#------------------------------------------------------------------------------
#$Date: 2016-02-21 02:03:34 +0200 (Sun, 21 Feb 2016) $
#$Revision: 176798 $
#$URL: svn://www.crystallography.net/cod/cif/2/23/18/2231841.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_2231841
loop_
_publ_author_name
'Ha, Kwang'
_publ_section_title
;
 cis-Aquabis(2,2'-bipyrimidine-κ²N¹,N^1'^)iodidomanganese(II)
 iodide monohydrate
;
_journal_coeditor_code           BV2192
_journal_issue                   10
_journal_name_full               'Acta Crystallographica Section E'
_journal_page_first              m1453
_journal_paper_doi               10.1107/S160053681103875X
_journal_volume                  67
_journal_year                    2011
_chemical_formula_iupac          '[Mn I (C8 H6 N4)2 (H2 O)] I, H2 O'
_chemical_formula_moiety         'C16 H14 I Mn N8 O +, I-, H2 O'
_chemical_formula_sum            'C16 H16 I2 Mn N8 O2'
_chemical_formula_weight         661.11
_chemical_name_systematic
'cis-Aquabis(2,2'-bipyrimidine-κ²N¹,N^1'^)iodidomanganese(II) iodide monohydrate'
_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                113.302(2)
_cell_angle_beta                 101.695(2)
_cell_angle_gamma                104.053(3)
_cell_formula_units_Z            2
_cell_length_a                   7.8799(9)
_cell_length_b                   12.8197(15)
_cell_length_c                   12.9563(15)
_cell_measurement_reflns_used    2443
_cell_measurement_temperature    200(2)
_cell_measurement_theta_max      27.57
_cell_measurement_theta_min      2.77
_cell_volume                     1098.6(2)
_computing_cell_refinement       'SAINT (Bruker, 2000)'
_computing_data_collection       'SMART (Bruker, 2000)'
_computing_data_reduction        'SAINT (Bruker, 2000)'
_computing_molecular_graphics
'ORTEP-3 (Farrugia, 1997) and PLATON (Spek, 2009)'
_computing_publication_material  'SHELXTL (Sheldrick, 2008)'
_computing_structure_refinement  'SHELXL97 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      200(2)
_diffrn_measured_fraction_theta_full 0.973
_diffrn_measured_fraction_theta_max 0.973
_diffrn_measurement_device_type  'Bruker SMART 1000 CCD'
_diffrn_measurement_method       'φ and ω scans'
_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  0.0350
_diffrn_reflns_av_sigmaI/netI    0.0857
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_k_max       9
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            8099
_diffrn_reflns_theta_full        28.31
_diffrn_reflns_theta_max         28.31
_diffrn_reflns_theta_min         1.82
_diffrn_standards_decay_%        0
_diffrn_standards_interval_count 0
_diffrn_standards_interval_time  0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    3.440
_exptl_absorpt_correction_T_max  1.000000
_exptl_absorpt_correction_T_min  0.859375
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   '(SADABS; Bruker, 2000)'
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.999
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             630
_exptl_crystal_size_max          0.18
_exptl_crystal_size_mid          0.17
_exptl_crystal_size_min          0.07
_refine_diff_density_max         1.685
_refine_diff_density_min         -1.978
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.069
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     262
_refine_ls_number_reflns         5309
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.069
_refine_ls_R_factor_all          0.1176
_refine_ls_R_factor_gt           0.0515
_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)+(0.0257P)²+5.0797P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0874
