#------------------------------------------------------------------------------
#$Date: 2016-02-21 02:03:34 +0200 (Sun, 21 Feb 2016) $
#$Revision: 176798 $
#$URL: svn://www.crystallography.net/cod/cif/2/23/11/2231160.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_2231160
loop_
_publ_author_name
'Gao, Shan'
'Ng, Seik Weng'
_publ_section_title
;
 trans-Bis(acetato-κO)diaquabis(2-aminopyrazine-κN⁴)manganese(II)
 dihydrate
;
_journal_coeditor_code           IM2304
_journal_issue                   8
_journal_name_full               'Acta Crystallographica Section E'
_journal_page_first              m1140
_journal_paper_doi               10.1107/S1600536811028583
_journal_volume                  67
_journal_year                    2011
_chemical_formula_iupac          '[Mn (C2 H3 O2)2 (C4 H5 N3)2 (H2 O)2], 2H2 O'
_chemical_formula_moiety         'C12 H20 Mn N6 O6, 2(H2 O)'
_chemical_formula_sum            'C12 H24 Mn N6 O8'
_chemical_formula_weight         435.31
_chemical_name_systematic
;
trans-Bis(acetato-\kO)diaquabis(2-aminopyrazine-
κN⁴)manganese(II) dihydrate
;
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                100.866(3)
_cell_angle_beta                 105.036(3)
_cell_angle_gamma                110.250(3)
_cell_formula_units_Z            1
_cell_length_a                   7.0761(7)
_cell_length_b                   8.5411(8)
_cell_length_c                   9.5162(10)
_cell_measurement_reflns_used    3626
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      27.45
_cell_measurement_theta_min      3.28
_cell_volume                     495.92(9)
_computing_cell_refinement       'RAPID-AUTO (Rigaku, 1998)'
_computing_data_collection       'RAPID-AUTO (Rigaku, 1998)'
_computing_data_reduction        'CrystalClear (Rigaku/MSC, 2002)'
_computing_molecular_graphics    'X-SEED (Barbour, 2001)'
_computing_publication_material  'publCIF (Westrip, 2010)'
_computing_structure_refinement  'SHELXL97 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 0.992
_diffrn_measured_fraction_theta_max 0.992
_diffrn_measurement_device_type  'Rigaku R-AXIS RAPID IP'
_diffrn_measurement_method       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  0.0330
_diffrn_reflns_av_sigmaI/netI    0.0456
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_h_min       -8
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_l_max       12
_diffrn_reflns_limit_l_min       -12
_diffrn_reflns_number            4911
_diffrn_reflns_theta_full        27.45
_diffrn_reflns_theta_max         27.45
_diffrn_reflns_theta_min         3.28
_diffrn_standards_decay_%        0
_diffrn_standards_interval_count 0
_diffrn_standards_interval_time  0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.716
_exptl_absorpt_correction_T_max  0.9651
_exptl_absorpt_correction_T_min  0.9318
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   '(ABSCOR; Higashi, 1995)'
