#------------------------------------------------------------------------------
#$Date: 2021-03-05 03:45:09 +0200 (Fri, 05 Mar 2021) $
#$Revision: 262567 $
#$URL: file:///home/coder/svn-repositories/cod/cif/7/24/18/7241877.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_7241877
loop_
_publ_author_name
'Kornyakov, Ilya V.'
'Tyumentseva, Olga S.'
'Krivovichev, Sergey V.'
'Tananaev, Ivan G.'
'Gurzhiy, Vladislav V.'
_publ_section_title
;
 Crystal chemistry of the M2+[(UO2)(T6+O4)2(H2O)](H2O)4 (M2+ = Mg, Mn, Fe,
 Co, Ni and Zn; T6+ = S, Se) compounds: the interplay between chemical
 composition, pH and structural architecture
;
_journal_issue                   5
_journal_name_full               CrystEngComm
_journal_page_first              1140
_journal_page_last               1148
_journal_paper_doi               10.1039/D0CE01587C
_journal_volume                  23
_journal_year                    2021
_chemical_formula_moiety         'H10 Mn O15 S2 U'
_chemical_formula_sum            'H10 Mn O15 S2 U'
_chemical_formula_weight         607.17
_space_group_crystal_system      monoclinic
_space_group_IT_number           4
_space_group_name_Hall           'P 2yb'
_space_group_name_H-M_alt        'P 1 21 1'
_atom_sites_solution_hydrogens   difmap
_atom_sites_solution_primary     dual
_audit_creation_date             2020-10-18
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_audit_update_record
;
2020-10-18 deposited with the CCDC.	2020-12-08 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90.773(2)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   6.51140(10)
_cell_length_b                   11.3829(2)
_cell_length_c                   8.3439(2)
_cell_measurement_reflns_used    10264
_cell_measurement_temperature    296(2)
_cell_measurement_theta_max      36.5390
_cell_measurement_theta_min      1.7820
_cell_volume                     618.38(2)
_computing_cell_refinement       'CrysAlisPro 1.171.39.44a (Rigaku OD, 2018)'
_computing_data_collection       'CrysAlisPro 1.171.39.44a (Rigaku OD, 2018)'
_computing_data_reduction        'CrysAlisPro 1.171.39.44a (Rigaku OD, 2018)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_computing_structure_solution    'ShelXT (Sheldrick, 2015)'
_diffrn_ambient_temperature      296(2)
_diffrn_detector                 'CCD plate'
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 1.000
_diffrn_measurement_details
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  tₑₓₚ   ω     θ     κ     φ   Frames
#--------------------------------------------------------------------------
  1  ω      8.21 192.21   0.50   60.00    --   34.00  73.86 -25.79  368
  2  ω      8.21 192.21   0.50   60.00    --   34.00  73.86  64.21  368
  3  ω      8.21 192.21   0.50   60.00    --   34.00  73.86 154.21  368
;
_diffrn_measurement_device       'abstract diffractometer'
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       'ω scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      -0.1085739000
_diffrn_orient_matrix_UB_12      -0.0049776000
_diffrn_orient_matrix_UB_13      -0.0032756000
_diffrn_orient_matrix_UB_21      0.0067559000
_diffrn_orient_matrix_UB_22      -0.0306072000
_diffrn_orient_matrix_UB_23      -0.0737062000
_diffrn_orient_matrix_UB_31      0.0062680000
_diffrn_orient_matrix_UB_32      -0.0541021000
_diffrn_orient_matrix_UB_33      0.0420813000
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0164
_diffrn_reflns_av_unetI/netI     0.0173
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 1.000
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       11
_diffrn_reflns_limit_l_min       -11
_diffrn_reflns_number            8215
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 1.000
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         29.988
_diffrn_reflns_theta_min         2.441
_diffrn_source                   'fine-focus sealed X-ray tube'
_diffrn_source_type              'Enhance (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    14.515
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.43201
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.39.44a (Rigaku Oxford Diffraction, 2018)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            'clear yellow'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    3.261
_exptl_crystal_description       plate
_exptl_crystal_F_000             558
_exptl_crystal_size_max          0.44
_exptl_crystal_size_mid          0.42
_exptl_crystal_size_min          0.12
_refine_diff_density_max         0.758
_refine_diff_density_min         -0.674
_refine_diff_density_rms         0.149
_refine_ls_abs_structure_details
;
 Flack x determined using 1629 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   -0.012(5)
_refine_ls_extinction_coef       0.0075(5)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4^
_refine_ls_extinction_method     SHELXL
_refine_ls_goodness_of_fit_ref   1.038
_refine_ls_hydrogen_treatment    refxyz
_refine_ls_matrix_type           full
_refine_ls_number_parameters     204
_refine_ls_number_reflns         3600
_refine_ls_number_restraints     28
_refine_ls_restrained_S_all      1.043
_refine_ls_R_factor_all          0.0171
_refine_ls_R_factor_gt           0.0163
_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)+(0.0283P)²+0.1753P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0398
_refine_ls_wR_factor_ref         0.0401
_reflns_Friedel_coverage         0.911
_reflns_Friedel_fraction_full    1.000
_reflns_Friedel_fraction_max     1.000
_reflns_number_gt                3495
_reflns_number_total             3600
_reflns_threshold_expression     'I > 2σ(I)'
_cod_data_source_file            d0ce01587c1.cif
_cod_data_source_block           Compound_14
_cod_depositor_comments
'Adding full bibliography for 7241870--7241883.cif.'
