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
Ibrahim, Mukaila A.; Boeré, René T.; New Journal of Chemistry 46 (2022) 5479–5488; doi:10.1039/D2NJ00169A

data_7061268
_publ_section_title
;
 The copper sulfate hydration cycle. Crystal structures of CuSO4
 (Chalcocyanite), CuSO4&#x00B7;H2O (Poitevinite), CuSO4&#x00B7;3H2O
 (Bonattite) and CuSO4&#x00B7;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 H2 O5 S'
_chemical_formula_sum            'Cu H2 O5 S'
_chemical_formula_weight         177.625
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_symmetry_Int_Tables_number      2
_atom_sites_solution_primary     dual
_audit_creation_date             2022-01-28
_audit_creation_method
;
Olex2 1.5
(compiled 2021.12.09 svn.r5202d8cf for OlexSys, GUI svn.r6439)
;
_audit_update_record
;
2022-01-28 deposited with the CCDC.	2022-02-02 downloaded from the CCDC.
;
_cell_angle_alpha                108.592(12)
_cell_angle_beta                 108.382(12)
_cell_angle_gamma                91.359(10)
_cell_formula_units_Z            2
_cell_length_a                   5.0281(5)
_cell_length_b                   5.1502(5)
_cell_length_c                   7.5607(9)
_cell_measurement_reflns_used    2958
_cell_measurement_temperature    100.01(10)
_cell_measurement_theta_max      79.9930
_cell_measurement_theta_min      9.1490
_cell_volume                     174.41(4)
_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    'SHELXT 2018/2 (Sheldrick, 2018)'
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      100.01(10)
_diffrn_detector                 'Hybrid Pixel Array Detector'
_diffrn_detector_area_resol_mean 5.8140
_diffrn_detector_type            'Pilatus 200K'
_diffrn_measured_fraction_theta_full 0.9857
_diffrn_measured_fraction_theta_max 0.9690
_diffrn_measurement_details
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  t~exp~   \w     \q     \k     \f   Frames
  1  \w   -102.00 -20.00   0.50    0.50    --  -38.50 -70.00 -29.11  164
  2  \w    -50.00  25.00   0.50    0.50    --  -38.50  57.00-120.00  150
  3  \w    -50.00  25.00   0.50    0.50    --  -38.50  57.00 120.00  150
  4  \w     27.00  99.00   0.50    0.50    --   47.56-125.00  30.00  144
  5  \w     36.00 111.00   0.50    0.50    --   47.56  57.00   0.00  150
  6  \w     47.00 117.00   0.50    0.50    --  111.00 -50.00  30.00  140
  7  \w     41.00 109.00   0.50    0.50    --  111.00-111.00 120.00  136
  8  \w    107.00 178.00   0.50    0.50    --  111.00  25.00  30.00  142
  9  \w     41.00 109.00   0.50    0.50    --  111.00-111.00-120.00  136
 10  \w    103.00 176.00   0.50    0.50    --  111.00  77.00 -30.00  146
 11  \w    105.00 175.00   0.50    0.50    --  111.00  50.00-120.00  140
 12  \w     41.00 107.00   0.50    0.50    --  111.00 -91.00 -90.00  132
 13  \w    103.00 176.00   0.50    0.50    --  111.00  77.00 -60.00  146
 14  \w     41.00 109.00   0.50    0.50    --  111.00-111.00 -90.00  136
 15  \w     41.00 107.00   0.50    0.50    --  111.00 -91.00 -30.00  132
 16  \w     41.00 107.00   0.50    0.50    --  111.00 -91.00 150.00  132
 17  \w    105.00 175.00   0.50    0.50    --  111.00  50.00   0.00  140
 18  \w    107.00 177.00   0.50    0.50    --  111.00  38.00  30.00  140
 19  \w    107.00 177.00   0.50    0.50    --  111.00  38.00  60.00  140
 20  \w     41.00 107.00   0.50    0.50    --  111.00 -91.00 -60.00  132
 21  \w     41.00 107.00   0.50    0.50    --  111.00 -91.00  30.00  132
 22  \w    107.00 177.00   0.50    0.50    --  111.00  38.00 -90.00  140
 23  \w     61.00 146.00   0.50    0.50    --  111.00 178.00 -90.00  170
 24  \w    107.00 178.00   0.50    0.50    --  111.00  25.00  90.00  142
 25  \w     46.00 134.00   0.50    0.50    --  111.00 -77.00-180.00  176
 26  \w     47.00 117.00   0.50    0.50    --  111.00 -50.00 -60.00  140
 27  \w     46.00 134.00   0.50    0.50    --  111.00 -77.00 -60.00  176
 28  \w     41.00 107.00   0.50    0.50    --  111.00 -91.00  90.00  132
 29  \w     45.00 115.00   0.50    0.50    --  111.00 -38.00-124.90  140
 30  \w   -102.00 -27.00   0.50    0.50    --  -38.50 -57.00-120.00  150
 31  \w   -102.00 -20.00   0.50    0.50    --  -38.50 -71.00-122.76  164
 32  \w     36.00 111.00   0.50    0.50    --   47.56  57.00 120.00  150
 33  \w     36.00 111.00   0.50    0.50    --   47.56  57.00  60.00  150
 34  \w     36.00 111.00   0.50    0.50    --   47.56  57.00-150.00  150
 35  \w     36.00 111.00   0.50    0.50    --   47.56  57.00 150.00  150
 36  \w     42.00 117.00   0.50    0.50    --   47.56  19.00-120.00  150
 37  \w    105.00 175.00   0.50    0.50    --  111.00  50.00 120.00  140
