Use of a miniature diamond-anvil cell in a joint X-ray and neutron high-pressure study on copper sulfate pentahydrate
Novelli, Giulia; Kamenev, Konstantin V.; Maynard-Casely, Helen E.; Parsons, Simon; McIntyre, Garry J.; IUCrJ 9 (2022) 73–85; doi:10.1107/S2052252521010708

data_1565849
_publ_section_title
;
 Use of a miniature diamond-anvil cell in a joint X-ray and neutron
 high-pressure study on copper sulfate pentahydrate
;
_journal_coeditor_code           FS5200
_journal_issue                   1
_journal_name_full               IUCrJ
_journal_page_first              73
_journal_page_last               85
_journal_paper_doi               10.1107/S2052252521010708
_journal_volume                  9
_journal_year                    2022
_chemical_formula_moiety         'Cu H8 O8 S, H2 O'
_chemical_formula_sum            'Cu H10 O9 S'
_chemical_formula_weight         249.69
_chemical_name_common            'blue vitriol'
_chemical_name_systematic        'copper(II) sulfate pentahydrate'
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_symmetry_cell_setting           triclinic
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_primary     direct
_audit_creation_date             2020-11-17
_audit_creation_method           'CRYSTALS_ver_14.61_build_7089 '
_cell_angle_alpha                77.308(10)
_cell_angle_beta                 82.353(10)
_cell_angle_gamma                72.640(10)
_cell_formula_units_Z            2
_cell_length_a                   5.9523(12)
_cell_length_b                   6.1001(13)
_cell_length_c                   10.6470(7)
_cell_measurement_reflns_used    2520
_cell_measurement_temperature    295(2)
_cell_measurement_theta_max      30.4280
_cell_measurement_theta_min      4.7800
_cell_volume                     359.02(11)
_computing_cell_refinement       'CrysAlisPro 1.171.39.46 (Rigaku OD, 2018)'
_computing_data_collection       'CrysAlisPro 1.171.39.46 (Rigaku OD, 2018)'
_computing_data_reduction        'CrysAlisPro 1.171.39.46 (Rigaku OD, 2018)'
_computing_molecular_graphics    'CAMERON (Watkin et al., 1996)'
_computing_publication_material  'CRYSTALS (Betteridge et al., 2003)'
_computing_structure_refinement  'CRYSTALS (Betteridge et al., 2003)'
_computing_structure_solution
'From ambient pressure coordinates by Varghese & Maslen (1985)'
_diffrn_ambient_environment      air
_diffrn_ambient_pressure         0.71
_diffrn_ambient_temperature      295(2)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 5.2930
_diffrn_detector_type            Atlas
_diffrn_measured_fraction_theta_full 0.272
_diffrn_measured_fraction_theta_max 0.252
_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    -36.00  13.00   1.00   65.00    --    0.39  82.00 151.00   49
  2  \w    -33.00  19.00   1.00   65.00    --    0.39  67.00 -23.00   52
  3  \w    -13.00  36.00   1.00   65.00    --    0.39 -82.00-151.00   49
  4  \w    -13.00  36.00   1.00   65.00    --    0.39 -82.00  29.00   49
  5  \w    -91.00 -18.00   1.00   65.00    --  -45.62 114.00 -45.00   73
  6  \w    -59.00  -6.00   1.00   65.00    --  -45.62 -19.00-120.00   53
  7  \w    -38.00  35.00   1.00   65.00    --  -45.62 -13.00   3.00   73
  8  \w    -53.00 -30.00   1.00   65.00    --  -45.62  57.00 -30.00   23
  9  \w    -65.00  18.00   1.00   65.00    --  -45.62  38.00-180.00   83
 10  \w    -44.00 -17.00   1.00   65.00    --  -45.62 -38.00-150.00   27
 11  \w    -91.00 -18.00   1.00   65.00    --  -45.62 114.00 135.00   73
 12  \w    -34.00  -8.00   1.00   65.00    --  -45.62 -26.00   8.00   26
 13  \w     19.00  68.00   1.00   65.00    --   46.40 -77.00-150.00   49
 14  \w     13.00  38.00   1.00   65.00    --   46.40  13.00  -3.00   25
 15  \w      9.00  34.00   1.00   65.00    --   46.40  26.00  -8.00   25
 16  \w    -25.00   1.00   1.00   65.00    --   46.40  13.00  -3.00   26
 17  \w     37.00  65.00   1.00   65.00    --   46.40 -67.00  23.00   28
 18  \w     -3.00  23.00   1.00   65.00    --   46.40  19.00-180.00   26
 19  \w     15.00  46.00   1.00   65.00    --   46.40 -13.00   3.00   31
