#------------------------------------------------------------------------------
#$Date: 2016-02-20 18:35:30 +0200 (Sat, 20 Feb 2016) $
#$Revision: 176787 $
#$URL: svn://www.crystallography.net/cod/cif/2/21/90/2219057.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_2219057
loop_
_publ_author_name
'Kurawa, Mukhtar A.'
'Adams, Christopher J.'
'Orpen, A. Guy'
_publ_section_title
;
 2,2'-Biimidazolium hexaaquamanganese(II) bis(sulfate)
;
_journal_coeditor_code           HY2142
_journal_issue                   8
_journal_name_full               'Acta Crystallographica Section E'
_journal_page_first              m1005
_journal_paper_doi               10.1107/S1600536808020291
_journal_volume                  64
_journal_year                    2008
_chemical_formula_iupac          '(C6 H8 N4) [Mn (H2 O)6] (S O4)2'
_chemical_formula_moiety         'C6 H8 N4 2+ , H12 Mn1 O6 2+ , 2S O4 2-'
_chemical_formula_sum            'C6 H20 Mn N4 O14 S2'
_chemical_formula_weight         491.34
_chemical_name_systematic
;
2,2'-Biimidazolium hexaaquamanganese(II) bis(sulfate)
;
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL97
_cell_angle_alpha                90.00
_cell_angle_beta                 91.650(10)
_cell_angle_gamma                90.00
_cell_formula_units_Z            2
_cell_length_a                   6.0625(7)
_cell_length_b                   11.606(2)
_cell_length_c                   12.218(2)
_cell_measurement_reflns_used    7442
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      27.46
_cell_measurement_theta_min      2.42
_cell_volume                     859.3(2)
_computing_cell_refinement       'SAINT (Bruker, 2007)'
_computing_data_collection       'SMART (Bruker, 2007)'
_computing_data_reduction        'SAINT (Bruker, 2007)'
_computing_molecular_graphics    'SHELXTL (Sheldrick, 2008)'
_computing_publication_material  'SHELXTL (Sheldrick, 2008)'
_computing_structure_refinement  'SHELXL97 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device_type  'Bruker SMART APEX CCD area-detector'
_diffrn_measurement_method       'φ and ω'
_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  0.0180
_diffrn_reflns_av_sigmaI/netI    0.0138
_diffrn_reflns_limit_h_max       7
_diffrn_reflns_limit_h_min       -7
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_number            9389
_diffrn_reflns_theta_full        27.46
_diffrn_reflns_theta_max         27.46
_diffrn_reflns_theta_min         2.42
_exptl_absorpt_coefficient_mu    1.094
_exptl_absorpt_correction_T_max  0.800
_exptl_absorpt_correction_T_min  0.6860
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   '(SADABS; Sheldrick,1996)'
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.899
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             506
_exptl_crystal_size_max          0.4
_exptl_crystal_size_mid          0.3
_exptl_crystal_size_min          0.2
_refine_diff_density_max         0.285
_refine_diff_density_min         -0.653
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.057
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     142
_refine_ls_number_reflns         1954
_refine_ls_number_restraints     6
_refine_ls_restrained_S_all      1.056
_refine_ls_R_factor_all          0.0233
_refine_ls_R_factor_gt           0.0227
_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/[σ²(Fo²)+(0.042P)²+0.4497P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0648
_refine_ls_wR_factor_ref         0.0658
_reflns_number_gt                1897
_reflns_number_total             1954
_reflns_threshold_expression     I>2σ(I)
_cod_data_source_file            hy2142.cif
_cod_data_source_block           I
_cod_original_sg_symbol_H-M      'P 21/c'
_cod_database_code               2219057
_cod_database_fobs_code          2219057
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, y+1/2, -z+1/2'
'-x, -y, -z'
'x, -y-1/2, z-1/2'
loop_
_atom_site_type_symbol
_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
Mn Mn1 0.5000 0.5000 0.0000 0.00892(9) Uani d S 1
S S1 0.87954(5) 0.76694(3) 0.24181(2) 0.00829(10) Uani d . 1
