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_7061270
_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 H8 O8 S, H2 O'
_chemical_formula_sum            'Cu H10 O9 S'
_chemical_formula_weight         249.686
_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             2022-01-08
_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                77.224(3)
_cell_angle_beta                 82.387(2)
_cell_angle_gamma                72.434(3)
_cell_formula_units_Z            2
_cell_length_a                   5.9676(2)
_cell_length_b                   6.0957(2)
_cell_length_c                   10.6366(3)
_cell_measurement_reflns_used    10138
_cell_measurement_temperature    100.00(10)
_cell_measurement_theta_max      38.2480
_cell_measurement_theta_min      3.5350
_cell_volume                     358.85(2)
_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      100.00(10)
_diffrn_detector                 'Hybrid Pixel Array Detector'
_diffrn_detector_area_resol_mean 5.8140
_diffrn_detector_type            'Pilatus 200K'
_diffrn_measured_fraction_theta_full 0.9992
_diffrn_measured_fraction_theta_max 0.9344
_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     37.00  91.00   0.50    0.66    --   22.41-178.00   0.00  108
  2  \w     39.00  91.00   0.50    0.66    --   22.41 178.00  60.00  104
  3  \w    -29.00  41.00   0.50    0.66    --  -25.54  38.00  90.00  140
  4  \w    -77.00 -27.00   0.50    0.66    --  -25.54 125.00 -92.32  100
  5  \w    -36.00  -6.00   0.50    0.66    --  -25.54 -73.00  21.11   60
  6  \w    -95.00  44.00   0.50    0.66    --  -25.54   0.00 -90.00  278
  7  \w    -89.00 -37.00   0.50    0.66    --  -25.54 145.00  66.26  104
  8  \w    -37.00  38.00   0.50    0.66    --  -25.54  57.00  30.00  150
  9  \w    -23.00   7.00   0.50    0.66    --  -25.54 -92.00 -52.16   60
 10  \w    -14.00  13.00   0.50    0.66    --  -25.54-104.00-178.69   54
 11  \w    -81.00 -30.00   0.50    0.66    --  -25.54 132.00 107.74  102
 12  \w    -24.00   6.00   0.50    0.66    --  -25.54 -91.00-168.86   60
 13  \w    -95.00  44.00   0.50    0.66    --  -25.54   0.00 -90.00  278
 14  \w    -89.00 -14.00   0.50    0.66    --  -25.54 -57.00 120.00  150
 15  \w    -92.00 -22.00   0.50    0.66    --  -25.54 -38.00 -90.00  140
 16  \w    -14.00  13.00   0.50    0.66    --  -25.54-104.00 -16.30   54
 17  \w    -89.00 -14.00   0.50    0.66    --  -25.54 -57.00  60.00  150
 18  \w    -89.00 -14.00   0.50    0.66    --  -25.54 -57.00-180.00  150
 19  \w    -49.00  21.00   0.50    0.66    --  -25.54  77.00-150.00  140
 20  \w    -90.00 -37.00   0.50    0.66    --  -25.54 146.00 -14.46  106
 21  \w    -92.00 -37.00   0.50    0.66    --  -25.54 -38.00-120.00  110
 22  \w    -36.00  -6.00   0.50    0.66    --  -25.54 -72.00-131.33   60
;
_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      0.0261332000
_diffrn_orient_matrix_UB_12      -0.1084481000
_diffrn_orient_matrix_UB_13      -0.0207348000
_diffrn_orient_matrix_UB_21      0.0956846000
_diffrn_orient_matrix_UB_22      -0.0469526000
_diffrn_orient_matrix_UB_23      0.0402417000
_diffrn_orient_matrix_UB_31      -0.0760451000
_diffrn_orient_matrix_UB_32      -0.0387255000
_diffrn_orient_matrix_UB_33      0.0514748000
_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  0.0463
_diffrn_reflns_av_unetI/netI     0.0349
_diffrn_reflns_Laue_measured_fraction_full 0.9992
_diffrn_reflns_Laue_measured_fraction_max 0.9344
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       10
_diffrn_reflns_limit_k_min       -10
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            18712
_diffrn_reflns_point_group_measured_fraction_full 0.9992
_diffrn_reflns_point_group_measured_fraction_max 0.9344
_diffrn_reflns_theta_full        25.2417
_diffrn_reflns_theta_max         38.30
_diffrn_reflns_theta_min         3.57
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    3.350
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.91744
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.41.116a (Rigaku Oxford Diffraction, 2021)
Empirical absorption correction using spherical harmonics,
implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            'clear blue'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_primary    blue
_exptl_crystal_density_diffrn    2.311
_exptl_crystal_description       irregular
_exptl_crystal_F_000             255.197
_exptl_crystal_size_max          0.222
_exptl_crystal_size_mid          0.173
_exptl_crystal_size_min          0.135
_refine_diff_density_max         0.5598
_refine_diff_density_min         -0.6281
_refine_diff_density_rms         0.1423
_refine_ls_d_res_high            0.5734
_refine_ls_d_res_low             5.7037
_refine_ls_goodness_of_fit_ref   1.0757
_refine_ls_hydrogen_treatment    refall
_refine_ls_matrix_type           full
_refine_ls_number_constraints    0
_refine_ls_number_parameters     193
_refine_ls_number_reflns         3729
_refine_ls_number_restraints     70
_refine_ls_restrained_S_all      1.0652
_refine_ls_R_factor_all          0.0290
_refine_ls_R_factor_gt           0.0249
_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^)+(0.0178P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0494
_refine_ls_wR_factor_ref         0.0513
_reflns_Friedel_coverage         0.0
_reflns_limit_h_max              10
_reflns_limit_h_min              -9
_reflns_limit_k_max              10
_reflns_limit_k_min              -10
_reflns_limit_l_max              18
_reflns_limit_l_min              0
_reflns_number_gt                3369
_reflns_number_total             3729
_reflns_threshold_expression     I>=2u(I)
_cod_data_source_file            d2nj00169a2.cif
_cod_data_source_block           RB21086i
_cod_depositor_comments
'Adding full bibliography for 7061267--7061270.cif.'
_cod_database_code               7061270
_chemical_oxdiff_formula         'Cu C O9 H10'
_chemical_oxdiff_usercomment     Mo
_olex2_refinement_description
;
1. Restrained distances
 O5-H5a = O5-H5b = O2-H2a = O2-H2b = O1-H1b = O1-H1a = O4-H4a = O4-H4b = O3-
 H3b = O3-H3a
 0.989 with sigma of 0.02
2. Uiso/Uaniso restraints and constraints
Uanis(H1a) \\sim Ueq, Uanis(H1b) \\sim Ueq, Uanis(H3a) \\sim Ueq, Uanis(H3b)
\\sim Ueq, Uanis(H4a) \\sim Ueq, Uanis(H4b) \\sim Ueq, Uanis(H5a) \\sim Ueq,
Uanis(H5b) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.01
Uanis(H2a) \\sim Ueq, Uanis(H2b) \\sim Ueq: with sigma of 0.005 and sigma for
terminal atoms of 0.005
3. 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 1.104
_oxdiff_exptl_absorpt_empirical_full_min 0.938