#------------------------------------------------------------------------------
#$Date: 2018-07-20 09:56:00 +0300 (Fri, 20 Jul 2018) $
#$Revision: 209162 $
#$URL: file:///home/coder/svn-repositories/cod/cif/2/02/11/2021185.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_2021185
loop_
_publ_author_name
'Kiriukhina, Galina V.'
'Yakubovich, Olga V.'
'Kochetkova, Ekaterina M.'
'Dimitrova, Olga V.'
'Volkov, Anatoliy S.'
_publ_section_title
;
 A first Mn member in the struvite morphotropic series,
 CsMn(H₂O)₆(PO₄): hydrothermal synthesis, crystal structure and
 interconnections within the family of related phosphates
;
_journal_coeditor_code           FN3263
_journal_issue                   8
_journal_name_full               'Acta Crystallographica Section C'
_journal_page_first
;
;
_journal_paper_doi               10.1107/S2053229618009798
_journal_volume                  74
_journal_year                    2018
_chemical_formula_iupac          'Cs Mn (H2 O)6 (P O4)'
_chemical_formula_moiety         'H12 Mn O6, O4 P, Cs'
_chemical_formula_sum            'Cs H12 Mn O10 P'
_chemical_formula_weight         390.92
_chemical_name_common            'Caesium manganese hexahydrate phosphate'
_chemical_name_systematic        'Caesium manganese hexahydrate phosphate'
_space_group_crystal_system      hexagonal
_space_group_IT_number           186
_space_group_name_Hall           'P 6c -2c'
_space_group_name_H-M_alt        'P 63 m c'
_symmetry_space_group_name_Hall  'P 6c -2c'
_symmetry_space_group_name_H-M   'P 63 m c'
_atom_sites_solution_hydrogens   difmap
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-2016/6
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                120
_cell_formula_units_Z            2
_cell_length_a                   6.9809(7)
_cell_length_b                   6.9809(7)
_cell_length_c                   12.0270(9)
_cell_measurement_reflns_used    3866
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      32.4917
_cell_measurement_theta_min      3.3630
_cell_volume                     507.59(8)
_computing_cell_refinement
;
CrysAlis PRO (Agilent, 2012)
;
_computing_data_collection
;
CrysAlis PRO (Agilent, 2012)
;
_computing_data_reduction
;
CrysAlis PRO (Agilent, 2012)
;
_computing_molecular_graphics
;
DIAMOND (Brandenburg, 2006)
;
_computing_publication_material
;
SHELXT (Sheldrick, 2015a) within WinGX (Farrugia, 2012)
;
_computing_structure_refinement
;
SHELXL2016 (Sheldrick, 2015b) within WinGX (Farrugia, 2012)
;
_computing_structure_solution
;
SHELXT (Sheldrick, 2015a) within WinGX (Farrugia, 2012)
;
_diffrn_ambient_temperature      293(2)
_diffrn_detector_area_resol_mean 16.0630
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.995
