#------------------------------------------------------------------------------
#$Date: 2016-02-14 16:26:36 +0200 (Sun, 14 Feb 2016) $
#$Revision: 176435 $
#$URL: svn://www.crystallography.net/cod/cif/2/20/13/2201302.cif $
#------------------------------------------------------------------------------
#
# This file is available in the Crystallography Open Database (COD),
# http://www.crystallography.net/. The original data for this entry
# were provided by IUCr Journals, http://journals.iucr.org/.
#
# The file may be used within the scientific community so long as
# proper attribution is given to the journal article from which the
# data were obtained.
#
data_2201302
loop_
_publ_author_name
'Greve, Jan'
'Näther, Christian'
_publ_section_title
;Poly[[diaqua(μ₄-squarato-O,O',O'',O''')manganese(II)]
 0.93-hydrate]
;
_journal_issue                   11
_journal_name_full               'Acta Crystallographica Section E'
_journal_page_first              m625
_journal_page_last               m627
_journal_paper_doi               10.1107/S1600536802018329
_journal_volume                  58
_journal_year                    2002
_chemical_formula_iupac          '[Mn (C4 O4) (H2 O1)2], 0.93H2 O'
_chemical_formula_moiety         'C4 H4 O6 Mn, 0.93H2 O'
_chemical_formula_sum            'C4 H5.86 Mn O6.93'
_chemical_formula_weight         219.77
_chemical_melting_point          'decomposes at about 250\%C'
_chemical_name_common
;
Poly[[diaqua(μ₄-squarato-O,O',O'',O''')manganese(II)] 0.93-hydrate]
;
_chemical_name_systematic
;
Poly[[diaqua(μ₄-squarato-O,O',O'',O''')manganese(II)] 0.93-hydrate]
;
_space_group_IT_number           222
_symmetry_cell_setting           cubic
_symmetry_space_group_name_Hall  '-P 4a 2bc 3'
_symmetry_space_group_name_H-M   'P n -3 n :2'
_atom_sites_solution_hydrogens   geom
_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            24
_cell_length_a                   16.5527(8)
_cell_length_b                   16.5527(8)
_cell_length_c                   16.5527(8)
_cell_measurement_reflns_used    8000
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      28
_cell_measurement_theta_min      2.5
_cell_volume                     4535.3(4)
_computing_cell_refinement       'IPDS Program Package'
_computing_data_collection       'IPDS Program Package (Stoe & Cie, 1998)'
_computing_data_reduction        'IPDS Program Package'
_computing_molecular_graphics    'XP in SHELXTL (Bruker, 1998)'
_computing_publication_material  'CIFTAB in SHELXL97'
_computing_structure_refinement  'SHELXL97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS97 (Sheldrick, 1997)'
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 0.980
_diffrn_measured_fraction_theta_max 0.980
_diffrn_measurement_device_type  'Stoe IPDS'
_diffrn_measurement_method       φ
_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  0.0494
_diffrn_reflns_av_sigmaI/netI    0.0127