_refine_ls_wR_factor_ref         0.1255
_reflns_number_gt                3106
_reflns_number_total             5309
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            bv2192.cif
_cod_data_source_block           I
_cod_database_code               2231841
_cod_database_fobs_code          2231841
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 0.00869(15) 0.35516(10) 0.67962(10) 0.0291(3) Uani d . 1 1
I I1 -0.28559(8) 0.41022(5) 0.57919(5) 0.04330(18) Uani d . 1 1
O O1 -0.0292(8) 0.4141(5) 0.8476(5) 0.0409(14) Uani d . 1 1
H H1A -0.0480 0.4795 0.8793 0.061 Uiso d R 1 1
H H1B 0.0151 0.3979 0.9017 0.061 Uiso d R 1 1
N N1 0.0377(8) 0.2491(5) 0.5019(5) 0.0241(13) Uani d . 1 1
N N2 -0.0908(9) 0.0587(6) 0.3252(6) 0.0351(16) Uani d . 1 1
N N3 -0.2538(9) -0.0424(6) 0.4477(6) 0.0341(16) Uani d . 1 1
N N4 -0.1572(8) 0.1567(5) 0.6127(5) 0.0280(14) Uani d . 1 1
N N5 0.2578(8) 0.5264(5) 0.7448(6) 0.0290(14) Uani d . 1 1
N N6 0.5769(9) 0.6325(6) 0.8644(6) 0.0318(15) Uani d . 1 1
N N7 0.5861(9) 0.4338(6) 0.8923(6) 0.0353(16) Uani d . 1 1
N N8 0.2658(8) 0.3303(6) 0.7736(5) 0.0297(15) Uani d . 1 1
C C1 0.1275(11) 0.2974(7) 0.4444(7) 0.037(2) Uani d . 1 1
H H1 0.2053 0.3808 0.4861 0.045 Uiso calc R 1 1
C C2 0.1111(12) 0.2304(8) 0.3274(8) 0.042(2) Uani d . 1 1
H H2 0.1755 0.2659 0.2880 0.050 Uiso calc R 1 1
C C3 -0.0021(13) 0.1100(9) 0.2699(8) 0.043(2) Uani d . 1 1
H H3 -0.0179 0.0619 0.1885 0.052 Uiso calc R 1 1
C C4 -0.0672(10) 0.1311(7) 0.4396(7) 0.0284(17) Uani d . 1 1
C C5 -0.1668(9) 0.0769(6) 0.5026(6) 0.0253(16) Uani d . 1 1
C C6 -0.3435(11) -0.0869(8) 0.5083(7) 0.037(2) Uani d . 1 1
H H6 -0.4092 -0.1721 0.4718 0.045 Uiso calc R 1 1
C C7 -0.3448(11) -0.0163(8) 0.6187(8) 0.038(2) Uani d . 1 1
H H7 -0.4096 -0.0500 0.6592 0.046 Uiso calc R 1 1
C C8 -0.2460(10) 0.1078(8) 0.6692(7) 0.0341(19) Uani d . 1 1
H H8 -0.2416 0.1596 0.7469 0.041 Uiso calc R 1 1
C C9 0.2540(11) 0.6266(8) 0.7371(7) 0.038(2) Uani d . 1 1
H H9 0.1418 0.6243 0.6906 0.046 Uiso calc R 1 1
C C10 0.4058(11) 0.7330(7) 0.7937(8) 0.040(2) Uani d . 1 1
H H10 0.3993 0.8046 0.7900 0.048 Uiso calc R 1 1
C C11 0.5674(11) 0.7309(7) 0.8557(7) 0.038(2) Uani d . 1 1
H H11 0.6759 0.8022 0.8937 0.046 Uiso calc R 1 1
C C12 0.4217(10) 0.5351(7) 0.8106(6) 0.0277(17) Uani d . 1 1
C C13 0.4269(10) 0.4261(7) 0.8252(6) 0.0290(17) Uani d . 1 1
C C14 0.5846(11) 0.3351(8) 0.9053(7) 0.037(2) Uani d . 1 1
H H14 0.6966 0.3361 0.9507 0.045 Uiso calc R 1 1
C C15 0.4283(11) 0.2325(8) 0.8558(7) 0.0361(19) Uani d . 1 1
H H15 0.4284 0.1639 0.8675 0.043 Uiso calc R 1 1
C C16 0.2732(12) 0.2347(7) 0.7892(6) 0.0332(19) Uani d . 1 1
H H16 0.1638 0.1640 0.7517 0.040 Uiso calc R 1 1
I I2 -0.22530(8) 0.08320(5) 0.95698(5) 0.04477(18) Uani d . 1 1
O O2 0.0658(7) 0.3656(5) 1.0267(5) 0.0432(15) Uani d . 1 1
H H2A 0.0086 0.2956 1.0159 0.065 Uiso d R 1 1
H H2B 0.1780 0.3826 1.0627 0.065 Uiso d 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'
I I -0.4742 1.8119 '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'
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'
loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_publ_flag
O1 Mn1 N1 166.1(2) ?
O1 Mn1 N4 94.6(2) ?
N1 Mn1 N4 72.8(2) y
O1 Mn1 N5 93.0(2) ?
N1 Mn1 N5 97.0(2) ?
N4 Mn1 N5 159.3(2) ?
O1 Mn1 N8 84.1(2) ?
N1 Mn1 N8 89.6(2) ?
N4 Mn1 N8 89.4(2) ?
N5 Mn1 N8 72.2(2) y
O1 Mn1 I1 93.91(15) ?
N1 Mn1 I1 93.41(15) ?
N4 Mn1 I1 96.02(16) ?
N5 Mn1 I1 102.63(16) ?
N8 Mn1 I1 174.35(16) ?
Mn1 O1 H1A 120.6 ?
Mn1 O1 H1B 125.9 ?
H1A O1 H1B 108.5 ?
C4 N1 C1 116.3(6) ?
C4 N1 Mn1 117.2(5) ?
C1 N1 Mn1 125.6(5) ?
C3 N2 C4 116.9(7) ?
