#------------------------------------------------------------------------------
#$Date: 2022-01-01 07:07:36 +0200 (Sat, 01 Jan 2022) $
#$Revision: 271674 $
#$URL: file:///home/coder/svn-repositories/cod/cif/1/56/58/1565850.cif $
#------------------------------------------------------------------------------
#
# This file is available in the Crystallography Open Database (COD),
# http://www.crystallography.net/. The original data for this entry
# were provided by IUCr Journals, http://journals.iucr.org/.
#
# The file may be used within the scientific community so long as
# proper attribution is given to the journal article from which the
# data were obtained.
#
data_1565850
loop_
_publ_author_name
'Novelli, Giulia'
'Kamenev, Konstantin V.'
'Maynard-Casely, Helen E.'
'Parsons, Simon'
'McIntyre, Garry J.'
_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/[σ²(F²) + ( 0.03P)² + 0.00P] 
 ,where P=(max(Fo²,0) + 2Fc²)/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)
loop_
_symmetry_equiv_pos_as_xyz
x,y,z
-x,-y,-z
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_occupancy
_atom_site_adp_type
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
_atom_site_attached_hydrogens
Cu1 Cu 0.5000 1.0000 0.5000 0.0177 1.0000 Uani S . . . . .
Cu2 Cu 0.5000 0.5000 1.0000 0.0202 1.0000 Uani S . . . . .
S1 S 0.131(2) 0.988(2) 0.7870(11) 0.0274 1.0000 Uani . . . . . .
O1 O 0.3483(14) 0.8089(16) 0.4305(10) 0.0293 1.0000 Uani . . . . . .
O2 O 0.6481(15) 0.7113(13) 0.6186(9) 0.0288 1.0000 Uani . . . . . .
O3 O 0.1725(11) 1.0904(11) 0.6524(6) 0.0264 1.0000 Uani . . . . . .
O4 O 0.1343(10) 1.1445(11) 0.8714(6) 0.0289 1.0000 Uani . . . . . .
O5 O -0.1179(10) 0.9525(11) 0.8037(6) 0.0277 1.0000 Uani . . . . . .
O6 O 0.2961(11) 0.7505(11) 0.8192(6) 0.0282 1.0000 Uani . . . . . .
O7 O 0.7965(13) 0.5347(15) 0.9056(7) 0.0313 1.0000 Uani . . . . . .
O8 O 0.5191(14) 0.2434(12) 0.9154(7) 0.0331 1.0000 Uani . . . . . .
O9 O 1.1300(11) 0.5663(13) 0.6221(7) 0.0270 1.0000 Uani . . . . . .
H11 H 0.245(2) 0.902(3) 0.3537(15) 0.0528 1.0000 Uani . . . . . .
H12 H 0.284(3) 0.719(3) 0.4865(15) 0.0520 1.0000 Uani . . . . . .
H21 H 0.577(3) 0.694(3) 0.6987(16) 0.0471 1.0000 Uani . . . . . .
H22 H 0.8244(19) 0.666(2) 0.6228(12) 0.0400 1.0000 Uani . . . . . .
H71 H 0.928(2) 0.396(3) 0.8942(14) 0.0528 1.0000 Uani . . . . . .
H72 H 0.837(2) 0.679(2) 0.8768(11) 0.0414 1.0000 Uani . . . . . .
H81 H 0.391(2) 0.1974(19) 0.8995(13) 0.0499 1.0000 Uani . . . . . .
H82 H 0.669(2) 0.140(2) 0.8828(13) 0.0444 1.0000 Uani . . . . . .
H91 H 1.172(2) 0.393(3) 0.6317(11) 0.0439 1.0000 Uani . . . . . .
H92 H 1.204(3) 0.591(2) 0.6954(14) 0.0643 1.0000 Uani . . . . . .
