Crystal structure of posnjakite formed in the first crystal water-cooling line of the ANSTO Melbourne Australian Synchrotron MX1 Double Crystal Monochromator
Mills, Stuart; Aishima, Jun; Aragao, David; Caradoc-Davies, Tom Tudor; Cowieson, Nathan; Gee, Christine L.; Ericsson, Daniel; Harrop, Stephen; Panjikar, Santosh; Smith, Kate Mary Louise; Riboldi-Tunnicliffe, Alan; Williamson, Rachel; Price, Jason Roy; Acta Crystallographica Section E 76 (2020) 1136–1138; doi:10.1107/S2056989020008099

data_2243452
_publ_section_title
;
 Crystal structure of posnjakite formed in the first crystal water-cooling
 line of the ANSTO Melbourne Australian Synchrotron MX1 Double Crystal
 Monochromator
;
_journal_coeditor_code           TX2024
_journal_issue                   7
_journal_name_full               'Acta Crystallographica Section E'
_journal_page_first              1136
_journal_page_last               1138
_journal_paper_doi               10.1107/S2056989020008099
_journal_volume                  76
_journal_year                    2020
_chemical_absolute_configuration ad
_chemical_formula_iupac          'Cu4 (S O)4 (O H)6 (H2 O)'
_chemical_formula_sum            'Cu4 H8 O11 S'
_chemical_formula_weight         470.28
_chemical_name_common            Posnjakite
_chemical_name_systematic
;
Poly[[hexa-\m-hydroxido-tetracopper(II)] sulfate monohydrate]
;
_space_group_crystal_system      monoclinic
_space_group_IT_number           7
_space_group_name_Hall           'P -2yac'
_space_group_name_H-M_alt        'P 1 n 1'
_atom_sites_solution_hydrogens   difmap
_audit_creation_method           SHELXL-2018/3
_cell_angle_alpha                90
_cell_angle_beta                 107.32(3)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   7.8400(16)
_cell_length_b                   6.3400(13)
_cell_length_c                   9.768(2)
_cell_measurement_reflns_used    96
_cell_measurement_temperature    100(2)
_cell_volume                     463.51(18)
_computing_cell_refinement
;
<i>XDS</i> (Kabsch, 2010)
;
_computing_data_collection       '<i>AS QEGUI</i>'
_computing_data_reduction
;
<i>XDS</i> (Kabsch, 2010))
;
_computing_molecular_graphics
;
<i>shelXle</i> (H\"ubschle <i>et al.</i>,  2011), ORTEP-3 for Windows
(Farrugia,
2012)
;
_computing_publication_material
;
publCIF (Westrip, 2010)
;
_computing_structure_refinement
;
SHELXL (Sheldrick, 2015b)
;
_computing_structure_solution
;
SHELXT (Sheldrick, 2015a)
;
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.992
_diffrn_measurement_device_type  'MX1 Beamline Australian Synchrotron'
_diffrn_measurement_method       'Silicon 111'
_diffrn_radiation_type           synchrotron
_diffrn_radiation_wavelength     0.71074
_diffrn_reflns_av_R_equivalents  0.0185
_diffrn_reflns_av_unetI/netI     0.0246
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_k_max       7
_diffrn_reflns_limit_k_min       -7
_diffrn_reflns_limit_l_max       11
_diffrn_reflns_limit_l_min       -12
_diffrn_reflns_number            5709
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         26.000
_diffrn_reflns_theta_min         2.939
_diffrn_source                   'Double Crystal Monochromator'
_exptl_absorpt_coefficient_mu    9.326
_exptl_absorpt_correction_T_max  0.7458
_exptl_absorpt_correction_T_min  0.5170
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
(SADABS; Bruker, 2001)
;
_exptl_crystal_colour            blue
_exptl_crystal_density_diffrn    3.370
_exptl_crystal_description       plate
_exptl_crystal_F_000             456
_exptl_crystal_size_max          0.150
_exptl_crystal_size_mid          0.100
_exptl_crystal_size_min          0.050
_refine_diff_density_max         0.666
_refine_diff_density_min         -0.919
_refine_ls_abs_structure_details
;
Flack <i>x</i> determined using 745 quotients
[(<i>I</i>^+^)-(<i>I</i>^-^)]/[(<i>I</i>^+^)+(<i>I</i>^-^)]
(Parsons <i>et al.</i>,  2013)
;
_refine_ls_abs_structure_Flack   0.128(16)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.059
_refine_ls_hydrogen_treatment    refxyz
_refine_ls_matrix_type           full
_refine_ls_number_parameters     157
_refine_ls_number_reflns         1763
_refine_ls_number_restraints     19
_refine_ls_restrained_S_all      1.056
_refine_ls_R_factor_all          0.0306
_refine_ls_R_factor_gt           0.0288
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0447P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0714
_refine_ls_wR_factor_ref         0.0738
_reflns_number_gt                1652
_reflns_number_total             1763
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            tx2024sup1.cif
_cod_data_source_block           I
_cod_original_sg_symbol_H-M      'P n'
_cod_database_code               2243452
_shelx_hkl_checksum              26300
_shelx_res_checksum              41006
_cod_database_fobs_code 2243452