_diffrn_measurement_device_type  'Agilent Xcalibur Sapphire3'
_diffrn_measurement_method       'ω scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0449
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       10
_diffrn_reflns_limit_k_min       -10
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            9705
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         32.529
_diffrn_reflns_theta_min         3.370
_exptl_absorpt_coefficient_mu    5.021
_exptl_absorpt_correction_T_max  0.658
_exptl_absorpt_correction_T_min  0.380
_exptl_absorpt_correction_type   gaussian
_exptl_absorpt_process_details
;
Numerical absorption correction based on gaussian
integration over a multifaceted crystal model
;
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    2.558
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       'hexagonal prism'
_exptl_crystal_F_000             374
_exptl_crystal_size_max          0.123
_exptl_crystal_size_mid          0.082
_exptl_crystal_size_min          0.064
_refine_diff_density_max         0.762
_refine_diff_density_min         -0.792
_refine_ls_abs_structure_details
;
Flack x determined using 283 quotients [(I+)-(I-)]/[(I+)+(I-)]
(Parsons et al.,  2013)
;
_refine_ls_abs_structure_Flack   -0.015(18)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.157
_refine_ls_hydrogen_treatment    refall
_refine_ls_matrix_type           full
_refine_ls_number_parameters     41
_refine_ls_number_reflns         737
_refine_ls_number_restraints     4
_refine_ls_restrained_S_all      1.153
_refine_ls_R_factor_all          0.0378
_refine_ls_R_factor_gt           0.0328
_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/[σ²(Fo²)+(0.0200P)²+0.8000P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0639
_refine_ls_wR_factor_ref         0.0656
_reflns_number_gt                687
_reflns_number_total             737
_reflns_threshold_expression     'I > 2σ(I)'
_cod_data_source_file            fn3263sup1.cif
_cod_data_source_block           I
_cod_original_cell_volume        507.59(11)
_cod_database_code               2021185
_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_min   0.577
_shelx_estimated_absorpt_t_max   0.739
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-y, x-y, z'
'-x+y, -x, z'
'-x, -y, z+1/2'
'y, -x+y, z+1/2'
'x-y, x, z+1/2'
'-y, -x, z'
'-x+y, y, z'
'x, x-y, z'
'y, x, z+1/2'
'x-y, -y, z+1/2'
'-x, -x+y, z+1/2'
loop_
_atom_site_type_symbol
_atom_site_label
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_calc_flag
_atom_site_occupancy
Cs Cs1 0.666667 0.333333 0.43938(17) 0.0518(3) Uani d 1
Mn Mn1 0.333333 0.666667 0.31642(19) 0.0238(4) Uani d 1
P P1 0.000000 0.000000 0.6603(2) 0.0185(4) Uani d 1