_cod_database_code               7241877
_shelxl_version_number           2014/6
_chemical_oxdiff_formula         'Mn1 U1 S2 O15'
_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.
;
_shelx_estimated_absorpt_t_max   0.275
_shelx_estimated_absorpt_t_min   0.061
_reflns_odcompleteness_completeness 96.58
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     36.27
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.5 times of:
  All H(H) groups, All O(H,H,H,H,H,H,H,H) groups
2. Restrained distances
 H3A-H3B
 1.54 with sigma of 0.02
 O3-H3B
 0.98 with sigma of 0.02
 O3-H3A
 0.98 with sigma of 0.02
 O6_$1-H3B
 1.65 with sigma of 0.02
 O14_$1-H14B_$1 = O14_$1-H14A_$1
 0.98 with sigma of 0.02
 H14B_$1-H14A_$1
 1.54 with sigma of 0.02
 O5_$2-H14B_$1
 2.1 with sigma of 0.02
 H14A_$1-O7_$3
 2.1 with sigma of 0.02
 O15-H15B = O15-H15A
 0.9 with sigma of 0.02
 H15A-H15B
 1.45 with sigma of 0.02
 H15A-O7_$4
 2.1 with sigma of 0.02
 H15B-O6
 2.1 with sigma of 0.02
 O13-H13A = O13-H13B
 0.9 with sigma of 0.02
 H13A-H13B
 1.45 with sigma of 0.02
 H13A-O1_$2
 2.1 with sigma of 0.02
 O13-H13B
 0.9 with sigma of 0.02
 H13B-H13A
 1.54 with sigma of 0.02
 H13B-O3_$3
 2.2 with sigma of 0.02
 O2_$3-H12A
 2.5 with sigma of 0.02
 O12-H12A
 0.9 with sigma of 0.02
 H12B-H12A
 1.54 with sigma of 0.02
 O12-H12B
 0.9 with sigma of 0.02
 H12A-O2_$3
 2.41 with sigma of 0.02
 H12B-O1
 2.2 with sigma of 0.02
;
_olex2_submission_special_instructions 'No special instructions were received'
_oxdiff_exptl_absorpt_empirical_details
;
Empirical correction (ABSPACK) includes:
- Absorption correction using spherical harmonics
- Frame scaling
- Detector area scaling
;
_oxdiff_exptl_absorpt_empirical_full_max 1.581
_oxdiff_exptl_absorpt_empirical_full_min 0.680
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, y+1/2, -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_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
U1 U 0.00250(2) 0.24499(3) 0.11186(2) 0.01308(6) Uani 1 1 d . . . . .
Mn1 Mn -0.49975(12) 0.06796(8) -0.33123(12) 0.02129(17) Uani 1 1 d . . . . .
S1 S -0.0167(2) 0.43881(13) -0.2355(2) 0.0160(3) Uani 1 1 d . . . . .
S2 S 0.0038(2) 0.05660(13) -0.25657(19) 0.0130(3) Uani 1 1 d . . . . .
O1 O -0.2596(6) 0.2163(3) 0.1489(6) 0.0265(9) Uani 1 1 d D . . . .
O2 O 0.2638(6) 0.2728(4) 0.0741(6) 0.0300(11) Uani 1 1 d D . . . .
