
O3 Cu O2 88.95(4) 5 2_455 ?
O3 Cu O2 91.05(4) . 2_455 ?
O3 Cu O2 88.95(4) . 4_554 ?
O3 Cu O2 91.05(4) 5 4_554 ?
O3 Cu O3 180.0 5 . ?
O2 S O1 110.31(7) . . ?
O3 S O1 110.52(4) . . ?
O3 S O1 110.52(4) 7_565 . ?
O3 S O2 105.96(4) 7_565 . ?
O3 S O2 105.96(4) . . ?
O3 S O3 113.36(7) 7_565 . ?
Cu O1 Cu 89.93(4) 3_556 1_556 ?
S O1 Cu 130.57(3) . 1_556 ?
S O1 Cu 130.57(3) . 3_556 ?
Cu O2 Cu 109.53(5) 4 2 ?
S O2 Cu 123.44(3) . 2 ?
S O2 Cu 123.44(3) . 4 ?
S O3 Cu 136.63(5) . . ?
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
Cu O1 2.3618(8) 3_546 ?
Cu O1 2.3618(8) 1_554 ?
Cu O2 2.0433(7) 2_455 ?
Cu O2 2.0433(7) 4_554 ?
Cu O3 1.9194(8) 5 ?
Cu O3 1.9194(8) . ?
S O1 1.4563(12) . ?
S O2 1.5170(12) . ?
S O3 1.4645(8) . ?
S O3 1.4645(8) 7_565 ?
loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
Cu O1 S O2 -111.52(7) 1_556 . . . ?
Cu O1 S O2 111.52(7) 3_556 . . . ?
Cu O1 S O3 131.63(7) 1_556 . . 7_565 ?
Cu O1 S O3 5.32(9) 1_556 . . . ?
Cu O1 S O3 -131.63(7) 3_556 . . . ?
Cu O1 S O3 -5.32(9) 3_556 . . 7_565 ?
Cu O2 S O1 -78.18(7) 2 . . . ?
Cu O2 S O1 78.18(7) 4 . . . ?
Cu O2 S O3 41.46(9) 2 . . 7_565 ?
Cu O2 S O3 -41.46(9) 4 . . . ?
Cu O2 S O3 162.18(7) 2 . . . ?
Cu O2 S O3 -162.18(7) 4 . . 7_565 ?
Cu O3 S O1 119.13(8) . . . . ?
Cu O3 S O1 119.13(8) 5 . . . ?
Cu O3 S O2 -121.37(8) 5 . . . ?
Cu O3 S O2 -121.37(8) . . . . ?
Cu O3 S O3 -5.57(5) 5 . . 7_565 ?
Cu O3 S O3 -5.57(5) . . . 7_565 ?
loop_
_exptl_oxdiff_crystal_face_indexfrac_h
_exptl_oxdiff_crystal_face_indexfrac_k
_exptl_oxdiff_crystal_face_indexfrac_l
_exptl_oxdiff_crystal_face_x
_exptl_oxdiff_crystal_face_y
_exptl_oxdiff_crystal_face_z
-0.0019 0.9994 -0.0004 0.0472 0.0804 0.0507
0.0019 -0.9994 0.0004 -0.0472 -0.0804 -0.0507
-0.9984 -0.0013 -0.9991 0.1510 -0.0713 -0.0272
0.9984 0.0013 0.9991 -0.1510 0.0713 0.0272
0.9995 -0.0005 -0.9976 0.0642 -0.1085 0.1128
-0.9995 0.0005 0.9976 -0.0642 0.1085 -0.1128
0.9990 0.0004 0.0007 -0.0434 -0.0186 0.0700
-0.9990 -0.0004 -0.0007 0.0434 0.0186 -0.0700
