#------------------------------------------------------------------------------
#$Date: 2016-02-21 02:03:34 +0200 (Sun, 21 Feb 2016) $
#$Revision: 176798 $
#$URL: svn://www.crystallography.net/cod/cif/2/23/30/2233094.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_2233094
loop_
_publ_author_name
'Ha, Kwang'
_publ_section_title
;
 cis-Bis(2,2'-bipyrimidine-κ²N¹,N^1'^)diiodidomanganese(II)
;
_journal_coeditor_code           BT5729
_journal_issue                   1
_journal_name_full               'Acta Crystallographica Section E'
_journal_page_first              m1
_journal_paper_doi               10.1107/S160053681105080X
_journal_volume                  68
_journal_year                    2012
_chemical_formula_iupac          '[Mn I2 (C8 H6 N4)2]'
_chemical_formula_moiety         'C16 H12 I2 Mn N8'
_chemical_formula_sum            'C16 H12 I2 Mn N8'
_chemical_formula_weight         625.08
_chemical_name_systematic
;
cis-Bis(2,2'-bipyrimidine-
κ²N¹,N^1'^)diiodidomanganese(II)
;
_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                 97.8220(10)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   8.2841(4)
_cell_length_b                   13.8442(7)
_cell_length_c                   17.8243(9)
_cell_measurement_reflns_used    3917
_cell_measurement_temperature    200(2)
_cell_measurement_theta_max      28.12
_cell_measurement_theta_min      2.89
_cell_volume                     2025.19(17)
_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  'SHELXL97 (Sheldrick, 2008)'
_computing_structure_refinement  'SHELXL97 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      200(2)
_diffrn_measured_fraction_theta_full 0.984
_diffrn_measured_fraction_theta_max 0.984
_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  0.0231
_diffrn_reflns_av_sigmaI/netI    0.0303
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       13
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_number            7130
_diffrn_reflns_theta_full        28.31
_diffrn_reflns_theta_max         28.31
_diffrn_reflns_theta_min         2.31
_diffrn_standards_decay_%        0
_diffrn_standards_interval_count 0
_diffrn_standards_interval_time  0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    3.719
_exptl_absorpt_correction_T_max  1.000000
_exptl_absorpt_correction_T_min  0.862580
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   '(SADABS; Bruker, 2000)'
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    2.050
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             1180
_exptl_crystal_size_max          0.34
_exptl_crystal_size_mid          0.22
_exptl_crystal_size_min          0.17
_refine_diff_density_max         0.944
_refine_diff_density_min         -0.501
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.095
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     123
_refine_ls_number_reflns         2477
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.095
_refine_ls_R_factor_all          0.0447
_refine_ls_R_factor_gt           0.0265
_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)+(0.0197P)²+5.0272P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0512
_refine_ls_wR_factor_ref         0.0644
