#------------------------------------------------------------------------------
#$Date: 2022-03-04 23:11:27 +0100 (vie 04 de mar de 2022) $
#$Revision: 273361 $
#$URL: svn://www.crystallography.net/cod/cif/7/70/93/7709390.cif $
#------------------------------------------------------------------------------
#
# This file is available in the Crystallography Open Database (COD),
# http://www.crystallography.net/
#
# All data on this site have been placed in the public domain by the
# contributors.
#
data_7709390
loop_
_publ_author_name
'Hämmer, Matthias'
'Pielnhofer, Florian'
'Janka, Oliver'
'Takahashi, Hirotaka'
'Gross, Peter'
'Pöttgen, Rainer'
'Höppe, Henning A'
_publ_section_title
;
 Polymorphism and optical, magnetic and thermal properties of the either
 phyllo- or inosilicate-analogous borosulfate
 Cu[B₂(SO₄)₄].
;
_journal_issue                   8
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              3104
_journal_page_last               3115
_journal_paper_doi               10.1039/d1dt04090a
_journal_volume                  51
_journal_year                    2022
_chemical_formula_moiety         'B2 Cu O16 S4'
_chemical_formula_sum            'B2 Cu O16 S4'
_chemical_formula_weight         469.40
_chemical_name_common            beta-Cupperborosulfate
_chemical_name_systematic        'beta-Copper(II) Borosulfate'
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2yn'
_space_group_name_H-M_alt        'P 1 21/n 1'
_audit_creation_method           SHELXL-2014/7
_cell_angle_alpha                90
_cell_angle_beta                 111.220(11)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   7.712(3)
_cell_length_b                   8.149(3)
_cell_length_c                   9.092(3)
_cell_measurement_reflns_used    3829
_cell_measurement_temperature    250(2)
_cell_measurement_theta_max      42.499
_cell_measurement_theta_min      2.979
_cell_volume                     532.6(3)
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_diffrn_ambient_temperature      250(2)
_diffrn_measured_fraction_theta_full 0.995
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device_type  'D8 Venture Bruker'
_diffrn_measurement_method       'generic phi and omega scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0326
_diffrn_reflns_av_unetI/netI     0.0161
_diffrn_reflns_Laue_measured_fraction_full 0.995
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            31258
_diffrn_reflns_point_group_measured_fraction_full 0.995
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         42.499
_diffrn_reflns_theta_min         2.979
_exptl_absorpt_coefficient_mu    2.944
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
; 
 multi-scan absorption correction using SADABS 
(G. M. Sheldrick, (1996). SADABS. Program for Empirical 
Absorption Correction. University of Göttingen, Germany.)
;
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    2.927
_exptl_crystal_description       block
_exptl_crystal_F_000             462
_exptl_crystal_size_max          0.19
_exptl_crystal_size_mid          0.15
_exptl_crystal_size_min          0.11
_exptl_transmission_factor_max   0.7503
_exptl_transmission_factor_min   0.6364
_refine_diff_density_max         0.643
_refine_diff_density_min         -0.668
_refine_diff_density_rms         0.102
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.085
_refine_ls_hydrogen_treatment    undef
_refine_ls_matrix_type           full
_refine_ls_number_parameters     106
_refine_ls_number_reflns         3829
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.085
_refine_ls_R_factor_all          0.0229
_refine_ls_R_factor_gt           0.0199
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[σ²(Fo²)+(0.0268P)²+0.1674P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0525
_refine_ls_wR_factor_ref         0.0535
_reflns_Friedel_coverage         0.000
_reflns_number_gt                3531
_reflns_number_total             3829
_reflns_threshold_expression     'I > 2σ(I)'
_cod_data_source_file            d1dt04090a5.cif
_cod_data_source_block           mo_MH362_1_0m
_cod_depositor_comments
'Adding full bibliography for 7709384--7709391.cif.'
_cod_original_cell_volume        532.7(4)
_cod_original_sg_symbol_H-M      'P 21/n'
_cod_database_code               7709390
_shelx_shelxl_version_number     2014/7
_shelx_space_group_comment
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x+1/2, y+1/2, -z+1/2'
'-x, -y, -z'
'x-1/2, -y-1/2, z-1/2'
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_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
Cu1 Cu 0.0000 0.0000 0.0000 0.00933(3) Uani 1 2 d S . P . .
S1 S -0.70341(2) 0.07666(2) 0.35248(2) 0.00709(3) Uani 1 1 d . . . . .
S2 S -0.28560(2) -0.15743(2) 0.14444(2) 0.00769(3) Uani 1 1 d . . . . .
O11 O -0.55574(8) -0.00837(6) 0.30328(7) 0.00964(7) Uani 1 1 d . . . . .
