Novel K/Mn phosphate hydrates, K~2~Mn~3~(H~2~O)~2~[P~2~O~7~]~2~ and KMn(H~2~O)~2~[Al~2~(PO~4~)~3~]: hydrothermal synthesis and crystal chemistry
Kiriukhina, Galina V.; Yakubovich, Olga V.; Shvanskaya, Larisa V.; Kochetkova, Ekaterina M.; Dimitrova, Olga V.; Volkov, Anatoliy S.; Simonov, Sergey V.; Acta Crystallographica Section C 76 (2020) –; doi:10.1107/S2053229620002466

data_2021990
_publ_section_title
;
 Novel K/Mn phosphate hydrates, K~2~Mn~3~(H~2~O)~2~[P~2~O~7~]~2~ and
 KMn(H~2~O)~2~[Al~2~(PO~4~)~3~]: hydrothermal synthesis and crystal
 chemistry
;
_journal_coeditor_code           FN3331
_journal_issue                   3
_journal_name_full               'Acta Crystallographica Section C'
_journal_page_first
;
;
_journal_paper_doi               10.1107/S2053229620002466
_journal_volume                  76
_journal_year                    2020
_chemical_formula_iupac          'K2 [Mn3 (P2 O7)2 (H2 O)2]'
_chemical_formula_moiety         'H4 K2 Mn3 O16 P4'
_chemical_formula_sum            'H4 K2 Mn3 O16 P4'
_chemical_formula_weight         626.93
_chemical_name_common            'Potassium manganese pyrophosphate hydrate'
_chemical_name_systematic
'Dipotassium trimanganese dipyrophosphate dihydrate'
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2ybc'
_space_group_name_H-M_alt        'P 1 21/c 1'
_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                 98.9240(10)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   9.19440(10)
_cell_length_b                   8.31340(10)
_cell_length_c                   9.3798(2)
_cell_measurement_reflns_used    6532
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      32.2460
_cell_measurement_theta_min      3.2920
_cell_volume                     708.282(19)
_computing_cell_refinement
;
CrysAlis PRO (Agilent, 2014)
;
_computing_data_collection
;
CrysAlis PRO (Agilent, 2014)
;
_computing_data_reduction
;
CrysAlis PRO (Agilent, 2014)
;
_computing_molecular_graphics
;
DIAMOND (Brandenburg, 2006)
;
_computing_publication_material
;
WinGX (Farrugia, 2012) and
<i>International Tables for Crystallography</i> (2004)
;
_computing_structure_refinement
;
SHELXL2016 (Sheldrick, 2015b)
;
_computing_structure_solution
;
SHELXT (Sheldrick, 2015a)
;
_diffrn_ambient_temperature      293(2)
_diffrn_detector_area_resol_mean 16.0630
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 1.000
_diffrn_measurement_device_type  'Agilent Xcalibur Sapphire3'
_diffrn_measurement_method       \w
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0430
_diffrn_reflns_av_unetI/netI     0.0269
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_l_max       13
_diffrn_reflns_limit_l_min       -13
_diffrn_reflns_number            13181
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         29.994
_diffrn_reflns_theta_min         3.292
_diffrn_source                   'Enhance (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    3.762
_exptl_absorpt_correction_T_max  0.787
_exptl_absorpt_correction_T_min  0.703
_exptl_absorpt_correction_type   gaussian
_exptl_absorpt_process_details
;
(CrysAlis PRO; Agilent, 2014)
;
_exptl_crystal_colour            'light pink'
_exptl_crystal_density_diffrn    2.940
_exptl_crystal_description       cube
_exptl_crystal_F_000             610
_exptl_crystal_size_max          0.141
_exptl_crystal_size_mid          0.093
_exptl_crystal_size_min          0.076
_refine_diff_density_max         0.411
_refine_diff_density_min         -0.454
_refine_ls_extinction_coef       0.0026(5)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method
;
SHELXL2016 (Sheldrick, 2015b)
;
_refine_ls_goodness_of_fit_ref   1.075
_refine_ls_hydrogen_treatment    refall
_refine_ls_matrix_type           full
_refine_ls_number_parameters     124
_refine_ls_number_reflns         2062
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.075
_refine_ls_R_factor_all          0.0271
_refine_ls_R_factor_gt           0.0233
_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/[\s^2^(Fo^2^)+(0.0160P)^2^+0.6000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0497
_refine_ls_wR_factor_ref         0.0511
_reflns_number_gt                1878
_reflns_number_total             2062
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            fn3331sup1.cif
_cod_data_source_block           I
_cod_original_sg_symbol_H-M      'P 21/c'
_cod_database_code               2021990
_shelx_estimated_absorpt_t_min   0.619
_shelx_estimated_absorpt_t_max   0.763
_shelx_hkl_checksum              86826
_shelx_res_checksum              52112
_cod_database_fobs_code 2021990