O3 O 0.0808(9) 0.2555(6) 0.4010(5) 0.0388(12) Uani 1 1 d D . . . .
O4 O -0.0978(8) 0.3659(5) -0.1035(7) 0.0314(12) Uani 1 1 d . . . . .
O5 O -0.1034(7) 0.5591(4) -0.2147(6) 0.0290(9) Uani 1 1 d D . . . .
O6 O -0.1054(9) 0.3915(5) -0.3829(6) 0.0362(12) Uani 1 1 d D . . . .
O7 O 0.2061(6) 0.4419(4) -0.2314(7) 0.0362(11) Uani 1 1 d D . . . .
O8 O -0.0320(10) 0.1154(6) -0.1043(7) 0.0413(16) Uani 1 1 d . . . . .
O9 O 0.1790(6) 0.1082(4) -0.3370(6) 0.0303(10) Uani 1 1 d . . . . .
O10 O -0.1758(6) 0.0670(6) -0.3598(6) 0.0337(12) Uani 1 1 d . . . . .
O11 O 0.0491(8) -0.0673(4) -0.2243(6) 0.0327(10) Uani 1 1 d . . . . .
O12 O -0.5006(9) 0.0286(6) -0.0706(7) 0.0464(14) Uani 1 1 d D . . . .
O13 O -0.5125(10) -0.1205(7) -0.3671(9) 0.0451(18) Uani 1 1 d D . . . .
H13A H -0.605(12) -0.167(9) -0.316(14) 0.18(10) Uiso 1 1 d D . . . .
H12A H -0.468(13) -0.046(4) -0.046(14) 0.268 Uiso 1 1 d DR . . . .
O14 O -0.5079(7) 0.0843(7) -0.5950(7) 0.0345(15) Uani 1 1 d D . . . .
O15 O -0.4785(7) 0.2582(6) -0.2870(8) 0.0449(15) Uani 1 1 d D . . . .
H3A H 0.110(15) 0.181(5) 0.453(10) 0.067 Uiso 1 1 d DR . . . .
H3B H 0.017(17) 0.302(7) 0.489(9) 0.067 Uiso 1 1 d DR . . . .
H12B H -0.434(16) 0.085(8) -0.004(12) 0.067 Uiso 1 1 d DR . . . .
H13B H -0.400(7) -0.164(7) -0.396(11) 0.067 Uiso 1 1 d DR . . . .
H14A H -0.391(7) 0.037(7) -0.612(8) 0.067 Uiso 1 1 d DR . . . .
H14B H -0.628(7) 0.048(6) -0.642(10) 0.067 Uiso 1 1 d DR . . . .
H15A H -0.593(7) 0.301(5) -0.277(14) 0.067 Uiso 1 1 d DR . . . .
H15B H -0.371(8) 0.310(6) -0.287(10) 0.067 Uiso 1 1 d DR . . . .
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Mn Mn 0.3368 0.7283 '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'
U U -9.6767 9.6646 '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
O1 U1 O3 91.5(2) . . ?
O1 U1 O4 89.02(19) . . ?
O1 U1 O5 92.02(17) . 2_545 ?
O1 U1 O8 86.3(2) . . ?
O1 U1 O11 87.42(18) . 2 ?
O2 U1 O1 179.6(2) . . ?
O2 U1 O3 88.8(2) . . ?
O2 U1 O4 90.98(19) . . ?
O2 U1 O5 87.79(18) . 2_545 ?
O2 U1 O8 93.3(2) . . ?
O2 U1 O11 92.94(19) . 2 ?
O4 U1 O3 140.6(2) . . ?
O4 U1 O5 150.7(2) . 2_545 ?
O4 U1 O11 74.6(2) . 2 ?
O5 U1 O3 68.7(2) 2_545 . ?
O8 U1 O3 143.4(2) . . ?
O8 U1 O4 75.9(2) . . ?
O8 U1 O5 74.9(2) . 2_545 ?
O8 U1 O11 149.9(2) . 2 ?
O11 U1 O3 66.1(2) 2 . ?
O11 U1 O5 134.76(17) 2 2_545 ?
O9 Mn1 O12 92.9(2) 1_455 . ?
O9 Mn1 O13 100.0(2) 1_455 . ?
O9 Mn1 O14 87.09(19) 1_455 . ?
O9 Mn1 O15 81.52(17) 1_455 . ?