_diffrn_reflns_limit_h_max       21
_diffrn_reflns_limit_h_min       -21
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -21
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            28798
_diffrn_reflns_theta_full        27.99
_diffrn_reflns_theta_max         27.99
_diffrn_reflns_theta_min         3.89
_diffrn_standards_decay_%        none
_diffrn_standards_interval_count 0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    1.74
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.931
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             2602
_exptl_crystal_size_max          0.15
_exptl_crystal_size_mid          0.05
_exptl_crystal_size_min          0.05
_refine_diff_density_max         0.733
_refine_diff_density_min         -0.650
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.179
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     58
_refine_ls_number_reflns         908
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.179
_refine_ls_R_factor_all          0.0396
_refine_ls_R_factor_gt           0.0370
_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/[σ²(Fo²)+(0.0485P)²+5.7874P] where P = (Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1109
_refine_ls_wR_factor_ref         0.1125
_reflns_number_gt                821
_reflns_number_total             908
_reflns_threshold_expression     I>2σ(I)
_cod_data_source_file            bt6191.cif
_cod_data_source_block           I
_cod_original_sg_symbol_H-M      'P n -3 n'
_cod_original_formula_sum        'C4 H5.86 Mn O6.93 '
_cod_database_code               2201302
_cod_database_fobs_code          2201302
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x+1/2, -y+1/2, z'
'-x+1/2, y, -z+1/2'
'x, -y+1/2, -z+1/2'
'z, x, y'
'z, -x+1/2, -y+1/2'
'-z+1/2, -x+1/2, y'
'-z+1/2, x, -y+1/2'
'y, z, x'
'-y+1/2, z, -x+1/2'
'y, -z+1/2, -x+1/2'
'-y+1/2, -z+1/2, x'
'y, x, -z+1/2'
'-y+1/2, -x+1/2, -z+1/2'
'y, -x+1/2, z'
'-y+1/2, x, z'
'x, z, -y+1/2'
'-x+1/2, z, y'
'-x+1/2, -z+1/2, -y+1/2'
'x, -z+1/2, y'
'z, y, -x+1/2'
'z, -y+1/2, x'
'-z+1/2, y, x'
'-z+1/2, -y+1/2, -x+1/2'
'-x, -y, -z'
'x-1/2, y-1/2, -z'
'x-1/2, -y, z-1/2'
'-x, y-1/2, z-1/2'
'-z, -x, -y'
'-z, x-1/2, y-1/2'
'z-1/2, x-1/2, -y'
'z-1/2, -x, y-1/2'
'-y, -z, -x'
'y-1/2, -z, x-1/2'
'-y, z-1/2, x-1/2'
'y-1/2, z-1/2, -x'
'-y, -x, z-1/2'
'y-1/2, x-1/2, z-1/2'
'-y, x-1/2, -z'
'y-1/2, -x, -z'
'-x, -z, y-1/2'
'x-1/2, -z, -y'
'x-1/2, z-1/2, y-1/2'
'-x, z-1/2, -y'
'-z, -y, x-1/2'
'-z, y-1/2, -x'
'z-1/2, -y, -x'
'z-1/2, y-1/2, x-1/2'
loop_
_atom_site_label
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
_atom_site_type_symbol
Mn 0.498174(14) 0.498174(14) 0.2500 0.0081(2) Uani d S 1 . . Mn
C1 0.30833(10) 0.48233(11) 0.22723(10) 0.0127(4) Uani d . 1 . . C
O1 0.37797(8) 0.48637(9) 0.19862(8) 0.0193(4) Uani d . 1 . . O
C2 0.50060(11) 0.69129(11) 0.22832(12) 0.0151(4) Uani d . 1 . . C
O2 0.50295(9) 0.62095(8) 0.20098(8) 0.0216(4) Uani d . 1 . . O
