A monoclinic pseudopolymorph of manganese squarate dihydrate, Mn(μ-C~4~O~4~)(H~2~O)~2~, built from cubic units
Gavilan, Elisabeth; Audebrand, Nathalie; Acta Crystallographica Section C 65 (2009) m156–m159; doi:10.1107/S0108270109004442

data_2017028
_publ_section_title
;
 A monoclinic pseudopolymorph of manganese squarate dihydrate,
 Mn(\m-C~4~O~4~)(H~2~O)~2~, built from cubic units
;
_journal_coeditor_code           DN3102
_journal_issue                   4
_journal_name_full               'Acta Crystallographica Section C'
_journal_page_first              m156
_journal_page_last               m159
_journal_paper_doi               10.1107/S0108270109004442
_journal_volume                  65
_journal_year                    2009
_chemical_formula_iupac          '[Mn3 (C4 O4)3 (H2 O)6], H2 O1'
_chemical_formula_moiety         'C12 H12 Mn3 O18, H2 O1'
_chemical_formula_sum            'C12 H14 Mn3 O19'
_chemical_formula_weight         627.04
_chemical_name_common            'Manganese squarate hexahydrate'
_chemical_name_systematic
;
poly[[[hexaaquatrimanganese(II)]-tri-\m-squarato] monohydrate]
;
_space_group_IT_number           15
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-C 2yc'
_symmetry_space_group_name_H-M   'C 1 2/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_cell_angle_alpha                90.00
_cell_angle_beta                 90.0840(10)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   11.5921(2)
_cell_length_b                   11.8471(2)
_cell_length_c                   16.5666(7)
_cell_measurement_reflns_used    13776
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      34.972
_cell_measurement_theta_min      2.546
_cell_volume                     2275.13(11)
_computing_cell_refinement       'SCALEPACK (Otwinowski & Minor, 1997)'
_computing_data_collection       'COLLECT (Nonius, 1998)'
_computing_data_reduction
'DENZO and SCALEPACK (Otwinowski & Minor, 1997)'
_computing_molecular_graphics
'PLATON (Spek, 2009) and DIAMOND (Brandenburg & Berndt, 2001)'
_computing_publication_material  'WinGX (Farrugia, 1999)'
_computing_structure_refinement  'SHELXL97 (Sheldrick, 2008)'
_computing_structure_solution    'SIR97 (Altomare <i>et al.</i>,  1999)'
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 0.990
_diffrn_measured_fraction_theta_max 0.990
_diffrn_measurement_device_type  'Nonius KappaCCD'
_diffrn_measurement_method       'Nonius CCD'
_diffrn_radiation_monochromator  'horizonally mounted graphite crystal'
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0300
_diffrn_reflns_av_sigmaI/netI    0.0388
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -18
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       26
_diffrn_reflns_limit_l_min       -26
_diffrn_reflns_number            19216
_diffrn_reflns_theta_full        35.04
_diffrn_reflns_theta_max         35.04
_diffrn_reflns_theta_min         3.52
_exptl_absorpt_coefficient_mu    1.73
_exptl_absorpt_correction_T_max  0.7585
_exptl_absorpt_correction_T_min  0.7390
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   '(Blessing, 1995)'
_exptl_crystal_colour            brown
_exptl_crystal_density_diffrn    1.83
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             1252
_exptl_crystal_size_max          0.19
_exptl_crystal_size_mid          0.17
_exptl_crystal_size_min          0.17
_refine_diff_density_max         1.306
_refine_diff_density_min         -0.423
_refine_ls_extinction_coef       0.0013(2)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     '(SHELXL97; Sheldrick, 2008)'
_refine_ls_goodness_of_fit_ref   1.045
_refine_ls_hydrogen_treatment    refxyz
_refine_ls_matrix_type           full
_refine_ls_number_parameters     172
_refine_ls_number_reflns         4984
_refine_ls_number_restraints     9
_refine_ls_restrained_S_all      1.045
_refine_ls_R_factor_all          0.0702
_refine_ls_R_factor_gt           0.0377
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0472P)^2^+2.1926P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0913
_refine_ls_wR_factor_ref         0.1015
_reflns_number_gt                3452
_reflns_number_total             4984
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            dn3102.cif
_cod_data_source_block           I
_cod_original_sg_symbol_H-M      'C 2/c'
_cod_database_code               2017028
_cod_database_fobs_code          2017028