C5 N3 C6 115.3(7) ?
C8 N4 C5 115.6(6) ?
C8 N4 Mn1 127.6(5) ?
C5 N4 Mn1 116.8(5) ?
C9 N5 C12 115.7(7) ?
C9 N5 Mn1 126.1(5) ?
C12 N5 Mn1 117.6(5) ?
C11 N6 C12 116.9(7) ?
C13 N7 C14 116.0(7) ?
C16 N8 C13 115.4(7) ?
C16 N8 Mn1 127.8(5) ?
C13 N8 Mn1 116.7(5) ?
N1 C1 C2 122.4(7) ?
N1 C1 H1 118.8 ?
C2 C1 H1 118.8 ?
C3 C2 C1 117.3(8) ?
C3 C2 H2 121.4 ?
C1 C2 H2 121.4 ?
N2 C3 C2 121.8(8) ?
N2 C3 H3 119.1 ?
C2 C3 H3 119.1 ?
N1 C4 N2 125.4(7) ?
N1 C4 C5 116.6(6) ?
N2 C4 C5 118.0(7) ?
N3 C5 N4 126.6(7) ?
N3 C5 C4 117.6(7) ?
N4 C5 C4 115.8(6) ?
N3 C6 C7 123.6(8) ?
N3 C6 H6 118.2 ?
C7 C6 H6 118.2 ?
C6 C7 C8 116.4(8) ?
C6 C7 H7 121.8 ?
C8 C7 H7 121.8 ?
N4 C8 C7 122.5(7) ?
N4 C8 H8 118.7 ?
C7 C8 H8 118.7 ?
N5 C9 C10 122.7(8) ?
N5 C9 H9 118.7 ?
C10 C9 H9 118.7 ?
C11 C10 C9 116.8(7) ?
C11 C10 H10 121.6 ?
C9 C10 H10 121.6 ?
N6 C11 C10 122.2(7) ?
N6 C11 H11 118.9 ?
C10 C11 H11 118.9 ?
N6 C12 N5 125.6(7) ?
N6 C12 C13 117.7(7) ?
N5 C12 C13 116.7(7) ?
N7 C13 N8 125.8(7) ?
N7 C13 C12 117.6(7) ?
N8 C13 C12 116.4(7) ?
N7 C14 C15 122.8(8) ?
N7 C14 H14 118.6 ?
C15 C14 H14 118.6 ?
C16 C15 C14 116.2(8) ?
C16 C15 H15 121.9 ?
C14 C15 H15 121.9 ?
N8 C16 C15 123.8(8) ?
N8 C16 H16 118.1 ?
C15 C16 H16 118.1 ?
H2A O2 H2B 106.3 ?
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_publ_flag
Mn1 O1 2.115(5) y
Mn1 N1 2.256(6) y
Mn1 N4 2.262(6) y
Mn1 N5 2.270(6) y
Mn1 N8 2.304(6) y
Mn1 I1 2.8048(13) y
O1 H1A 0.8400 ?
O1 H1B 0.8400 ?
N1 C4 1.334(9) ?
N1 C1 1.343(9) ?
N2 C3 1.338(10) ?
N2 C4 1.345(9) ?
N3 C5 1.322(9) ?
N3 C6 1.350(10) ?
N4 C8 1.332(9) ?
N4 C5 1.361(9) ?
N5 C9 1.333(10) ?
N5 C12 1.348(9) ?
N6 C11 1.328(10) ?
N6 C12 1.328(9) ?
N7 C13 1.330(9) ?
N7 C14 1.338(10) ?
N8 C16 1.331(10) ?
N8 C13 1.347(9) ?
C1 C2 1.374(11) ?
C1 H1 0.9500 ?
C2 C3 1.372(12) ?
C2 H2 0.9500 ?
C3 H3 0.9500 ?
C4 C5 1.486(10) ?
C6 C7 1.361(11) ?
C6 H6 0.9500 ?
C7 C8 1.391(11) ?
C7 H7 0.9500 ?
C8 H8 0.9500 ?
C9 C10 1.375(11) ?
C9 H9 0.9500 ?
C10 C11 1.374(11) ?
C10 H10 0.9500 ?
C11 H11 0.9500 ?
C12 C13 1.492(11) ?
C14 C15 1.373(11) ?
C14 H14 0.9500 ?
C15 C16 1.359(11) ?
C15 H15 0.9500 ?
C16 H16 0.9500 ?
O2 H2A 0.8400 ?
O2 H2B 0.8400 ?
