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_7061269
_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 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  t~exp~   \w     \q     \k     \f   Frames
  1  \w     37.00  91.00   0.50    5.73    --   22.41-178.00   0.00  108
  2  \w    -44.00  26.00   0.50    5.73    --   22.41 -38.00-180.00  140
  3  \w     39.00  91.00   0.50    5.73    --   22.41 178.00 150.00  104
  4  \w    -92.00 -22.00   0.50    5.73    --  -25.54 -38.00-150.00  140
  5  \w    -92.00 -22.00   0.50    5.73    --  -25.54 -38.00 -60.00  140
  6  \w    -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       '\w 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/[\s^2^(Fo^2^)+(0.0296P)^2^+0.0357P] where P=(Fo^2^+2Fc^2^)/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