Hydrothermal synthesis, crystal structure, spectroscopic and magnetic properties of Mn4(H2O)3(SeO3)4 and Mn3(H2O)(SeO3)3
Aitor Larrañaga; José L. Mesa; José L. Pizarro; R. Olazcuaga; María I. Arriortua; Teófilo Rojo; J. Chem. Soc., Dalton Trans.  (2002) 3447–3453; doi:10.1039/b206515k

data_7011992
_publ_section_title
;
 Hydrothermal synthesis, crystal structure, spectroscopic and magnetic
 properties of Mn4(H2O)3(SeO3)4 and Mn3(H2O)(SeO3)3
;
_journal_issue                   18
_journal_name_full               'J. Chem. Soc., Dalton Trans.'
_journal_page_first              3447
_journal_page_last               3453
_journal_paper_doi               10.1039/b206515k
_journal_year                    2002
_chemical_compound_source        'synthesis as described'
_chemical_formula_moiety         'H6 Mn4 O15 Se4'
_chemical_formula_structural     'H6 MN4 O15 SE4'
_chemical_formula_sum            'H6 Mn4 O15 Se4'
_chemical_formula_weight         781.65
_space_group_IT_number           4
_symmetry_cell_setting           monoclinic
_symmetry_Int_Tables_number      4
_symmetry_space_group_name_Hall  'P 2yb'
_symmetry_space_group_name_H-M   'P 1 21 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_conform_dict_location     ftp://ftp.iucr.org/cifdics/cif_core.dic
_audit_conform_dict_name         cif_core.dic
_audit_conform_dict_version      2.1
_audit_creation_date             2002-06-13T15:45:34-00:00
_audit_creation_method           'WinGX routine CIF_UPDATE'
_cell_angle_alpha                90
_cell_angle_beta                 116.63(2)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   9.181(2)
_cell_length_b                   8.602(3)
_cell_length_c                   9.852(4)
_cell_measurement_reflns_used    25
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      13
_cell_measurement_theta_min      6
_cell_measurement_wavelength     0.71073
_cell_volume                     695.5(4)
_computing_cell_refinement       'CAD4 Express (Enraf Nonius, 1994)'
_computing_data_collection       'CAD4 Express (Enraf Nonius, 1994)'
_computing_data_reduction        'XCAD4 (Harms & Wocadlo, 1995)'
_computing_molecular_graphics    'Ortep-3 for Windows (Farrugia, 1997)'
_computing_publication_material  'WinGX publication routines (Farrugia, 1999)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1997)'
_diffrn_ambient_temperature      293(2)
_diffrn_detector                 'scintillation LiI'
_diffrn_detector_dtime           1.195
_diffrn_measured_fraction_theta_full 0.986
_diffrn_measured_fraction_theta_max 0.986
_diffrn_measurement_device       '\k-geometry diffractometer'
_diffrn_measurement_device_type  'Enraf Nonius CAD4'
_diffrn_measurement_method       'non-profiled omega/2theta scans'
_diffrn_orient_matrix_type
;
x-axis points to radiation source
the matrix is specified in reciprocal space
;
_diffrn_orient_matrix_UB_11      0.98039E-1
_diffrn_orient_matrix_UB_12      0.5158E-2
_diffrn_orient_matrix_UB_13      0.8459E-2
_diffrn_orient_matrix_UB_21      0.19951E-1
_diffrn_orient_matrix_UB_22      -0.5749E-2
_diffrn_orient_matrix_UB_23      -0.29692E-1
_diffrn_orient_matrix_UB_31      -0.3369E-2
_diffrn_orient_matrix_UB_32      0.116068
_diffrn_orient_matrix_UB_33      -0.1846E-2
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.7107
_diffrn_reflns_av_R_equivalents  0.0444
_diffrn_reflns_av_unetI/netI     0.083
_diffrn_reflns_limit_h_max       5
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       0
_diffrn_reflns_limit_k_min       -10
_diffrn_reflns_limit_l_max       11
_diffrn_reflns_limit_l_min       -5
_diffrn_reflns_number            1334
_diffrn_reflns_theta_full        24.98
_diffrn_reflns_theta_max         24.98
_diffrn_reflns_theta_min         2.31
_diffrn_source                   'Enraf Nonius FR590'
_diffrn_standards_decay_%        0
_diffrn_standards_interval_count 94
_diffrn_standards_interval_time  60
_diffrn_standards_number         2
_exptl_absorpt_coefficient_mu    14.093
_exptl_absorpt_correction_T_max  0.3206
_exptl_absorpt_correction_T_min  0.1927
_exptl_absorpt_correction_type   psi-scan
_exptl_absorpt_process_details
;
North A.C.T., Phillips D.C. & Mathews F.S. (1968) Acta. Cryst. A24, 351
Number of psi-scan sets used was   8
Theta correction was applied.
Weighted transmission curves were used.
No Fourier smoothing was applied.
;
_exptl_crystal_colour            'pale pink'
_exptl_crystal_density_diffrn    3.732
_exptl_crystal_density_meas      3.6
_exptl_crystal_density_method    Picnometry
_exptl_crystal_description       acicular
_exptl_crystal_F_000             724
_exptl_crystal_size_max          0.4
_exptl_crystal_size_mid          0.07
_exptl_crystal_size_min          0.02
_refine_diff_density_max         2.065
_refine_diff_density_min         -1.55
_refine_diff_density_rms         0.39
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   0.16(4)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.06
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     133
_refine_ls_number_reflns         1290
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.06
_refine_ls_R_factor_all          0.0597
_refine_ls_R_factor_gt           0.0563
_refine_ls_shift/su_max          0
_refine_ls_shift/su_mean         0
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0857P)^2^+11.9607P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.152
_refine_ls_wR_factor_ref         0.1562
_reflns_number_gt                1204
_reflns_number_total             1290
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            b206515k.txt
_cod_data_source_block           mnt2pnab
_cod_original_sg_symbol_H-M      'P 21'
_cod_database_code               7011992
_exptl_absorpt_factor_mur        1.126
_exptl_absorpt_correction_t_ave  0.2615
_diffrn_standards_decay_corr_max 1
_diffrn_standards_decay_corr_min 1