loop_
_atom_type_symbol
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_Cromer_Mann_a1
_atom_type_scat_Cromer_Mann_b1
_atom_type_scat_Cromer_Mann_a2
_atom_type_scat_Cromer_Mann_b2
_atom_type_scat_Cromer_Mann_a3
_atom_type_scat_Cromer_Mann_b3
_atom_type_scat_Cromer_Mann_a4
_atom_type_scat_Cromer_Mann_b4
_atom_type_scat_Cromer_Mann_c
_atom_type_scat_source
H 0.0000 0.0000 0.0000 0.0000 0.0000 0.0000 0.0000 0.0000 0.0000 0.0000 -3.7409
'International Tables Vol C 4.2.6.8 and 6.1.1.4'
Cu 0.2873 1.4974 0.0000 0.0000 0.0000 0.0000 0.0000 0.0000 0.0000 0.0000 7.7180
'International Tables Vol C 4.2.6.8 and 6.1.1.4'
O 0.0134 0.0075 0.0000 0.0000 0.0000 0.0000 0.0000 0.0000 0.0000 0.0000 5.8050
'International Tables Vol C 4.2.6.8 and 6.1.1.4'
S 0.1445 0.1499 0.0000 0.0000 0.0000 0.0000 0.0000 0.0000 0.0000 0.0000 2.8470
'International Tables Vol C 4.2.6.8 and 6.1.1.4'
loop_
_geom_angle_atom_site_label_1
_geom_angle_site_symmetry_1
_geom_angle_atom_site_label_2
_geom_angle_site_symmetry_2
_geom_angle_atom_site_label_3
_geom_angle_site_symmetry_3
_geom_angle
_geom_angle_publ_flag
O3 2_676 Cu1 . O1 2_676 90.7(3) yes
O3 2_676 Cu1 . O2 2_676 91.0(3) yes
O1 2_676 Cu1 . O2 2_676 86.8(3) yes
O3 2_676 Cu1 . O1 . 89.3(3) yes
O1 2_676 Cu1 . O1 . 179.99 yes
O2 2_676 Cu1 . O1 . 93.2(3) yes
O3 2_676 Cu1 . O2 . 89.0(3) yes
O1 2_676 Cu1 . O2 . 93.2(3) yes
O2 2_676 Cu1 . O2 . 179.99 yes
O1 . Cu1 . O2 . 86.8(3) yes
O3 2_676 Cu1 . O3 . 180.00 yes
O1 2_676 Cu1 . O3 . 89.3(3) yes
O2 2_676 Cu1 . O3 . 89.0(3) yes
O1 . Cu1 . O3 . 90.7(3) yes
O2 . Cu1 . O3 . 91.0(3) yes
O6 2_667 Cu2 . O7 2_667 88.4(3) yes
O6 2_667 Cu2 . O8 2_667 86.3(3) yes
O7 2_667 Cu2 . O8 2_667 89.5(3) yes
O6 2_667 Cu2 . O6 . 180.00 yes
O7 2_667 Cu2 . O6 . 91.6(3) yes
O8 2_667 Cu2 . O6 . 93.7(3) yes
O6 2_667 Cu2 . O7 . 91.6(3) yes
O7 2_667 Cu2 . O7 . 179.99 yes
O8 2_667 Cu2 . O7 . 90.5(3) yes
O6 . Cu2 . O7 . 88.4(3) yes
O6 2_667 Cu2 . O8 . 93.7(3) yes
O7 2_667 Cu2 . O8 . 90.5(3) yes
O8 2_667 Cu2 . O8 . 179.99 yes
O6 . Cu2 . O8 . 86.3(3) yes
O7 . Cu2 . O8 . 89.5(3) yes
O3 . S1 . O4 . 111.2(8) yes
O3 . S1 . O5 . 107.4(7) yes
O4 . S1 . O5 . 107.7(8) yes
O3 . S1 . O6 . 110.3(8) yes
O4 . S1 . O6 . 114.0(9) yes
O5 . S1 . O6 . 105.8(8) yes
Cu1 . O1 . H11 . 114.0(10) no
Cu1 . O1 . H12 . 115.7(9) no
H11 . O1 . H12 . 113.9(13) no
Cu1 . O2 . H21 . 115.1(9) no
Cu1 . O2 . H22 . 118.0(9) no
H21 . O2 . H22 . 110.1(12) no
Cu1 . O3 . S1 . 132.1(6) yes
Cu2 . O6 . S1 . 138.8(6) yes
Cu2 . O7 . H71 . 120.5(10) no
Cu2 . O7 . H72 . 125.5(10) no
H71 . O7 . H72 . 113.5(13) no
Cu2 . O8 . H81 . 125.6(9) no
Cu2 . O8 . H82 . 124.7(9) no
H81 . O8 . H82 . 109.7(11) no
H91 . O9 . H92 . 104.0(11) no
loop_
_geom_bond_atom_site_label_1
_geom_bond_site_symmetry_1
_geom_bond_atom_site_label_2
_geom_bond_site_symmetry_2
_geom_bond_distance
_geom_bond_publ_flag
Cu1 . O3 2_676 2.376(6) yes
Cu1 . O1 2_676 1.977(7) yes
Cu1 . O2 2_676 1.966(8) yes
Cu1 . O1 . 1.977(7) yes
Cu1 . O2 . 1.966(8) yes
Cu1 . O3 . 2.376(6) yes
Cu2 . O6 2_667 2.395(6) yes
Cu2 . O7 2_667 1.956(7) yes
Cu2 . O8 2_667 1.939(7) yes
Cu2 . O6 . 2.395(6) yes
Cu2 . O7 . 1.956(7) yes
Cu2 . O8 . 1.939(7) yes
S1 . O3 . 1.452(13) yes
S1 . O4 . 1.454(13) yes
S1 . O5 . 1.541(13) yes
S1 . O6 . 1.486(13) yes
O1 . H11 . 1.04(2) no
O1 . H12 . 0.85(2) no
O2 . H21 . 0.90(2) no
O2 . H22 . 1.006(16) no
O7 . H71 . 0.984(19) no
O7 . H72 . 0.956(17) no
O8 . H81 . 0.933(17) no
O8 . H82 . 0.994(19) no
O9 . H91 . 0.993(19) no
O9 . H92 . 1.004(18) no
loop_
_oxford_refln_omitted_index_h
_oxford_refln_omitted_index_k
_oxford_refln_omitted_index_l
_oxford_refln_omitted_flag
_oxford_refln_omitted_details
1 7 6 x .
