#------------------------------------------------------------------------------
#$Date: 2022-01-01 07:07:36 +0200 (Sat, 01 Jan 2022) $
#$Revision: 271674 $
#$URL: file:///home/coder/svn-repositories/cod/cif/1/56/58/1565849.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_1565849
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_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  tₑₓₚ   ω     θ     κ     φ   Frames
--------------------------------------------------------------------------
  1  ω    -36.00  13.00   1.00   65.00    --    0.39  82.00 151.00   49
  2  ω    -33.00  19.00   1.00   65.00    --    0.39  67.00 -23.00   52
  3  ω    -13.00  36.00   1.00   65.00    --    0.39 -82.00-151.00   49
  4  ω    -13.00  36.00   1.00   65.00    --    0.39 -82.00  29.00   49
  5  ω    -91.00 -18.00   1.00   65.00    --  -45.62 114.00 -45.00   73
  6  ω    -59.00  -6.00   1.00   65.00    --  -45.62 -19.00-120.00   53
  7  ω    -38.00  35.00   1.00   65.00    --  -45.62 -13.00   3.00   73
  8  ω    -53.00 -30.00   1.00   65.00    --  -45.62  57.00 -30.00   23
  9  ω    -65.00  18.00   1.00   65.00    --  -45.62  38.00-180.00   83
 10  ω    -44.00 -17.00   1.00   65.00    --  -45.62 -38.00-150.00   27
 11  ω    -91.00 -18.00   1.00   65.00    --  -45.62 114.00 135.00   73
 12  ω    -34.00  -8.00   1.00   65.00    --  -45.62 -26.00   8.00   26
 13  ω     19.00  68.00   1.00   65.00    --   46.40 -77.00-150.00   49
 14  ω     13.00  38.00   1.00   65.00    --   46.40  13.00  -3.00   25
 15  ω      9.00  34.00   1.00   65.00    --   46.40  26.00  -8.00   25
 16  ω    -25.00   1.00   1.00   65.00    --   46.40  13.00  -3.00   26
 17  ω     37.00  65.00   1.00   65.00    --   46.40 -67.00  23.00   28
 18  ω     -3.00  23.00   1.00   65.00    --   46.40  19.00-180.00   26
 19  ω     15.00  46.00   1.00   65.00    --   46.40 -13.00   3.00   31
 20  ω     27.00  53.00   1.00   65.00    --   46.40 -57.00-150.00   26
 21  ω      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       'ω 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/[σ²(F²) + ( 0.03P)² + 0.00P] 
 ,where P=(max(Fo²,0) + 2Fc²)/3 
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_ref         0.1599
_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)
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 0.0393 1.0000 Uani S . . . . .
Cu2 Cu 0.5000 0.5000 1.0000 0.0362 1.0000 Uani S . . . . .
S1 S 0.1248(6) 0.9857(6) 0.78627(14) 0.0337 1.0000 Uani . . . . . .
O1 O 0.359(2) 0.821(2) 0.4267(6) 0.0275(12) 1.0000 Uiso . . . . . .
O3 O 0.1740(17) 1.0940(16) 0.6508(4) 0.0182(10) 1.0000 Uiso . . . . . .
O6 O 0.2983(17) 0.7559(16) 0.8176(4) 0.0215(11) 1.0000 Uiso . . . . . .
O7 O 0.793(2) 0.5286(19) 0.9065(5) 0.0321(13) 1.0000 Uiso . . . . . .
O8 O 0.519(2) 0.245(2) 0.9155(5) 0.0393(15) 1.0000 Uiso . . . . . .
O4 O 0.132(2) 1.136(2) 0.8718(5) 0.0276(12) 1.0000 Uiso . . . . . .
O5 O -0.116(2) 0.9537(18) 0.8018(5) 0.0275(12) 1.0000 Uiso . . . . . .
O2 O 0.6491(16) 0.7084(15) 0.6174(4) 0.0218(11) 1.0000 Uiso . . . . . .
O9 O 1.1356(19) 0.5705(18) 0.6230(5) 0.0292(13) 1.0000 Uiso . . . . . .
H81 H 0.4000 0.2114 0.9020 0.0578 1.0000 Uiso . . . . . .
H82 H 0.6337 0.1542 0.8802 0.0578 1.0000 Uiso . . . . . .
H71 H 0.8980 0.4060 0.8956 0.0476 1.0000 Uiso . . . . . .
H72 H 0.8197 0.6570 0.8747 0.0476 1.0000 Uiso . . . . . .
H11 H 0.2878 0.8877 0.3597 0.0416 1.0000 Uiso . . . . . .
H12 H 0.2907 0.7449 0.4868 0.0416 1.0000 Uiso . . . . . .
H21 H 0.5433 0.7229 0.6779 0.0318 1.0000 Uiso . . . . . .
H22 H 0.7969 0.6666 0.6190 0.0318 1.0000 Uiso . . . . . .
H91 H 1.1470 0.4277 0.6312 0.0438 1.0000 Uiso . . . . . .
H92 H 1.1819 0.6234 0.6781 0.0438 1.0000 Uiso . . . . . .