 38  \w     41.00 115.00   0.50    0.50    --  111.00 -25.00 -60.00  148
 39  \w    107.00 177.00   0.50    0.50    --  111.00  38.00 150.00  140
 40  \w    105.00 175.00   0.50    0.50    --  111.00  50.00 -60.00  140
 41  \w    107.00 177.00   0.50    0.50    --  111.00  38.00-150.00  140
 42  \w    107.00 178.00   0.50    0.50    --  111.00  25.00 120.00  142
 43  \w     99.00 174.00   0.50    0.50    --  111.00  57.00 -77.00  150
 44  \w     96.00 174.00   0.50    0.50    --  111.00  63.00 -30.00  156
 45  \w     96.00 174.00   0.50    0.50    --  111.00  63.00-150.00  156
 46  \w     96.00 174.00   0.50    0.50    --  111.00  63.00  30.00  156
 47  \w    107.00 178.00   0.50    0.50    --  111.00  25.00-180.00  142
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type
'SuperNova, Dual, Cu at home/near, Pilatus 200K'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      0.0717360000
_diffrn_orient_matrix_UB_12      0.1446468000
_diffrn_orient_matrix_UB_13      -0.1321430000
_diffrn_orient_matrix_UB_21      0.1502716000
_diffrn_orient_matrix_UB_22      -0.2442468000
_diffrn_orient_matrix_UB_23      -0.0812762000
_diffrn_orient_matrix_UB_31      -0.2802666000
_diffrn_orient_matrix_UB_32      -0.1446397000
_diffrn_orient_matrix_UB_33      -0.1679531000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Cu K\a'
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0399
_diffrn_reflns_av_unetI/netI     0.0243
_diffrn_reflns_Laue_measured_fraction_full 0.9857
_diffrn_reflns_Laue_measured_fraction_max 0.9690
_diffrn_reflns_limit_h_max       6
_diffrn_reflns_limit_h_min       -6
_diffrn_reflns_limit_k_max       6
_diffrn_reflns_limit_k_min       -6
_diffrn_reflns_limit_l_max       9
_diffrn_reflns_limit_l_min       -9
_diffrn_reflns_number            3078
_diffrn_reflns_point_group_measured_fraction_full 0.9857
_diffrn_reflns_point_group_measured_fraction_max 0.9690
_diffrn_reflns_theta_full        67.6840
_diffrn_reflns_theta_max         80.33
_diffrn_reflns_theta_min         6.57
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    13.717
_exptl_absorpt_correction_T_max  0.822
_exptl_absorpt_correction_T_min  0.302
_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 light blue'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   light
_exptl_crystal_colour_primary    blue
_exptl_crystal_density_diffrn    3.382
_exptl_crystal_description       prism
_exptl_crystal_F_000             171.290
_exptl_crystal_size_max          0.14
_exptl_crystal_size_mid          0.06
_exptl_crystal_size_min          0.027
_refine_diff_density_max         2.4945
_refine_diff_density_min         -1.4795
_refine_diff_density_rms         0.4254
_refine_ls_d_res_high            0.7820
_refine_ls_d_res_low             6.7372
_refine_ls_goodness_of_fit_ref   1.0366
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_constraints    2
_refine_ls_number_parameters     73
_refine_ls_number_reflns         751
_refine_ls_number_restraints     32
_refine_ls_restrained_S_all      1.0130
_refine_ls_R_factor_all          0.0759
_refine_ls_R_factor_gt           0.0753
_refine_ls_shift/su_max          0.0001
_refine_ls_shift/su_mean         0.0000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.1207P)^2^+6.9086P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2174
_refine_ls_wR_factor_ref         0.2178
_reflns_Friedel_coverage         0.0
_reflns_limit_h_max              6
_reflns_limit_h_min              -6
_reflns_limit_k_max              6
_reflns_limit_k_min              -6
_reflns_limit_l_max              9
_reflns_limit_l_min              0
_reflns_number_gt                736
_reflns_number_total             751
_reflns_threshold_expression     I>=2u(I)
_cod_data_source_file            d2nj00169a2.cif
_cod_data_source_block           RB21080ai2f
_cod_depositor_comments
'Adding full bibliography for 7061267--7061270.cif.'
_cod_database_code               7061268
_chemical_oxdiff_formula         'Cu H2 O5 S'
_chemical_oxdiff_usercomment     'Prism from H2SO4'
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All O(H,H) groups
2. Restrained distances
 O1-H1a = O1-H1b
 0.989 with sigma of 0.02
3. Uiso/Uaniso restraints and constraints
Uanis(O1) \\sim Ueq, Uanis(O2) \\sim Ueq, Uanis(O5) \\sim Ueq, Uanis(O3) \\sim
Ueq, Uanis(O4) \\sim Ueq: with sigma of 0.05 and sigma for terminal atoms of
0.001
4. Rigid body (RIGU) restrains
 S1, Cu2, Cu1
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
;
_smtbx_masks_void_probe_radius   1.2
_smtbx_masks_void_truncation_radius 1.2
_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 1.403
_oxdiff_exptl_absorpt_empirical_full_min 0.760