O3 0.45951(9) 0.53810(9) 0.36679(9) 0.0204(4) Uani d . 1 . . O
H1 0.4126 0.5195 0.3793 0.031 Uiso d R 1 . . H
H2 0.4690 0.5877 0.3790 0.031 Uiso d R 1 . . H
O4 0.2500 0.6703(13) 0.2500 0.143(7) Uiso d SP 0.48(2) . . O
O5 0.7016(11) 0.7039(11) 0.2082(8) 0.143(7) Uiso d P 0.345(15) . . O
loop_
_atom_site_aniso_label
_atom_site_aniso_U_11
_atom_site_aniso_U_22
_atom_site_aniso_U_33
_atom_site_aniso_U_12
_atom_site_aniso_U_13
_atom_site_aniso_U_23
Mn 0.0080(2) 0.0080(2) 0.0083(3) 0.00028(11) -0.00055(8) 0.00055(8)
C1 0.0084(8) 0.0213(9) 0.0083(7) 0.0013(7) -0.0001(6) 0.0003(7)
O1 0.0064(6) 0.0406(9) 0.0109(6) -0.0002(5) 0.0008(5) 0.0017(6)
C2 0.0271(10) 0.0092(8) 0.0092(8) -0.0003(6) 0.0010(6) 0.0003(6)
O2 0.0467(9) 0.0066(6) 0.0115(6) 0.0005(5) 0.0029(5) -0.0009(5)
O3 0.0215(7) 0.0207(7) 0.0190(7) -0.0053(5) 0.0086(5) -0.0087(5)
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Mn Mn 0.3368 0.7283 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle
_geom_angle_publ_flag
O3 Mn O3 . 13 179.21(8) y
O3 Mn O1 . . 96.17(5) n
O3 Mn O1 13 . 84.40(5) y
O3 Mn O1 . 13 84.40(5) n
O3 Mn O1 13 13 96.17(5) y
O1 Mn O1 . 13 89.34(8) y
O3 Mn O2 . 13 86.09(5) y
O3 Mn O2 13 13 93.37(5) y
O1 Mn O2 . 13 176.62(6) y
O1 Mn O2 13 13 88.37(6) n
O3 Mn O2 . . 93.37(5) n
O3 Mn O2 13 . 86.09(5) n
O1 Mn O2 . . 88.37(6) y
O1 Mn O2 13 . 176.62(6) n
O2 Mn O2 13 . 94.03(8) y
O1 C1 C1 . 23 135.93(19) y
O1 C1 C1 . 21 133.91(19) y
C1 C1 C1 23 21 90.0 y
C1 O1 Mn . . 134.60(12) y
O2 C2 C2 . 44_666 136.0(2) y
O2 C2 C2 . 41_665 134.0(2) y
C2 C2 C2 44_666 41_665 89.990(4) y
C2 O2 Mn . . 136.83(13) y
Mn O3 H1 . . 112.2 n
Mn O3 H2 . . 116.8 n
H1 O3 H2 . . 116.8 n
O5 O4 O5 44_666 43_565 121(2) n
O5 O4 O5 44_666 36_566 75.9(11) n
O5 O4 O5 43_565 36_566 75.9(11) n
O5 O4 O5 44_666 35_665 75.9(11) n
O5 O4 O5 43_565 35_665 75.9(11) n
O5 O4 O5 36_566 35_665 121(2) n
O4 O5 O5 30_665 13 119.4(12) n
O4 O5 O5 30_665 15_565 52.0(5) n
O5 O5 O5 13 15_565 91.6(11) n
O4 O5 O5 30_665 16_655 52.0(5) n
O5 O5 O5 13 16_655 88.4(12) n
O5 O5 O5 15_565 16_655 90.000(7) n
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_site_symmetry_2
_geom_bond_distance
_geom_bond_publ_flag
Mn O3 . 2.1409(14) y
Mn O3 13 2.1409(14) n
Mn O1 . 2.1727(13) y
Mn O1 13 2.1727(13) n
Mn O2 13 2.1898(13) n
Mn O2 . 2.1898(13) y
C1 O1 . 1.248(2) y
C1 C1 23 1.466(2) y
C1 C1 21 1.466(2) n
C2 O2 . 1.250(2) y
C2 C2 44_666 1.465(3) y
C2 C2 41_665 1.465(3) n
O3 H1 . 0.8600 n
O3 H2 . 0.8601 n
O4 O5 44_666 1.272(16) n
O4 O5 43_565 1.272(16) n
O4 O5 36_566 1.272(16) n
O4 O5 35_665 1.272(16) n
O5 O4 30_665 1.272(16) n
O5 O5 13 1.39(3) n
O5 O5 15_565 1.57(2) n
O5 O5 16_655 1.57(2) n
loop_
_geom_hbond_atom_site_label_D
_geom_hbond_atom_site_label_H
_geom_hbond_atom_site_label_A
_geom_hbond_site_symmetry_A
_geom_hbond_distance_DH
_geom_hbond_distance_HA
_geom_hbond_distance_DA
_geom_hbond_angle_DHA
O3 H1 O1 23 0.86 1.92 2.7602(19) 165
O3 H2 O2 44_666 0.86 1.93 2.7742(19) 166
