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_7061267
_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_absolute_configuration ad
_chemical_formula_moiety         'Cu H6 O7 S'
_chemical_formula_sum            'Cu H6 O7 S'
_chemical_formula_weight         213.655
_space_group_crystal_system      monoclinic
_space_group_IT_number           9
_space_group_name_Hall           'C -2yc'
_space_group_name_H-M_alt        'C 1 c 1'
_symmetry_Int_Tables_number      9
_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                90
_cell_angle_beta                 96.450(3)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   5.5708(2)
_cell_length_b                   12.9751(4)
_cell_length_c                   7.3754(2)
_cell_measurement_reflns_used    10841
_cell_measurement_temperature    100.01(10)
_cell_measurement_theta_max      38.3700
_cell_measurement_theta_min      3.0270
_cell_volume                     529.73(3)
_computing_cell_refinement       'CrysAlisPro 1.171.41.110a (Rigaku OD, 2021)'
_computing_data_collection       'CrysAlisPro 1.171.41.110a (Rigaku OD, 2021)'
_computing_data_reduction        'CrysAlisPro 1.171.41.110a (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 1.0000
_diffrn_measured_fraction_theta_max 0.9639
_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    3.59    --   22.41-178.00-150.00  108
  2  \w     37.00  91.00   0.50    3.59    --   22.41-178.00 -30.00  108
  3  \w    -15.00  58.00   0.50    3.59    --   22.41 -99.00 120.00  146
  4  \w    -37.00  38.00   0.50    3.59    --  -25.54  57.00 -60.00  150
  5  \w    -80.00 -30.00   0.50    3.59    --  -25.54 130.00 113.16  100
  6  \w    -87.00 -36.00   0.50    3.59    --  -25.54 142.00-147.35  102
  7  \w    -14.00  13.00   0.50    3.59    --  -25.54-103.00  42.04   54
  8  \w    -29.00  41.00   0.50    3.59    --  -25.54  38.00  60.00  140
  9  \w    -19.00   9.00   0.50    3.59    --  -25.54 -96.00-108.75   56
 10  \w    -95.00 -20.00   0.50    3.59    --  -25.54 -19.00 -60.00  150
 11  \w    -22.00   7.00   0.50    3.59    --  -25.54 -93.00 -21.65   58
 12  \w    -36.00  -6.00   0.50    3.59    --  -25.54 -73.00 161.82   60
 13  \w    -82.00 -33.00   0.50    3.59    --  -25.54 133.00 -54.40   98
 14  \w    -29.00  41.00   0.50    3.59    --  -25.54  38.00-180.00  140
 15  \w    -92.00 -22.00   0.50    3.59    --  -25.54 -38.00  30.00  140
 16  \w     11.00  85.00   0.50    3.59    --   22.41  57.00 -90.00  148
 17  \w     37.00  91.00   0.50    3.59    --   22.41-178.00  90.00  108
 18  \w     11.00  85.00   0.50    3.59    --   22.41  57.00-150.00  148
 19  \w    -22.00   7.00   0.50    3.59    --  -25.54 -93.00  67.26   58
 20  \w    -89.00 -14.00   0.50    3.59    --  -25.54 -57.00   0.00  150
 21  \w    -14.00  12.00   0.50    3.59    --  -25.54-102.00 -66.73   52
 22  \w    -93.00 -49.00   0.50    3.59    --  -25.54 150.00 129.03   88
 23  \w    -89.00 -14.00   0.50    3.59    --  -25.54 -57.00-120.00  150
 24  \w    -92.00 -22.00   0.50    3.59    --  -25.54 -38.00 120.00  140
;
_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      0.0781743000
_diffrn_orient_matrix_UB_12      -0.0114271000
_diffrn_orient_matrix_UB_13      -0.0668453000
_diffrn_orient_matrix_UB_21      0.0414769000
_diffrn_orient_matrix_UB_22      -0.0445329000
_diffrn_orient_matrix_UB_23      0.0497496000
_diffrn_orient_matrix_UB_31      -0.0927301000
_diffrn_orient_matrix_UB_32      -0.0295665000
_diffrn_orient_matrix_UB_33      -0.0491910000
_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  0.0375
_diffrn_reflns_av_unetI/netI     0.0284
_diffrn_reflns_Laue_measured_fraction_full 1.0000