O10 Mn1 O9 165.7(2) . 1_455 ?
O10 Mn1 O12 97.1(2) . . ?
O10 Mn1 O13 90.9(2) . . ?
O10 Mn1 O14 84.21(18) . . ?
O10 Mn1 O15 87.9(2) . . ?
O13 Mn1 O12 86.3(3) . . ?
O13 Mn1 O14 86.9(3) . . ?
O13 Mn1 O15 177.8(3) . . ?
O14 Mn1 O12 173.0(3) . . ?
O15 Mn1 O12 92.0(3) . . ?
O15 Mn1 O14 94.9(3) . . ?
O4 S1 O5 106.7(3) . . ?
O6 S1 O4 106.2(3) . . ?
O6 S1 O5 107.0(3) . . ?
O7 S1 O4 111.2(3) . . ?
O7 S1 O5 110.8(3) . . ?
O7 S1 O6 114.5(3) . . ?
O8 S2 O11 108.4(4) . . ?
O9 S2 O8 110.6(4) . . ?
O9 S2 O11 108.4(3) . . ?
O10 S2 O8 110.1(4) . . ?
O10 S2 O9 108.9(3) . . ?
O10 S2 O11 110.3(3) . . ?
S1 O4 U1 143.0(3) . . ?
S1 O5 U1 139.2(3) . 2 ?
S2 O8 U1 161.3(5) . . ?
S2 O9 Mn1 132.5(3) . 1_655 ?
S2 O10 Mn1 136.7(3) . . ?
S2 O11 U1 156.3(3) . 2_545 ?
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
U1 O1 1.769(4) . ?
U1 O2 1.763(4) . ?
U1 O3 2.462(4) . ?
U1 O4 2.349(5) . ?
U1 O5 2.373(4) 2_545 ?
U1 O8 2.338(6) . ?
U1 O11 2.359(4) 2 ?
Mn1 O9 2.141(4) 1_455 ?
Mn1 O10 2.126(4) . ?
Mn1 O12 2.220(6) . ?
Mn1 O13 2.168(8) . ?
Mn1 O14 2.209(6) . ?
Mn1 O15 2.201(7) . ?
S1 O4 1.482(5) . ?
S1 O5 1.492(4) . ?
S1 O6 1.455(5) . ?
S1 O7 1.451(4) . ?
S2 O8 1.458(6) . ?
S2 O9 1.455(4) . ?
S2 O10 1.448(5) . ?
S2 O11 1.465(5) . ?
O5 U1 2.373(4) 2 ?
O9 Mn1 2.141(4) 1_655 ?
O11 U1 2.359(4) 2_545 ?
loop_
_geom_hbond_atom_site_label_D
_geom_hbond_atom_site_label_H
_geom_hbond_atom_site_label_A
_geom_hbond_distance_DH
_geom_hbond_distance_HA
_geom_hbond_distance_DA
_geom_hbond_angle_DHA
_geom_hbond_site_symmetry_A
O3 H3A O9 0.97(3) 1.98(7) 2.822(7) 143(8) 1_556
O3 H3B O6 1.00(2) 1.68(2) 2.679(7) 172(9) 1_556
loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
O4 S1 O5 U1 100.3(5) . . . 2 ?
O5 S1 O4 U1 -123.7(6) . . . . ?
O6 S1 O4 U1 122.4(6) . . . . ?
O6 S1 O5 U1 -146.3(4) . . . 2 ?
O7 S1 O4 U1 -2.8(7) . . . . ?
O7 S1 O5 U1 -20.9(6) . . . 2 ?
O8 S2 O9 Mn1 90.7(5) . . . 1_655 ?
O8 S2 O10 Mn1 -36.0(7) . . . . ?
O8 S2 O11 U1 50.1(9) . . . 2_545 ?
O9 S2 O8 U1 0.5(14) . . . . ?
O9 S2 O10 Mn1 -157.5(5) . . . . ?
O9 S2 O11 U1 170.2(7) . . . 2_545 ?
O10 S2 O8 U1 -119.9(13) . . . . ?
O10 S2 O9 Mn1 -148.2(4) . . . 1_655 ?
O10 S2 O11 U1 -70.6(9) . . . 2_545 ?
O11 S2 O8 U1 119.3(13) . . . . ?
O11 S2 O9 Mn1 -28.1(5) . . . 1_655 ?
O11 S2 O10 Mn1 83.6(6) . . . . ?
