Chain caesium borophosphates with B:P ratio 1:2: synthesis, structure relationships and low-temperature thermodynamic properties
Shvanskaya, Larisa; Yakubovich, Olga; Krikunova, Polina; Ovchenkov, Evgeny; Vasiliev, Alexander; Acta Crystallographica Section B 75 (2019) –; doi:10.1107/S2052520619013763

data_2108554
_publ_section_title
;
 Chain caesium borophosphates with B:P ratio 1:2: synthesis, structure
 relationships and low-temperature thermodynamic properties
;
_journal_issue                   6
_journal_name_full               'Acta Crystallographica Section B'
_journal_page_first
;
;
_journal_paper_doi               10.1107/S2052520619013763
_journal_volume                  75
_journal_year                    2019
_chemical_formula_moiety
'Cs0.51 Mn1.17, 2(H2 O), B1 P2 O8, 0.45(H2 O)'
_chemical_formula_sum            'B Cs0.51 H4.9 Mn1.17 O10.45 P2'
_chemical_formula_weight         380.66
_chemical_name_common            'Caesium manganese borophosphate hydrate'
_chemical_name_systematic
;         
Caesium Diaquamanganese (II,III) Borodiphosphate Hydrate
;
_space_group_crystal_system      hexagonal
_space_group_IT_number           178
_space_group_name_Hall           'P 61 2 (0 0 5)'
_space_group_name_H-M_alt        'P 61 2 2'
_atom_sites_solution_hydrogens   difmap
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-2014/7
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                120
_cell_formula_units_Z            6
_cell_length_a                   9.6292(3)
_cell_length_b                   9.6292(3)
_cell_length_c                   15.8051(5)
_cell_measurement_reflns_used    3809
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      23.8340
_cell_measurement_theta_min      3.5330
_cell_volume                     1269.14(7)
_computing_cell_refinement
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.35 (release 13-08-2014 CrysAlis171 .NET)
(compiled Aug 13 2014,18:06:01)
;
_computing_data_collection
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.35 (release 13-08-2014 CrysAlis171 .NET)
(compiled Aug 13 2014,18:06:01)
;
_computing_data_reduction
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.35 (release 13-08-2014 CrysAlis171 .NET)
(compiled Aug 13 2014,18:06:01)
;
_computing_molecular_graphics    'DIMOND (Brandenburg, 2006)'
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_structure_solution    'SHELXS-2014/7 (Sheldrick, 2014)'
_diffrn_ambient_temperature      293(2)
_diffrn_detector_area_resol_mean 16.0630
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measurement_device_type  'Xcalibur, Sapphire3'
_diffrn_measurement_method       \w
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.1088
_diffrn_reflns_av_unetI/netI     0.0463
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.997
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            21747
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         29.997
_diffrn_reflns_theta_min         2.762
_diffrn_source                   'Enhance (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    4.409
_exptl_absorpt_correction_T_max  0.878
_exptl_absorpt_correction_T_min  0.746
_exptl_absorpt_correction_type   gaussian
_exptl_absorpt_process_details
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.35 (release 13-08-2014 CrysAlis171 .NET)
(compiled Aug 13 2014,18:06:01)
Numerical absorption correction based on gaussian integration over
   a multifaceted crystal model
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            'light blue'
_exptl_crystal_density_diffrn    2.956
_exptl_crystal_description       'Hexagonal bipyramide'
_exptl_crystal_F_000             1081
_exptl_crystal_size_max          0.070
_exptl_crystal_size_mid          0.050
_exptl_crystal_size_min          0.030
_refine_diff_density_max         0.641
_refine_diff_density_min         -0.519
_refine_diff_density_rms         0.119
_refine_ls_abs_structure_details
;
 Flack x determined using 345 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   0.04(3)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.264
_refine_ls_hydrogen_treatment    refall
_refine_ls_matrix_type           full
_refine_ls_number_parameters     98
_refine_ls_number_reflns         1242
_refine_ls_number_restraints     2
_refine_ls_restrained_S_all      1.263
_refine_ls_R_factor_all          0.0699
_refine_ls_R_factor_gt           0.0614
_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^)+(0.0164P)^2^+4.9684P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0960
_refine_ls_wR_factor_ref         0.0987
_reflns_Friedel_coverage         0.568
_reflns_Friedel_fraction_full    1.000
_reflns_Friedel_fraction_max     1.000
_reflns_number_gt                1162
_reflns_number_total             1242
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            je5022sup1.cif
_cod_data_source_block           II
_cod_original_cell_volume        1269.14(9)
_cod_original_sg_symbol_Hall     'P 61 2 (0 0 -1)'
_cod_original_formula_sum        'B1 Cs0.51 H4.9 Mn1.17 O10.45 P2'
_cod_database_code               2108554
_shelx_shelxl_version_number     2014/7
_shelx_estimated_absorpt_t_min   0.748
_shelx_estimated_absorpt_t_max   0.879
_shelx_res_checksum              69515
_shelx_hkl_checksum              9011
_cod_database_fobs_code 2108554