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_1565850
_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_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_hydrogens   difmap
_atom_sites_solution_primary     other
_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    2094
_cell_measurement_temperature    295(2)
_cell_measurement_theta_max      20
_cell_measurement_theta_min      3
_cell_volume                     359.02(11)
_computing_cell_refinement       'LaueG (Piltz, 2011)'
_computing_data_collection       'MAATEL/ANSTO control program'
_computing_data_reduction
'argonne_boxes (Wilkinson et al., 1988) & LaueG (Piltz, 2011)'
_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 X-ray diffraction experiment'
_diffrn_ambient_pressure         0.71
_diffrn_ambient_temperature      295(2)
_diffrn_measured_fraction_theta_full 0.827
_diffrn_measured_fraction_theta_max 0.827
_diffrn_measurement_device       'Laue image-plate diffractometer'
_diffrn_measurement_device_type  KOALA
_diffrn_measurement_method       Laue
_diffrn_radiation_probe          neutron
_diffrn_radiation_type           neutron
_diffrn_radiation_wavelength     0.78
_diffrn_reflns_av_R_equivalents  0.2916
_diffrn_reflns_av_unetI/netI     0.2094
_diffrn_reflns_limit_h_max       7
_diffrn_reflns_limit_h_min       -7
_diffrn_reflns_limit_k_max       7
_diffrn_reflns_limit_k_min       -7
_diffrn_reflns_limit_l_max       13
_diffrn_reflns_limit_l_min       -13
_diffrn_reflns_number            9163
_diffrn_reflns_reduction_process 'LaueG (Piltz, 2011)'
_diffrn_reflns_resolution_max    1.25
_diffrn_reflns_theta_full        27.598
_diffrn_reflns_theta_max         28.748
_diffrn_reflns_theta_min         2.158
_diffrn_source                   'nuclear reactor'
_diffrn_source_details           'thermal neutrons, supermirror guides'
_diffrn_source_type
'OPAL reactor, ANSTO, Lucas Heights, Australia'
_exptl_absorpt_coefficient_mu    0.0
_exptl_absorpt_correction_type   none
_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             50
_exptl_crystal_size_max          0.40
_exptl_crystal_size_mid          0.22
_exptl_crystal_size_min          0.20
_refine_diff_density_max         2.69
_refine_diff_density_min         -2.65
_refine_ls_abs_structure_details
;
Absolute structure known from synthesis
;
_refine_ls_extinction_method     None
_refine_ls_goodness_of_fit_ref   0.9999
_refine_ls_hydrogen_treatment    refall
_refine_ls_matrix_type           full
_refine_ls_number_parameters     193
_refine_ls_number_reflns         990
_refine_ls_number_restraints     0
_refine_ls_shift/su_max          0.0000536
_refine_ls_shift/su_mean         0.0000109
_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         0.1651
_reflns_number_total             1147
_oxford_refine_ls_r_factor_ref   0.2398
_oxford_refine_ls_scale          1.51(4)
_cod_data_source_file            fs5200.cif
_cod_data_source_block           Ncuso4h2o_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               1565850
_diffrn_wilson_b_factor          0.31
_diffrn_wilson_scale             7.46
_refine_reflns_threshold_expression_ref I>-3.0\s(I)