 20  \w     27.00  53.00   1.00   65.00    --   46.40 -57.00-150.00   26
 21  \w      9.00  34.00   1.00   65.00    --   46.40  26.00 171.00   25
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at home/near, Atlas'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      0.0754622000
_diffrn_orient_matrix_UB_12      0.0652906000
_diffrn_orient_matrix_UB_13      0.0087202000
_diffrn_orient_matrix_UB_21      -0.0367166000
_diffrn_orient_matrix_UB_22      -0.0129816000
_diffrn_orient_matrix_UB_23      0.0667315000
_diffrn_orient_matrix_UB_31      0.0928854000
_diffrn_orient_matrix_UB_32      -0.1047275000
_diffrn_orient_matrix_UB_33      0.0126033000
_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  0.055
_diffrn_reflns_av_unetI/netI     0.020
_diffrn_reflns_Laue_measured_fraction_full 0.278
_diffrn_reflns_Laue_measured_fraction_max 0.228
_diffrn_reflns_limit_h_max       5
_diffrn_reflns_limit_h_min       -5
_diffrn_reflns_limit_k_max       5
_diffrn_reflns_limit_k_min       -6
_diffrn_reflns_limit_l_max       14
_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_number            3200
_diffrn_reflns_point_group_measured_fraction_full 0.278
_diffrn_reflns_point_group_measured_fraction_max 0.228
_diffrn_reflns_theta_full        25.293
_diffrn_reflns_theta_max         30.474
_diffrn_reflns_theta_min         3.934
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    3.348
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.64608
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.39.46 (Rigaku Oxford Diffraction, 2018)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            blue
_exptl_crystal_density_diffrn    2.310
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       trapezoid
_exptl_crystal_F_000             254
_exptl_crystal_size_max          0.40
_exptl_crystal_size_mid          0.22
_exptl_crystal_size_min          0.20
_refine_diff_density_max         0.46
_refine_diff_density_min         -0.56
_refine_ls_extinction_coef       176.619
_refine_ls_extinction_method     'Larson (1970), Equation 22'
_refine_ls_goodness_of_fit_ref   0.9980
_refine_ls_hydrogen_treatment    noref
_refine_ls_matrix_type           full
_refine_ls_number_parameters     58
_refine_ls_number_reflns         532
_refine_ls_number_restraints     0
_refine_ls_shift/su_max          0.0000821
_refine_ls_shift/su_mean         0.0000195
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
;
 Method= Modified Sheldrick 
 w=1/[\s^2^(F^2^) + ( 0.03P)^2^ + 0.00P] 
 ,where P=(max(Fo^2^,0) + 2Fc^2^)/3 
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_ref         0.1599
_reflns_limit_h_max              5
_reflns_limit_h_min              -5
_reflns_limit_k_max              6
_reflns_limit_k_min              -6
_reflns_limit_l_max              14
_reflns_limit_l_min              0
_reflns_number_total             552
_oxford_refine_ls_r_factor_ref   0.0620
_oxford_refine_ls_scale          16(4)
_cod_data_source_file            fs5200.cif
_cod_data_source_block           Xcuso4h2o_0.71GPa
_cod_depositor_comments
;
The following automatic conversions were performed:

data item '_exptl_crystal_density_meas' value 'not measured' was
changed to '?' -- the value is perceived as not measured.

Automatic conversion script
Id: cif_fix_values 7556 2019-12-06 15:28:31Z antanas 
;
_cod_database_code               1565849
_exptl_absorpt_empirical_full_min 0.674
_exptl_absorpt_empirical_full_max 2.634
_exptl_absorpt_empirical_details
;
Empirical correction (ABSPACK) includes:
- Absorption correction using spherical harmonics
- Frame scaling
;
_diffrn_oxdiff_ac3_digest_frames
;
01f3ad9c1d15e41c11dfaabe8381b80aac00929d7b1
;
_diffrn_oxdiff_ac3_digest_hkl
;
012a6099d3d3b5233bbe4c3e629129063bcfd8
;
_reflns_odcompleteness_completeness 29.00
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     26.32
_diffrn_wilson_b_factor          0.73
_diffrn_wilson_scale             0.01
_refine_reflns_threshold_expression_ref I>-3.0\s(I)