O12 O -0.87397(8) 0.07810(8) 0.21722(6) 0.01422(9) Uani 1 1 d . . . . .
O13 O -0.64004(8) 0.23123(7) 0.42539(7) 0.01207(8) Uani 1 1 d . . . . .
O14 O -0.26687(8) 0.04582(7) 0.53142(6) 0.01043(8) Uani 1 1 d . . . . .
O21 O -0.25352(8) -0.07600(8) 0.30280(7) 0.01397(9) Uani 1 1 d . . . . .
O22 O -0.46910(8) -0.21490(8) 0.06918(8) 0.01697(10) Uani 1 1 d . . . . .
O23 O -0.35696(8) 0.20538(7) 0.29376(7) 0.01285(9) Uani 1 1 d . . . . .
O24 O -0.21969(9) -0.04854(9) 0.04967(8) 0.01643(10) Uani 1 1 d . . . . .
B1 B -0.35882(10) 0.04137(9) 0.35692(8) 0.00835(10) Uani 1 1 d . . . . .
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
B B 0.0013 0.0007 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Cu Cu 0.3201 1.2651 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
O24 Cu1 O24 180.0 . 3 ?
O24 Cu1 O12 89.32(3) . 1_655 ?
O24 Cu1 O12 90.68(4) 3 1_655 ?
O24 Cu1 O12 90.68(3) . 3_455 ?
O24 Cu1 O12 89.32(4) 3 3_455 ?
O12 Cu1 O12 180.000(19) 1_655 3_455 ?
O24 Cu1 O13 95.07(3) . 2_445 ?
O24 Cu1 O13 84.93(3) 3 2_445 ?
O12 Cu1 O13 90.18(3) 1_655 2_445 ?
O12 Cu1 O13 89.82(3) 3_455 2_445 ?
O24 Cu1 O13 84.93(3) . 4_665 ?
O24 Cu1 O13 95.07(3) 3 4_665 ?
O12 Cu1 O13 89.82(3) 1_655 4_665 ?
O12 Cu1 O13 90.18(3) 3_455 4_665 ?
O13 Cu1 O13 180.00(3) 2_445 4_665 ?
O13 S1 O12 116.34(4) . . ?
O13 S1 O14 111.58(4) . 3_456 ?
O12 S1 O14 106.03(4) . 3_456 ?
O13 S1 O11 111.70(4) . . ?
O12 S1 O11 107.48(4) . . ?
O14 S1 O11 102.67(4) 3_456 . ?
O22 S2 O24 114.88(4) . . ?
O22 S2 O21 113.25(4) . . ?
O24 S2 O21 108.85(5) . . ?
O22 S2 O23 113.46(4) . 2_445 ?
O24 S2 O23 107.84(4) . 2_445 ?
O21 S2 O23 97.03(4) . 2_445 ?
B1 O11 S1 124.40(5) . . ?
S1 O12 Cu1 145.36(4) . 1_455 ?
S1 O13 Cu1 166.05(4) . 2_455 ?
B1 O14 S1 126.05(5) . 3_456 ?
B1 O21 S2 133.54(5) . . ?
B1 O23 S2 129.48(5) . 2_455 ?
S2 O24 Cu1 141.62(4) . . ?
O21 B1 O23 112.61(6) . . ?
O21 B1 O11 110.03(6) . . ?
O23 B1 O11 106.13(6) . . ?
O21 B1 O14 105.59(6) . . ?
O23 B1 O14 109.25(6) . . ?
O11 B1 O14 113.36(6) . . ?
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Cu1 O24 1.9455(9) . ?
Cu1 O24 1.9455(9) 3 ?
Cu1 O12 1.9649(8) 1_655 ?
Cu1 O12 1.9649(8) 3_455 ?
Cu1 O13 2.4277(10) 2_445 ?
Cu1 O13 2.4277(10) 4_665 ?
S1 O13 1.4250(7) . ?
S1 O12 1.4393(7) . ?
S1 O14 1.5292(7) 3_456 ?
S1 O11 1.5317(7) . ?
S2 O22 1.4105(8) . ?
S2 O24 1.4509(7) . ?
S2 O21 1.5221(7) . ?
S2 O23 1.5255(7) 2_445 ?
O11 B1 1.4739(11) . ?
O12 Cu1 1.9649(8) 1_455 ?
O13 Cu1 2.4277(10) 2_455 ?
O14 B1 1.4855(10) . ?
O14 S1 1.5291(7) 3_456 ?
O21 B1 1.4512(9) . ?
O23 B1 1.4568(10) . ?
O23 S2 1.5255(7) 2_455 ?