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
O1 H1A O2 2_567 0.84 1.93 2.767(8) 171.7
O1 H1B O2 . 0.84 1.82 2.645(8) 167.4
O2 H2A I2 . 0.84 2.60 3.423(6) 168.4
O2 H2B N6 2_667 0.84 2.06 2.871(8) 162.2
O2 H2B N7 2_667 0.84 2.38 2.918(9) 122.0
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
O1 Mn1 N1 C4 33.9(12)
N4 Mn1 N1 C4 7.6(5)
N5 Mn1 N1 C4 169.2(5)
N8 Mn1 N1 C4 97.2(5)
I1 Mn1 N1 C4 -87.6(5)
O1 Mn1 N1 C1 -157.6(8)
N4 Mn1 N1 C1 176.1(6)
N5 Mn1 N1 C1 -22.3(6)
N8 Mn1 N1 C1 -94.3(6)
I1 Mn1 N1 C1 80.9(6)
O1 Mn1 N4 C8 1.8(6)
N1 Mn1 N4 C8 175.7(7)
N5 Mn1 N4 C8 113.1(8)
N8 Mn1 N4 C8 85.9(6)
I1 Mn1 N4 C8 -92.6(6)
O1 Mn1 N4 C5 -177.4(5)
N1 Mn1 N4 C5 -3.6(5)
N5 Mn1 N4 C5 -66.2(9)
N8 Mn1 N4 C5 -93.4(5)
I1 Mn1 N4 C5 88.2(5)
O1 Mn1 N5 C9 -93.1(7)
N1 Mn1 N5 C9 96.7(7)
N4 Mn1 N5 C9 155.4(7)
N8 Mn1 N5 C9 -176.0(7)
I1 Mn1 N5 C9 1.6(7)
O1 Mn1 N5 C12 78.0(5)
N1 Mn1 N5 C12 -92.2(5)
N4 Mn1 N5 C12 -33.5(10)
N8 Mn1 N5 C12 -4.9(5)
I1 Mn1 N5 C12 172.7(5)
O1 Mn1 N8 C16 84.7(6)
N1 Mn1 N8 C16 -82.8(6)
N4 Mn1 N8 C16 -10.0(6)
N5 Mn1 N8 C16 179.8(7)
O1 Mn1 N8 C13 -91.1(5)
N1 Mn1 N8 C13 101.4(5)
N4 Mn1 N8 C13 174.2(5)
N5 Mn1 N8 C13 4.0(5)
C4 N1 C1 C2 1.0(11)
Mn1 N1 C1 C2 -167.6(6)
N1 C1 C2 C3 -0.1(13)
C4 N2 C3 C2 1.4(12)
C1 C2 C3 N2 -1.2(13)
C1 N1 C4 N2 -0.8(11)
Mn1 N1 C4 N2 168.7(6)
C1 N1 C4 C5 179.9(6)
Mn1 N1 C4 C5 -10.5(8)
C3 N2 C4 N1 -0.3(12)
C3 N2 C4 C5 178.9(7)
C6 N3 C5 N4 1.1(11)
C6 N3 C5 C4 -179.5(6)
C8 N4 C5 N3 -0.3(11)
Mn1 N4 C5 N3 179.1(6)
C8 N4 C5 C4 -179.7(6)
Mn1 N4 C5 C4 -0.4(8)
N1 C4 C5 N3 -172.3(6)
N2 C4 C5 N3 8.4(10)
N1 C4 C5 N4 7.2(9)
N2 C4 C5 N4 -172.1(7)
C5 N3 C6 C7 -0.8(11)
N3 C6 C7 C8 -0.3(12)
C5 N4 C8 C7 -1.0(11)
Mn1 N4 C8 C7 179.8(6)
C6 C7 C8 N4 1.3(12)
C12 N5 C9 C10 -0.9(12)
Mn1 N5 C9 C10 170.3(6)
N5 C9 C10 C11 2.7(13)
C12 N6 C11 C10 -0.4(12)
C9 C10 C11 N6 -2.0(13)
C11 N6 C12 N5 2.5(11)
C11 N6 C12 C13 -176.6(7)
C9 N5 C12 N6 -1.8(11)
Mn1 N5 C12 N6 -173.8(6)
C9 N5 C12 C13 177.2(7)
Mn1 N5 C12 C13 5.2(8)
C14 N7 C13 N8 2.3(11)
C14 N7 C13 C12 178.7(7)
C16 N8 C13 N7 -2.6(11)
Mn1 N8 C13 N7 173.7(6)
C16 N8 C13 C12 -179.1(6)
Mn1 N8 C13 C12 -2.8(8)
N6 C12 C13 N7 0.8(10)
N5 C12 C13 N7 -178.4(6)
N6 C12 C13 N8 177.5(6)
N5 C12 C13 N8 -1.6(10)
C13 N7 C14 C15 -1.8(12)
N7 C14 C15 C16 1.6(12)
C13 N8 C16 C15 2.4(11)
Mn1 N8 C16 C15 -173.4(6)
C14 C15 C16 N8 -2.0(12)