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.458
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             227
_exptl_crystal_size_max          0.10
_exptl_crystal_size_mid          0.08
_exptl_crystal_size_min          0.05
_refine_diff_density_max         0.801
_refine_diff_density_min         -1.009
_refine_ls_extinction_coef       0.021(8)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4^
_refine_ls_extinction_method     'SHELXL97 (Sheldrick, 2008)'
_refine_ls_goodness_of_fit_ref   1.069
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     148
_refine_ls_number_reflns         2249
_refine_ls_number_restraints     8
_refine_ls_restrained_S_all      1.067
_refine_ls_R_factor_all          0.0789
_refine_ls_R_factor_gt           0.0427
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.001
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[σ²(Fo²)+(0.0633P)²+0.7384P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1023
_refine_ls_wR_factor_ref         0.1589
_reflns_number_gt                1558
_reflns_number_total             2249
_reflns_threshold_expression     I>2σ(I)
_cod_data_source_file            im2304.cif
_cod_data_source_block           I
_cod_database_code               2231160
_cod_database_fobs_code          2231160
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, -y, -z'
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
_atom_site_symmetry_multiplicity
Mn Mn1 0.5000 0.5000 0.5000 0.0358(3) Uani d S 1 2
O O1 0.6700(4) 0.6113(3) 0.7465(3) 0.0413(6) Uani d . 1 1
O O2 0.9808(5) 0.5959(6) 0.7684(4) 0.0826(12) Uani d . 1 1
O O1W 0.7647(4) 0.4463(3) 0.4659(3) 0.0414(6) Uani d D 1 1
H H11 0.858(6) 0.503(5) 0.553(3) 0.082(18) Uiso d D 1 1
H H12 0.763(8) 0.346(3) 0.440(5) 0.09(2) Uiso d D 1 1
O O2W 0.4054(5) 0.6764(5) -0.0904(4) 0.0719(10) Uani d D 1 1
H H21 0.470(6) 0.649(7) -0.147(4) 0.085(18) Uiso d D 1 1
H H22 0.273(2) 0.636(6) -0.141(4) 0.084(18) Uiso d D 1 1
N N1 0.6498(5) 0.7758(4) 0.4722(3) 0.0406(7) Uani d . 1 1
N N2 0.7601(5) 1.1077(4) 0.4338(4) 0.0464(8) Uani d . 1 1
N N3 0.6301(9) 0.9802(5) 0.1732(4) 0.0738(13) Uani d D 1 1
H H31 0.562(9) 0.888(5) 0.091(4) 0.111 Uiso d D 1 1
H H32 0.654(10) 1.085(4) 0.163(7) 0.111 Uiso d D 1 1
C C1 0.7478(6) 0.9231(5) 0.5927(4) 0.0465(9) Uani d . 1 1
H H1 0.7803 0.9147 0.6914 0.056 Uiso calc R 1 1
C C2 0.7999(7) 1.0845(5) 0.5717(4) 0.0476(9) Uani d . 1 1
H H2 0.8665 1.1830 0.6576 0.057 Uiso calc R 1 1
C C3 0.6692(7) 0.9628(5) 0.3141(4) 0.0448(9) Uani d . 1 1
C C4 0.6154(6) 0.7964(5) 0.3351(4) 0.0408(8) Uani d . 1 1
H H4 0.5537 0.6977 0.2497 0.049 Uiso calc R 1 1
C C5 0.8583(6) 0.6370(5) 0.8229(4) 0.0428(8) Uani d . 1 1
C C6 0.9380(8) 0.7229(7) 0.9942(5) 0.0659(13) Uani d . 1 1
H H6A 1.0903 0.7569 1.0363 0.099 Uiso calc R 1 1
H H6B 0.8658 0.6414 1.0402 0.099 Uiso calc R 1 1