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 0.4930 10.5109 0.3229 26.1257 0.1402 3.1424 0.0408 57.7998
0.0030 'International Tables Vol C 4.2.6.8 and 6.1.1.4'
O 0.0106 0.0060 3.0485 13.2771 2.2868 5.7011 1.5463 0.3239 0.8670 32.9089 0.2508
'International Tables Vol C 4.2.6.8 and 6.1.1.4'
S 0.1246 0.1234 6.9053 1.4679 5.2034 22.2151 1.4379 0.2536 1.5863 56.1720 0.8669
'International Tables Vol C 4.2.6.8 and 6.1.1.4'
Cu 0.3201 1.2651 13.3380 3.5828 7.1676 0.2470 5.6158 11.3966 1.6735 64.8126
1.1910 '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 . O2 2_676 91.93(19) yes
O3 2_676 Cu1 . O1 2_676 92.8(5) yes
O2 2_676 Cu1 . O1 2_676 87.7(4) yes
O3 2_676 Cu1 . O1 . 87.2(5) yes
O2 2_676 Cu1 . O1 . 92.3(4) yes
O1 2_676 Cu1 . O1 . 179.99 yes
O3 2_676 Cu1 . O3 . 180.00 yes
O2 2_676 Cu1 . O3 . 88.07(19) yes
O1 2_676 Cu1 . O3 . 87.2(5) yes
O1 . Cu1 . O3 . 92.8(5) yes
O3 2_676 Cu1 . O2 . 88.07(19) yes
O2 2_676 Cu1 . O2 . 179.99 yes
O1 2_676 Cu1 . O2 . 92.3(4) yes
O1 . Cu1 . O2 . 87.7(4) yes
O3 . Cu1 . O2 . 91.93(19) yes
O6 2_667 Cu2 . O8 2_667 86.8(3) yes
O6 2_667 Cu2 . O7 2_667 88.1(3) yes
O8 2_667 Cu2 . O7 2_667 88.4(6) yes
O6 2_667 Cu2 . O6 . 180.00 yes
O8 2_667 Cu2 . O6 . 93.2(3) yes
O7 2_667 Cu2 . O6 . 91.9(3) yes
O6 2_667 Cu2 . O7 . 91.9(3) yes
O8 2_667 Cu2 . O7 . 91.6(6) yes
O7 2_667 Cu2 . O7 . 179.99 yes
O6 . Cu2 . O7 . 88.1(3) yes
O6 2_667 Cu2 . O8 . 93.2(3) yes
O8 2_667 Cu2 . O8 . 179.99 yes
O7 2_667 Cu2 . O8 . 91.6(6) yes
O6 . Cu2 . O8 . 86.8(3) yes
O7 . Cu2 . O8 . 88.4(6) yes
O3 . S1 . O6 . 109.2(3) yes
O3 . S1 . O4 . 110.2(7) yes
O6 . S1 . O4 . 111.0(6) yes
O3 . S1 . O5 . 109.1(6) yes
O6 . S1 . O5 . 109.2(7) yes
O4 . S1 . O5 . 108.1(6) yes
Cu1 . O1 . H11 . 117.3 no
Cu1 . O1 . H12 . 108.1 no
H11 . O1 . H12 . 118.2 no
Cu1 . O3 . S1 . 132.3(3) yes
Cu2 . O6 . S1 . 139.6(4) yes
Cu2 . O7 . H71 . 118.5 no
Cu2 . O7 . H72 . 123.4 no
H71 . O7 . H72 . 118.1 no
Cu2 . O8 . H81 . 122.3 no
Cu2 . O8 . H82 . 132.2 no
H81 . O8 . H82 . 105.3 no
Cu1 . O2 . H21 . 96.6 no
Cu1 . O2 . H22 . 118.6 no
H21 . O2 . H22 . 130.3 no
H91 . O9 . H92 . 122.1 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 2.363(6) yes
Cu1 . O2 2_676 1.972(4) yes
Cu1 . O1 2_676 1.90(2) yes
Cu1 . O1 . 1.90(2) yes
Cu1 . O3 . 2.363(6) yes
Cu1 . O2 . 1.972(4) yes
Cu2 . O6 2_667 2.412(5) yes
Cu2 . O8 2_667 1.932(16) yes
Cu2 . O7 2_667 1.923(12) yes
Cu2 . O6 . 2.412(5) yes
Cu2 . O7 . 1.923(12) yes
Cu2 . O8 . 1.932(16) yes
S1 . O3 . 1.479(5) yes
S1 . O6 . 1.471(5) yes
S1 . O4 . 1.442(15) yes
S1 . O5 . 1.487(16) yes
O1 . H11 . 0.838 no
O1 . H12 . 0.838 no
O7 . H71 . 0.839 no
O7 . H72 . 0.835 no
O8 . H81 . 0.832 no
O8 . H82 . 0.841 no
O2 . H21 . 0.839 no
O2 . H22 . 0.841 no
O9 . H91 . 0.839 no
O9 . H92 . 0.839 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
-2 1 3 x .
-2 -2 8 x .
-1 -3 9 x .
4 -2 4 x .
-2 -2 10 x .
3 -3 11 x .
2 -2 13 x .
-3 6 0 x .
0 2 9 x .
-1 -3 7 x .
0 -4 7 x .
-1 1 4 x .
0 0 4 x .
0 -4 8 x .
5 -3 1 x .
-1 -3 8 x .
-3 3 8 x .
0 -4 6 x .
-4 4 5 x .
-4 3 6 x .