O O1 0.1198(3) 0.2396(6) 0.6191(5) 0.0269(8) Uani d 1
O O2 0.000000 0.000000 0.7891(6) 0.030(2) Uani d 1
O O3 0.1816(4) 0.3632(9) 0.4103(3) 0.0496(16) Uani d 1
O O4 0.4834(6) 0.5166(6) 0.2141(5) 0.0507(17) Uani d 1
H H1 0.126(3) 0.252(6) 0.374(5) 0.06(3) Uiso d 1
H H2 0.387(9) 0.413(7) 0.182(4) 0.05(2) Uiso d 1
H H3 0.168(8) 0.337(15) 0.4755(16) 0.07(4) Uiso d 1
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
P P 0.1023 0.0942 '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'
Cs Cs -0.3680 2.1192 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 '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_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle
O4 Cs1 O4 2_655 3_665 66.50(13)
O4 Cs1 O4 2_655 . 66.50(13)
O4 Cs1 O4 3_665 . 66.50(13)
O4 Cs1 O3 2_655 2_665 116.84(10)
O4 Cs1 O3 3_665 2_665 87.45(9)
O4 Cs1 O3 . 2_665 50.35(10)
O4 Cs1 O3 2_655 3 50.35(10)
O4 Cs1 O3 3_665 3 116.84(10)
O4 Cs1 O3 . 3 87.45(9)
O3 Cs1 O3 2_665 3 119.02(3)
O4 Cs1 O3 2_655 . 87.45(9)
O4 Cs1 O3 3_665 . 116.84(10)
O4 Cs1 O3 . . 50.35(10)
O3 Cs1 O3 2_665 . 53.79(17)
O3 Cs1 O3 3 . 65.56(17)
O4 Cs1 O3 2_655 3_665 116.84(10)
O4 Cs1 O3 3_665 3_665 50.35(10)
O4 Cs1 O3 . 3_665 87.45(9)
O3 Cs1 O3 2_665 3_665 65.56(17)
O3 Cs1 O3 3 3_665 167.14(15)
O3 Cs1 O3 . 3_665 119.02(3)
O4 Cs1 O3 2_655 2_655 50.35(10)
O4 Cs1 O3 3_665 2_655 87.45(9)
O4 Cs1 O3 . 2_655 116.84(10)
O3 Cs1 O3 2_665 2_655 167.14(15)
O3 Cs1 O3 3 2_655 53.78(17)
O3 Cs1 O3 . 2_655 119.02(3)
O3 Cs1 O3 3_665 2_655 119.02(3)
O4 Cs1 O3 2_655 1_655 87.45(9)
O4 Cs1 O3 3_665 1_655 50.35(10)
O4 Cs1 O3 . 1_655 116.84(10)
O3 Cs1 O3 2_665 1_655 119.02(3)
O3 Cs1 O3 3 1_655 119.02(3)
O3 Cs1 O3 . 1_655 167.14(15)
O3 Cs1 O3 3_665 1_655 53.78(17)
O3 Cs1 O3 2_655 1_655 65.56(17)
O4 Cs1 O4 2_655 4_665 146.19(4)
O4 Cs1 O4 3_665 4_665 146.19(4)
O4 Cs1 O4 . 4_665 111.95(2)
O3 Cs1 O4 2_665 4_665 70.16(11)
O3 Cs1 O4 3 4_665 96.43(8)
O3 Cs1 O4 . 4_665 70.16(11)
O3 Cs1 O4 3_665 4_665 96.43(8)
O3 Cs1 O4 2_655 4_665 119.28(10)
O3 Cs1 O4 1_655 4_665 119.28(10)
O4 Cs1 O4 2_655 6_655 146.19(4)
O4 Cs1 O4 3_665 6_655 111.95(2)
O4 Cs1 O4 . 6_655 146.19(4)
O3 Cs1 O4 2_665 6_655 96.43(8)
O3 Cs1 O4 3 6_655 119.28(10)
O3 Cs1 O4 . 6_655 119.28(10)
O3 Cs1 O4 3_665 6_655 70.16(11)
O3 Cs1 O4 2_655 6_655 96.43(8)
O3 Cs1 O4 1_655 6_655 70.16(11)
O4 Cs1 O4 4_665 6_655 49.27(14)
O4 Cs1 O4 2_655 5 111.95(2)
O4 Cs1 O4 3_665 5 146.19(4)
O4 Cs1 O4 . 5 146.19(4)
O3 Cs1 O4 2_665 5 119.28(10)
O3 Cs1 O4 3 5 70.16(11)
O3 Cs1 O4 . 5 96.43(8)
O3 Cs1 O4 3_665 5 119.28(10)
O3 Cs1 O4 2_655 5 70.16(11)
O3 Cs1 O4 1_655 5 96.43(8)
O4 Cs1 O4 4_665 5 49.27(14)
O4 Cs1 O4 6_655 5 49.27(14)
O3 Mn1 O3 3_565 2_665 95.04(19)
O3 Mn1 O3 3_565 . 95.04(19)
O3 Mn1 O3 2_665 . 95.04(19)
