M3(P2O7)2(2-)-Type Open Frameworks Featuring [M2O8] and [M3O12] Multinuclear Transition-Metal Oxide Units. Serendipitous Synthesis of Six Polymorphic Salt-Inclusion Magnetic Solids: Na2M3(P2O7)2·ACl (M = Mn, Fe; A = Rb, Cs) and K2M3(P2O7)2·CsCl (M = Fe, Mn).
Gao, Jianhua; Li, Jian; Sulejmanovic, Dino; Hwu, Shiou-Jyh; Inorganic chemistry 54 (2015) 1136–1144; doi:10.1021/ic5024696

data_4341744
_publ_section_title
;
 M3(P2O7)2(2-)-Type Open Frameworks Featuring [M2O8] and [M3O12]
 Multinuclear Transition-Metal Oxide Units. Serendipitous Synthesis of Six
 Polymorphic Salt-Inclusion Magnetic Solids: Na2M3(P2O7)2&#x00B7;ACl (M =
 Mn, Fe; A = Rb, Cs) and K2M3(P2O7)2&#x00B7;CsCl (M = Fe, Mn).
;
_journal_issue                   3
_journal_name_full               'Inorganic chemistry'
_journal_page_first              1136
_journal_page_last               1144
_journal_paper_doi               10.1021/ic5024696
_journal_volume                  54
_journal_year                    2015
_chemical_formula_sum            'Cl Cs Fe3 K2 O14 P4'
_chemical_formula_weight         761.98
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   none
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                79.41(3)
_cell_angle_beta                 76.04(3)
_cell_angle_gamma                89.66(3)
_cell_formula_units_Z            1
_cell_length_a                   5.3125(11)
_cell_length_b                   7.6130(15)
_cell_length_c                   9.6697(19)
_cell_measurement_temperature    293(2)
_cell_volume                     372.76(14)
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 0.979
_diffrn_measured_fraction_theta_max 0.979
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0294
_diffrn_reflns_av_sigmaI/netI    0.0301
_diffrn_reflns_limit_h_max       6
_diffrn_reflns_limit_h_min       -5
_diffrn_reflns_limit_k_max       9
_diffrn_reflns_limit_k_min       -9
_diffrn_reflns_limit_l_max       12
_diffrn_reflns_limit_l_min       -12
_diffrn_reflns_number            3459
_diffrn_reflns_theta_full        26.37
_diffrn_reflns_theta_max         26.37
_diffrn_reflns_theta_min         2.21
_exptl_absorpt_coefficient_mu    6.525
_exptl_absorpt_correction_T_max  0.593
_exptl_absorpt_correction_T_min  0.406
_exptl_absorpt_correction_type   empirical
_exptl_crystal_colour            'light brown'
_exptl_crystal_density_diffrn    3.395
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             360
_exptl_crystal_size_max          0.16
_exptl_crystal_size_mid          0.12
_exptl_crystal_size_min          0.08
_refine_diff_density_max         1.944
_refine_diff_density_min         -1.181
_refine_diff_density_rms         0.216
_refine_ls_extinction_coef       0.007(2)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     SHELXL
_refine_ls_goodness_of_fit_ref   1.102
_refine_ls_hydrogen_treatment    none
_refine_ls_matrix_type           full
_refine_ls_number_parameters     119
_refine_ls_number_reflns         1496
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.102
_refine_ls_R_factor_all          0.0443
_refine_ls_R_factor_gt           0.0433
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0543P)^2^+3.4690P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1138
_refine_ls_wR_factor_ref         0.1147
_reflns_number_gt                1440
_reflns_number_total             1529
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic5024696_si_002.cif
_cod_data_source_block           K2Fe3(P2O7)2CsCl_(6)
_cod_depositor_comments
'Adding full bibliography for 4341739--4341744.cif.'
_cod_original_cell_volume        372.76(13)
_cod_original_sg_symbol_H-M      P-1
_cod_database_code               4341744