KZn(HP~2~O~7~)·2H~2~O and KMn(HP~2~O~7~)·2H~2~O: acid pyrophosphate metallates(II) with layer structures
Assaaoudi, Hassane; Ennaciri, Abdelaziz; Harcharras, Mohamed; El Bali, Brahim; Reinauer, Felix; Glaum, Robert; Rulmont, André; Spirlet, Marie-Rose; Acta Crystallographica Section C 58 (2002) i79–i81; doi:10.1107/S0108270102007394

data_2012742
_publ_section_title
;
 KZn(HP~2~O~7~)&#x00B7;2H~2~O and KMn(HP~2~O~7~)&#x00B7;2H~2~O: acid
 pyrophosphate metallates(II) with layer structures
;
_journal_issue                   6
_journal_name_full               'Acta Crystallographica Section C'
_journal_page_first              i79
_journal_page_last               i81
_journal_paper_doi               10.1107/S0108270102007394
_journal_volume                  58
_journal_year                    2002
_chemical_formula_iupac          'K Mn (H P2 O7) (H2 O)2'
_chemical_formula_structural     'K Mn (H P2 O7) (H2 O)2'
_chemical_formula_sum            'H5 K Mn O9 P2'
_chemical_formula_weight         305.02
_chemical_name_systematic
;
potassium manganese(II) hydrogenpyrophosphate dihydrate
;
_space_group_IT_number           62
_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_Hall  '-P 2ac 2n'
_symmetry_space_group_name_H-M   'P n m a'
_atom_sites_solution_hydrogens   difmap
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   15.7186(5)
_cell_length_b                   7.8706(5)
_cell_length_c                   6.5297(5)
_cell_measurement_reflns_used    21
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      25.0
_cell_measurement_theta_min      5.0
_cell_volume                     807.82(8)
_computing_cell_refinement       'CAD-4 EXPRESS'
_computing_data_collection       'CAD-4 EXPRESS (Enraf-Nonius, 1994)'
_computing_data_reduction        'XCAD4 (Harms & Wocadlo, 1995)'
_computing_molecular_graphics    'ATOMS (Dowty, 1998)'
_computing_structure_refinement  'SHELXL97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS97 (Sheldrick, 1997)'
_diffrn_ambient_temperature      293(2)
_diffrn_measurement_device       '\k-geometry diffractometer'
_diffrn_measurement_device_type  'Enraf Nonius CAD-4'
_diffrn_measurement_method       'non-profiled \w'
_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  0.0458
_diffrn_reflns_av_sigmaI/netI    0.0248
_diffrn_reflns_limit_h_max       28
_diffrn_reflns_limit_h_min       -22
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       11
_diffrn_reflns_limit_l_min       -11
_diffrn_reflns_number            17404
_diffrn_reflns_theta_full        39.95
_diffrn_reflns_theta_max         39.95
_diffrn_reflns_theta_min         2.59
_diffrn_standards_decay_%        0
_diffrn_standards_interval_time  60
_diffrn_standards_number         3
_exptl_absorpt_coefficient_mu    2.568
_exptl_absorpt_correction_T_max  0.6018
_exptl_absorpt_correction_T_min  0.5316
_exptl_absorpt_correction_type   '\y scan'
_exptl_absorpt_process_details
;
Number of psi-scan sets used was 9.
Theta correction was applied.
Averaged transmission function was used.
No Fourier smoothing was applied
'North & al. (1968)'
;
_exptl_crystal_colour            pink
_exptl_crystal_density_diffrn    2.508
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prismatic
_exptl_crystal_F_000             604
_exptl_crystal_size_max          0.30
_exptl_crystal_size_mid          0.30
_exptl_crystal_size_min          0.30
_refine_diff_density_max         0.725
_refine_diff_density_min         -0.463
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.061
_refine_ls_hydrogen_treatment    refall
_refine_ls_matrix_type           full
_refine_ls_number_parameters     79
_refine_ls_number_reflns         2633
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.061
_refine_ls_R_factor_all          0.0316
_refine_ls_R_factor_gt           0.0241
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w = 1/[\s^2^(Fo^2^)+(0.0305P)^2^+0.2440P] where P = (Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0586
_refine_ls_wR_factor_ref         0.0613
_reflns_number_gt                2278
_reflns_number_total             2633
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            br1366.cif
_cod_data_source_block           II
_cod_database_code               2012742