H H6C 0.9085 0.8248 1.0145 0.099 Uiso calc R 1 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'
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
O1W Mn1 O1W 2_666 . 180.0000(10)
O1W Mn1 O1 2_666 2_666 91.79(10)
O1W Mn1 O1 . 2_666 88.21(9)
O1W Mn1 O1 2_666 . 88.21(10)
O1W Mn1 O1 . . 91.79(10)
O1 Mn1 O1 2_666 . 180.0000(10)
O1W Mn1 N1 2_666 2_666 90.34(10)
O1W Mn1 N1 . 2_666 89.66(10)
O1 Mn1 N1 2_666 2_666 89.93(10)
O1 Mn1 N1 . 2_666 90.07(10)
O1W Mn1 N1 2_666 . 89.66(10)
O1W Mn1 N1 . . 90.34(10)
O1 Mn1 N1 2_666 . 90.07(10)
O1 Mn1 N1 . . 89.93(10)
N1 Mn1 N1 2_666 . 180.0000(10)
C5 O1 Mn1 . . 128.8(2)
Mn1 O1W H11 . . 99(3)
Mn1 O1W H12 . . 125(4)
H11 O1W H12 . . 109(2)
H21 O2W H22 . . 110(2)
C4 N1 C1 . . 116.8(3)
C4 N1 Mn1 . . 120.7(2)
C1 N1 Mn1 . . 121.9(2)
C3 N2 C2 . . 116.2(3)
C3 N3 H31 . . 121(4)
C3 N3 H32 . . 119(4)
H31 N3 H32 . . 119(6)
N1 C1 C2 . . 120.9(4)
N1 C1 H1 . . 119.6
C2 C1 H1 . . 119.6
N2 C2 C1 . . 123.2(3)
N2 C2 H2 . . 118.4
C1 C2 H2 . . 118.4
N2 C3 N3 . . 118.3(4)
N2 C3 C4 . . 120.7(3)
N3 C3 C4 . . 121.0(3)
N1 C4 C3 . . 122.1(3)
N1 C4 H4 . . 118.9
C3 C4 H4 . . 118.9
O2 C5 O1 . . 124.7(3)
O2 C5 C6 . . 118.0(4)
O1 C5 C6 . . 117.4(4)
C5 C6 H6A . . 109.5
C5 C6 H6B . . 109.5
H6A C6 H6B . . 109.5
C5 C6 H6C . . 109.5
H6A C6 H6C . . 109.5
H6B C6 H6C . . 109.5
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_site_symmetry_2
_geom_bond_distance
Mn1 O1W 2_666 2.163(3)
Mn1 O1W . 2.163(3)
Mn1 O1 2_666 2.181(2)
Mn1 O1 . 2.181(2)
Mn1 N1 2_666 2.323(3)
Mn1 N1 . 2.323(3)
O1 C5 . 1.260(4)
O2 C5 . 1.232(5)
O1W H11 . 0.840(10)
O1W H12 . 0.841(10)
O2W H21 . 0.838(10)
O2W H22 . 0.838(10)
N1 C4 . 1.321(5)
N1 C1 . 1.348(5)
N2 C3 . 1.335(5)
N2 C2 . 1.336(5)
N3 C3 . 1.344(5)
N3 H31 . 0.879(10)
N3 H32 . 0.878(10)
C1 C2 . 1.366(5)
C1 H1 . 0.9300
C2 H2 . 0.9300
C3 C4 . 1.406(5)
C4 H4 . 0.9300
C5 C6 . 1.516(5)
C6 H6A . 0.9600
C6 H6B . 0.9600
C6 H6C . 0.9600
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
O1w H11 O2 . 0.840(10) 1.89(2) 2.690(4) 160(5) yes
O1w H12 N2 1_545 0.840(10) 2.02(2) 2.837(4) 165(5) yes
O2w H21 O1 1_554 0.840(10) 2.020(10) 2.851(4) 171(4) yes
O2w H22 O2 1_454 0.840(10) 1.90(2) 2.726(5) 167(5) yes
N3 H31 O2w . 0.880(10) 1.980(10) 2.859(5) 178(6) yes
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_1
_geom_torsion
O1W Mn1 O1 C5 2_666 -175.9(3)
O1W Mn1 O1 C5 . 4.1(3)
N1 Mn1 O1 C5 2_666 93.7(3)
N1 Mn1 O1 C5 . -86.3(3)
O1W Mn1 N1 C4 2_666 -95.9(3)
O1W Mn1 N1 C4 . 84.1(3)
O1 Mn1 N1 C4 2_666 -4.2(3)
O1 Mn1 N1 C4 . 175.8(3)
O1W Mn1 N1 C1 2_666 74.3(3)
O1W Mn1 N1 C1 . -105.7(3)
O1 Mn1 N1 C1 2_666 166.1(3)
O1 Mn1 N1 C1 . -13.9(3)
C4 N1 C1 C2 . 2.6(6)
Mn1 N1 C1 C2 . -168.1(3)
C3 N2 C2 C1 . -1.6(6)
N1 C1 C2 N2 . -0.5(6)
C2 N2 C3 N3 . -178.7(4)
C2 N2 C3 C4 . 1.5(6)
C1 N1 C4 C3 . -2.7(5)
Mn1 N1 C4 C3 . 168.1(3)
N2 C3 C4 N1 . 0.7(6)
N3 C3 C4 N1 . -179.1(4)
Mn1 O1 C5 O2 . -2.8(6)
Mn1 O1 C5 C6 . 178.0(3)