7 1 1 x .
4 -1 6 x .
1 6 5 x .
0 -2 11 x .
1 6 8 x .
4 4 3 x .
4 7 2 x .
3 -4 5 x .
6 1 1 x .
2 3 0 x .
-2 1 7 x .
-5 -3 2 x .
-2 5 3 x .
4 6 9 x .
-6 2 1 x .
3 2 8 x .
-1 5 10 x .
-6 -3 5 x .
1 7 3 x .
6 1 6 x .
-6 -1 3 x .
7 3 0 x .
-1 2 11 x .
1 4 11 x .
2 5 11 x .
2 1 2 x .
1 5 4 x .
-3 0 10 x .
1 -3 9 x .
2 -4 7 x .
-3 2 10 x .
1 -4 8 x .
-1 0 11 x .
-3 5 5 x .
-5 -4 6 x .
3 -5 2 x .
-1 1 12 x .
1 0 12 x .
-5 3 3 x .
-4 1 9 x .
-1 -1 11 x .
-2 5 1 x .
-1 1 11 x .
-5 0 8 x .
7 1 0 x .
1 -1 11 x .
-1 -3 10 x .
3 -4 6 x .
-3 5 2 x .
-3 1 11 x .
4 -4 1 x .
-3 0 11 x .
-2 1 12 x .
3 -3 4 x .
-3 -2 10 x .
-4 2 9 x .
4 -1 10 x .
-5 3 5 x .
3 -1 9 x .
-2 -7 2 x .
3 -5 1 x .
-1 2 8 x .
2 -4 5 x .
1 -2 11 x .
4 -3 6 x .
-2 1 11 x .
-4 4 3 x .
-3 4 8 x .
0 -1 11 x .
-2 -2 11 x .
-2 5 8 x .
1 7 2 x .
1 -4 3 x .
5 3 2 x .
6 5 6 x .
3 4 6 x .
-1 0 9 x .
-3 1 10 x .
1 -6 3 x .
-4 1 8 x .
2 -5 5 x .
-1 -3 9 x .
-6 1 3 x .
-2 6 3 x .
-3 -4 8 x .
-7 -3 1 x .
-3 4 6 x .
-5 2 4 x .
3 -2 10 x .
0 -4 9 x .
-4 3 6 x .
-3 5 4 x .
-2 4 7 x .
-1 -4 9 x .
0 -1 9 x .
-2 0 11 x .
-6 1 4 x .
0 -5 7 x .
-3 1 9 x .
-4 3 4 x .
-3 4 3 x .
4 -3 3 x .
0 -1 12 x .
1 2 2 x .
-3 -4 3 x .
-1 0 7 x .
1 7 1 x .
-1 2 0 x .
3 -4 2 x .
3 5 8 x .
-2 3 2 x .
-1 5 5 x .
6 1 3 x .
0 -5 3 x .
1 2 0 x .
4 5 6 x .
3 -1 8 x .
1 -2 7 x .
1 -4 5 x .
-2 3 6 x .
-1 1 4 x .
3 1 3 x .
-3 2 5 x .
-3 -4 4 x .
0 4 5 x .
2 2 3 x .
-1 -2 2 x .
3 6 5 x .
4 6 1 x .
-1 -2 1 x .
6 1 2 x .
-2 2 5 x .
-3 3 4 x .
-4 -3 3 x .
-1 2 1 x .
-5 -1 5 x .
0 7 4 x .
1 -4 4 x .
5 2 2 x .
1 3 2 x .
-5 -1 3 x .
2 7 7 x .
1 -2 3 x .
-3 3 2 x .
-6 -2 1 x .
3 2 0 x .
3 7 6 x .
0 -3 5 x .
5 5 2 x .
0 -3 7 x .
-4 -2 1 x .
-6 -1 1 x .
3 1 4 x .
-3 -1 3 x .
2 0 3 x .
3 0 1 x .