O3 Mn1 O4 3_565 3_565 86.67(16)
O3 Mn1 O4 2_665 3_565 177.5(3)
O3 Mn1 O4 . 3_565 86.67(16)
O3 Mn1 O4 3_565 2_665 86.67(16)
O3 Mn1 O4 2_665 2_665 86.67(16)
O3 Mn1 O4 . 2_665 177.5(3)
O4 Mn1 O4 3_565 2_665 91.6(3)
O3 Mn1 O4 3_565 . 177.5(3)
O3 Mn1 O4 2_665 . 86.67(16)
O3 Mn1 O4 . . 86.67(16)
O4 Mn1 O4 3_565 . 91.6(3)
O4 Mn1 O4 2_665 . 91.6(3)
O3 Mn1 Cs1 3_565 . 128.24(15)
O3 Mn1 Cs1 2_665 . 54.527(13)
O3 Mn1 Cs1 . . 54.528(13)
O4 Mn1 Cs1 3_565 . 125.580(11)
O4 Mn1 Cs1 2_665 . 125.580(11)
O4 Mn1 Cs1 . . 54.3(2)
O3 Mn1 Cs1 3_565 1_565 54.528(14)
O3 Mn1 Cs1 2_665 1_565 54.529(13)
O3 Mn1 Cs1 . 1_565 128.24(15)
O4 Mn1 Cs1 3_565 1_565 125.578(11)
O4 Mn1 Cs1 2_665 1_565 54.3(2)
O4 Mn1 Cs1 . 1_565 125.580(11)
Cs1 Mn1 Cs1 . 1_565 108.79(2)
O3 Mn1 Cs1 3_565 1_455 54.528(14)
O3 Mn1 Cs1 2_665 1_455 128.24(15)
O3 Mn1 Cs1 . 1_455 54.528(14)
O4 Mn1 Cs1 3_565 1_455 54.3(2)
O4 Mn1 Cs1 2_665 1_455 125.578(11)
O4 Mn1 Cs1 . 1_455 125.580(11)
Cs1 Mn1 Cs1 . 1_455 108.79(2)
Cs1 Mn1 Cs1 1_565 1_455 108.78(2)
O1 P1 O1 2 3 110.1(2)
O1 P1 O1 2 . 110.1(2)
O1 P1 O1 3 . 110.1(2)
O1 P1 O2 2 . 108.9(2)
O1 P1 O2 3 . 108.9(2)
O1 P1 O2 . . 108.9(2)
Mn1 O3 Cs1 . . 95.51(8)
Mn1 O3 Cs1 . 1_455 95.51(8)
Cs1 O3 Cs1 . 1_455 167.14(15)
Mn1 O3 H1 . . 115(5)
Cs1 O3 H1 . . 90.7(6)
Cs1 O3 H1 1_455 . 90.7(6)
Mn1 O3 H3 . . 133(7)
Cs1 O3 H3 . . 83.8(2)
Cs1 O3 H3 1_455 . 83.8(2)
H1 O3 H3 . . 112(8)
Mn1 O4 Cs1 . . 95.1(2)
Mn1 O4 Cs1 . 4_664 95.4(2)
Cs1 O4 Cs1 . 4_664 169.50(16)
Mn1 O4 H2 . . 108(6)
Cs1 O4 H2 . . 110(5)
Cs1 O4 H2 4_664 . 66(5)
Mn1 O4 H2 . 7_665 108(6)
Cs1 O4 H2 . 7_665 110(5)
Cs1 O4 H2 4_664 7_665 66(5)
H2 O4 H2 . 7_665 122(9)
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_site_symmetry_2
_geom_bond_distance
_geom_bond_publ_flag
Cs1 O4 2_655 3.500(8) ?
Cs1 O4 3_665 3.500(8) ?
Cs1 O4 . 3.501(8) y
Cs1 O3 2_665 3.5125(6) ?
Cs1 O3 3 3.5126(6) ?
Cs1 O3 . 3.5126(6) y
Cs1 O3 3_665 3.5126(6) y
Cs1 O3 2_655 3.5126(6) ?
Cs1 O3 1_655 3.5126(6) ?
Cs1 O4 4_665 3.769(8) ?
Cs1 O4 6_655 3.769(8) ?
Cs1 O4 5 3.769(8) y
Mn1 O3 3_565 2.154(5) ?
Mn1 O3 2_665 2.154(5) ?
Mn1 O3 . 2.154(5) y
Mn1 O4 3_565 2.192(5) ?
Mn1 O4 2_665 2.192(5) ?
Mn1 O4 . 2.192(5) y
P1 O1 2 1.531(4) ?
P1 O1 3 1.531(4) ?
P1 O1 . 1.531(4) y
P1 O2 . 1.550(8) y
O3 H1 . 0.8000(15) ?
O3 H3 . 0.8000(15) ?
O4 H2 . 0.8000(15) ?
O4 H2 7_665 0.8000(15) ?
loop_
_geom_hbond_atom_site_label_D
_geom_hbond_atom_site_label_H
_geom_hbond_atom_site_label_A
_geom_hbond_site_symmetry_A
_geom_hbond_distance_DH
_geom_hbond_distance_HA
_geom_hbond_distance_DA
_geom_hbond_angle_DHA
O3 H1 O2 4_554 0.8000(15) 1.836(7) 2.636(7) 179(7)
O4 H2 O1 5_554 0.8000(15) 1.93(3) 2.676(4) 155(8)
O3 H3 O1 . 0.8000(15) 1.825(15) 2.620(7) 173(10)

_cod_database_fobs_code 2021185
