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_2108555
_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         'Cs, Mn, B O8 P2, O H'
_chemical_formula_sum            'B Cs H Mn O9 P2'
_chemical_formula_weight         405.61
_chemical_name_common            'Caesium manganese borophosphate hydroxide'
_chemical_name_systematic
;         
Caesium manganese (III) Borodiphosphate Hydroxide
;
_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-2014/7
_cell_angle_alpha                90
_cell_angle_beta                 100.141(2)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   9.1494(3)
_cell_length_b                   8.6991(2)
_cell_length_c                   9.6413(3)
_cell_measurement_reflns_used    5939
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      31.6600
_cell_measurement_theta_min      3.1700
_cell_volume                     755.38(4)
_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
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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 0.999
_diffrn_measured_fraction_theta_max 1.000
_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  0.0505
_diffrn_reflns_av_unetI/netI     0.0317
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 1.000
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       13
_diffrn_reflns_limit_l_min       -13
_diffrn_reflns_number            14159
_diffrn_reflns_point_group_measured_fraction_full 0.999
_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         3.177
_diffrn_source                   'Enhance (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    6.947
_exptl_absorpt_correction_T_max  0.682
_exptl_absorpt_correction_T_min  0.631
_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            purple
_exptl_crystal_density_diffrn    3.567
_exptl_crystal_description       ambiguous
_exptl_crystal_F_000             752
_exptl_crystal_size_max          0.090
_exptl_crystal_size_mid          0.080
_exptl_crystal_size_min          0.070
_refine_diff_density_max         1.023
_refine_diff_density_min         -1.153
_refine_diff_density_rms         0.158
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.161
_refine_ls_hydrogen_treatment    refall
_refine_ls_matrix_type           full
_refine_ls_number_parameters     131
_refine_ls_number_reflns         2203
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.161
_refine_ls_R_factor_all          0.0353
_refine_ls_R_factor_gt           0.0294
_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^)+(0.0129P)^2^+1.6434P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0532
_refine_ls_wR_factor_ref         0.0551
_reflns_Friedel_coverage         0.000
_reflns_number_gt                1998
_reflns_number_total             2203
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            je5022sup1.cif
_cod_data_source_block           III
_cod_original_sg_symbol_H-M      'P 21/c'
_cod_original_formula_sum        'B1 Cs1 H1 Mn1 O9 P2'
_cod_database_code               2108555
_shelx_shelxl_version_number     2014/7
_shelx_estimated_absorpt_t_min   0.574
_shelx_estimated_absorpt_t_max   0.642
_shelx_res_checksum              87162
_shelx_hkl_checksum              72050
_cod_database_fobs_code 2108555