_diffrn_reflns_Laue_measured_fraction_max 0.9639
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_k_max       21
_diffrn_reflns_limit_k_min       -22
_diffrn_reflns_limit_l_max       12
_diffrn_reflns_limit_l_min       -12
_diffrn_reflns_number            13522
_diffrn_reflns_point_group_measured_fraction_full 1.0000
_diffrn_reflns_point_group_measured_fraction_max 0.9446
_diffrn_reflns_theta_full        25.2417
_diffrn_reflns_theta_max         38.16
_diffrn_reflns_theta_min         3.14
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    4.488
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.95627
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.41.110a (Rigaku Oxford Diffraction, 2021)
Empirical absorption correction using spherical harmonics,
implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            'clear grayish blue'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   grayish
_exptl_crystal_colour_primary    blue
_exptl_crystal_density_diffrn    2.679
_exptl_crystal_description       prism
_exptl_crystal_F_000             430.301
_exptl_crystal_recrystallization_method
'The material was recrystallised from --- by'
_exptl_crystal_size_max          0.101
_exptl_crystal_size_mid          0.07
_exptl_crystal_size_min          0.057
_refine_diff_density_max         0.3868
_refine_diff_density_min         -0.8111
_refine_diff_density_rms         0.1105
_refine_ls_abs_structure_details
'Hooft, R.W.W., Straver, L.H., Spek, A.L. (2010). J. Appl. Cryst., 43, 665-668.'
_refine_ls_abs_structure_Flack   0.001(4)
_refine_ls_d_res_high            0.5752
_refine_ls_d_res_low             6.4875
_refine_ls_goodness_of_fit_ref   1.0125
_refine_ls_hydrogen_treatment    refall
_refine_ls_matrix_type           full
_refine_ls_number_constraints    0
_refine_ls_number_parameters     136
_refine_ls_number_reflns         2761
_refine_ls_number_restraints     128
_refine_ls_restrained_S_all      0.9891
_refine_ls_R_factor_all          0.0194
_refine_ls_R_factor_gt           0.0188
_refine_ls_shift/su_max          -0.0009
_refine_ls_shift/su_mean         0.0000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0228P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0424
_refine_ls_wR_factor_ref         0.0429
_reflns_Friedel_coverage         0.925
_reflns_limit_h_max              9
_reflns_limit_h_min              -9
_reflns_limit_k_max              22
_reflns_limit_k_min              -22
_reflns_limit_l_max              12
_reflns_limit_l_min              -12
_reflns_number_gt                2715
_reflns_number_total             2761
_reflns_threshold_expression     I>=2u(I)
_cod_data_source_file            d2nj00169a2.cif
_cod_data_source_block           RB21092_auto
_cod_depositor_comments
'Adding full bibliography for 7061267--7061270.cif.'
_cod_original_sg_symbol_Hall     ' C -2yc'
_cod_database_code               7061267
_chemical_oxdiff_formula         'Cu S O7 H6'
_chemical_oxdiff_usercomment
'Smaller Xtal - small block cut from larger crystals'
_olex2_refinement_description
;
1. Restrained distances
 O6-H6b = O6-H6a = O5-H5a = O5-H5b = O7-H7b = O7-H7a
 0.989 with sigma of 0.02
2. Uiso/Uaniso restraints and constraints
Uanis(H7b) \\sim Ueq, Uanis(H6a) \\sim Ueq: with sigma of 0.01 and sigma for
terminal atoms of 0.02
3. Rigid body (RIGU) restrains
 Cu1, O1, O1, O1, O2, O2, O2, O3, O3, O3, O4, O4, O4, O5, H5a, H5b, O6, H6a,
 H6b, O7, H7a, H7b, S1, S1, S1
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 H7b, H6b, H5b, H5a
 with sigma for 1-2 distances of 0.001 and sigma for 1-3 distances of 0.001
;
_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 1.083
_oxdiff_exptl_absorpt_empirical_full_min 0.947