N N1 0.20621(19) 1.00486(9) 0.11407(9) 0.0107(2) Uani d . 1
H H1A 0.1629 1.0584 0.1597 0.013 Uiso calc R 1
N N2 0.21706(17) 0.89187(9) -0.02676(9) 0.0105(2) Uani d . 1
H H2A 0.1825 0.8585 -0.0896 0.013 Uiso calc R 1
C C1 0.3926(2) 0.93818(11) 0.12742(11) 0.0125(2) Uani d . 1
H H1B 0.4969 0.9413 0.1869 0.015 Uiso calc R 1
C C2 0.3988(2) 0.86702(11) 0.03924(11) 0.0124(2) Uani d . 1
H H2B 0.5082 0.8106 0.0257 0.015 Uiso calc R 1
C C3 0.1021(2) 0.97533(11) 0.02099(10) 0.0098(2) Uani d . 1
O O1 0.87996(15) 0.78300(8) 0.12285(7) 0.0128(2) Uani d . 1
O O2 0.65505(15) 0.73605(8) 0.27723(8) 0.0126(2) Uani d . 1
O O3 1.02939(15) 0.66897(8) 0.27336(7) 0.01179(19) Uani d . 1
O O4 0.95582(15) 0.87250(8) 0.29863(8) 0.01210(19) Uani d . 1
O O5 0.39485(16) 0.59047(8) 0.15004(8) 0.0137(2) Uani d D 1
O O6 0.19308(16) 0.40995(8) -0.00527(8) 0.0135(2) Uani d D 1
O O7 0.63321(15) 0.36233(8) 0.10452(8) 0.01286(19) Uani d D 1
H H5A 0.474(3) 0.6368(14) 0.1868(14) 0.015 Uiso d D 1
H H6A 0.134(3) 0.4002(15) 0.0553(13) 0.015 Uiso d D 1
H H7A 0.753(3) 0.3688(15) 0.1418(14) 0.015 Uiso d D 1
H H5B 0.273(2) 0.6050(15) 0.1724(14) 0.015 Uiso d D 1
H H6B 0.162(3) 0.3514(14) -0.0441(14) 0.015 Uiso d D 1
H H7B 0.548(3) 0.3290(15) 0.1482(13) 0.015 Uiso d D 1
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'
N N 0.0061 0.0033 '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'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
S S 0.1246 0.1234 '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
O6 Mn1 O6 . 3_665 180.0
O6 Mn1 O7 . 3_665 91.90(4)
O6 Mn1 O7 3_665 3_665 88.10(4)
O6 Mn1 O7 . . 88.10(4)
O6 Mn1 O7 3_665 . 91.90(4)
O7 Mn1 O7 3_665 . 180.0
O6 Mn1 O5 . . 89.18(4)
O6 Mn1 O5 3_665 . 90.82(4)
O7 Mn1 O5 3_665 . 91.53(4)
O7 Mn1 O5 . . 88.47(4)
O6 Mn1 O5 . 3_665 90.82(4)
O6 Mn1 O5 3_665 3_665 89.18(4)
O7 Mn1 O5 3_665 3_665 88.47(4)
O7 Mn1 O5 . 3_665 91.53(4)
O5 Mn1 O5 . 3_665 180.0
O1 S1 O4 . . 110.58(6)
O1 S1 O2 . 1 110.35(6)
O4 S1 O2 . 1 109.94(6)
O1 S1 O2 . . 110.35(6)
O4 S1 O2 . . 109.94(6)
O1 S1 O3 . . 109.47(6)
O4 S1 O3 . . 109.23(6)
O2 S1 O3 1 . 107.21(6)
O2 S1 O3 . . 107.21(6)
C3 N1 C1 . . 108.94(11)
C3 N1 H1A . . 125.5
C1 N1 H1A . . 125.5
C3 N2 C2 . . 108.33(11)
C3 N2 H2A . . 125.8
C2 N2 H2A . . 125.8
C2 C1 N1 . . 106.82(11)
C2 C1 H1B . . 126.6
N1 C1 H1B . . 126.6
C1 C2 N2 . . 107.28(11)
C1 C2 H2B . . 126.4
N2 C2 H2B . . 126.4
N1 C3 N2 . . 108.63(11)
N1 C3 C3 . 3_575 125.62(15)
N2 C3 C3 . 3_575 125.75(15)
Mn1 O5 H5A . . 124.6(12)
Mn1 O5 H5B . . 131.4(13)
H5A O5 H5B . . 101.5(17)
Mn1 O6 H6A . . 115.7(12)
Mn1 O6 H6B . . 126.2(12)
H6A O6 H6B . . 107.0(17)
Mn1 O7 H7A . . 123.0(12)
Mn1 O7 H7B . . 118.8(12)
H7A O7 H7B . . 103.3(17)
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
Mn1 O6 . 2.1335(10) yes
Mn1 O6 3_665 2.1335(10) ?
Mn1 O7 3_665 2.1856(10) ?
Mn1 O7 . 2.1856(10) yes
Mn1 O5 . 2.2218(10) yes
Mn1 O5 3_665 2.2218(10) ?
S1 O1 . 1.4653(10) ?
S1 O4 . 1.4759(10) ?
S1 O2 1 1.4839(10) ?
S1 O2 . 1.4839(10) ?
S1 O3 . 1.4989(9) ?
N1 C3 . 1.3296(17) ?
N1 C1 . 1.3754(17) ?
N1 H1A . 0.8800 ?
N2 C3 . 1.3371(16) ?
N2 C2 . 1.3771(17) ?
N2 H2A . 0.8800 ?
C1 C2 . 1.3589(19) ?
C1 H1B . 0.9500 ?
C2 H2B . 0.9500 ?
C3 C3 3_575 1.445(2) yes
O5 H5A . 0.843(14) ?
O5 H5B . 0.813(14) ?
O6 H6A . 0.839(14) ?
O6 H6B . 0.846(14) ?
O7 H7A . 0.851(14) ?
O7 H7B . 0.846(14) ?
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
_geom_hbond_publ_flag
N1 H1A O3 2_655 0.88 1.93 2.7699(15) 159 y
N1 H1A O2 2_655 0.88 2.45 3.0994(15) 131 y
N2 H2A O3 4_475 0.88 1.92 2.7562(16) 159 y
O5 H5A O2 1 0.843(14) 1.917(15) 2.7600(15) 176.8(18) y
O5 H5B O3 1_455 0.813(14) 2.088(15) 2.8638(15) 159.7(17) y
O6 H6A O4 2_645 0.839(14) 1.908(15) 2.7402(15) 171.2(18) y
O6 H6B O1 3_665 0.846(14) 1.847(15) 2.6904(14) 174.2(18) y
O7 H7A O4 2_745 0.851(14) 1.888(15) 2.7298(15) 169.5(18) y
O7 H7B O2 2_645 0.846(14) 1.892(14) 2.7266(14) 169.0(17) y
loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion_site_symmetry_4
_geom_torsion
C3 N1 C1 C2 . 0.07(15)
N1 C1 C2 N2 . 0.36(14)
C3 N2 C2 C1 . -0.66(14)
C1 N1 C3 N2 . -0.48(14)
C1 N1 C3 C3 3_575 179.08(15)
C2 N2 C3 N1 . 0.71(14)
C2 N2 C3 C3 3_575 -178.85(15)