_reflns_number_gt                1923
_reflns_number_total             2477
_reflns_threshold_expression     I>2σ(I)
_cod_data_source_file            bt5729.cif
_cod_data_source_block           I
_cod_original_sg_symbol_H-M      'C 2/c'
_cod_database_code               2233094
_cod_database_fobs_code          2233094
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, y, -z+1/2'
'x+1/2, y+1/2, z'
'-x+1/2, y+1/2, -z+1/2'
'-x, -y, -z'
'x, -y, z-1/2'
'-x+1/2, -y+1/2, -z'
'x+1/2, -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
_atom_site_symmetry_multiplicity
Mn Mn1 0.5000 0.28328(5) 0.2500 0.03038(18) Uani d S 1 2
I I1 0.68736(3) 0.409360(18) 0.170347(15) 0.03768(9) Uani d . 1 1
N N1 0.2923(4) 0.2495(2) 0.15380(16) 0.0316(7) Uani d . 1 1
N N2 0.2149(4) 0.1486(2) 0.04676(18) 0.0372(7) Uani d . 1 1
N N3 0.4761(4) 0.0785(2) 0.4388(2) 0.0444(9) Uani d . 1 1
N N4 0.4157(4) 0.1610(2) 0.32184(18) 0.0349(7) Uani d . 1 1
C C1 0.1449(5) 0.2901(3) 0.1444(2) 0.0359(8) Uani d . 1 1
H H1 0.1204 0.3392 0.1783 0.043 Uiso calc R 1 1
C C2 0.0271(5) 0.2616(3) 0.0861(2) 0.0421(10) Uani d . 1 1
H H2 -0.0780 0.2903 0.0789 0.051 Uiso calc R 1 1
C C3 0.0689(5) 0.1895(3) 0.0387(2) 0.0408(9) Uani d . 1 1
H H3 -0.0105 0.1682 -0.0013 0.049 Uiso calc R 1 1
C C4 0.3207(4) 0.1809(2) 0.10433(19) 0.0302(8) Uani d . 1 1
C C5 0.5128(4) 0.1365(3) 0.3852(2) 0.0322(8) Uani d . 1 1
C C6 0.3261(5) 0.0392(3) 0.4279(3) 0.0478(11) Uani d . 1 1
H H6 0.2938 -0.0021 0.4657 0.057 Uiso calc R 1 1
C C7 0.2193(5) 0.0569(3) 0.3644(2) 0.0448(10) Uani d . 1 1
H H7 0.1152 0.0271 0.3563 0.054 Uiso calc R 1 1
C C8 0.2688(5) 0.1201(3) 0.3123(2) 0.0411(9) Uani d . 1 1
H H8 0.1956 0.1349 0.2680 0.049 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'
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'
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
N4 Mn1 N4 2_655 . 84.55(16) ?
N4 Mn1 N1 2_655 . 71.78(10) y
N4 Mn1 N1 . . 90.72(11) ?
N4 Mn1 N1 2_655 2_655 90.72(11) ?
N4 Mn1 N1 . 2_655 71.78(10) ?
N1 Mn1 N1 . 2_655 156.60(15) ?
N4 Mn1 I1 2_655 . 86.90(8) ?
N4 Mn1 I1 . . 164.40(8) ?
N1 Mn1 I1 . . 98.98(7) ?
N1 Mn1 I1 2_655 . 95.35(7) ?
N4 Mn1 I1 2_655 2_655 164.40(8) ?
N4 Mn1 I1 . 2_655 86.90(8) ?
N1 Mn1 I1 . 2_655 95.35(7) ?
N1 Mn1 I1 2_655 2_655 98.98(7) ?
I1 Mn1 I1 . 2_655 104.19(3) y
C1 N1 C4 . . 117.1(3) ?
C1 N1 Mn1 . . 125.8(2) ?
C4 N1 Mn1 . . 117.0(2) ?
C3 N2 C4 . . 115.8(3) ?
C5 N3 C6 . . 116.2(3) ?
C8 N4 C5 . . 115.7(3) ?
C8 N4 Mn1 . . 125.9(3) ?
C5 N4 Mn1 . . 117.7(2) ?
N1 C1 C2 . . 120.9(3) ?
N1 C1 H1 . . 119.5 ?
C2 C1 H1 . . 119.5 ?
C3 C2 C1 . . 117.1(4) ?
C3 C2 H2 . . 121.4 ?
C1 C2 H2 . . 121.4 ?
N2 C3 C2 . . 122.9(4) ?
N2 C3 H3 . . 118.5 ?
C2 C3 H3 . . 118.5 ?
N2 C4 N1 . . 126.1(3) ?
N2 C4 C5 . 2_655 117.2(3) ?
N1 C4 C5 . 2_655 116.7(3) ?
N3 C5 N4 . . 126.6(3) ?
N3 C5 C4 . 2_655 117.4(3) ?
N4 C5 C4 . 2_655 116.0(3) ?
N3 C6 C7 . . 122.0(4) ?
N3 C6 H6 . . 119.0 ?
C7 C6 H6 . . 119.0 ?
C6 C7 C8 . . 117.2(4) ?
C6 C7 H7 . . 121.4 ?
C8 C7 H7 . . 121.4 ?
N4 C8 C7 . . 122.2(4) ?
N4 C8 H8 . . 118.9 ?
C7 C8 H8 . . 118.9 ?
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 N4 2_655 2.289(3) ?
Mn1 N4 . 2.289(3) y
Mn1 N1 . 2.305(3) y
Mn1 N1 2_655 2.305(3) ?
Mn1 I1 . 2.8410(5) y
Mn1 I1 2_655 2.8410(5) ?
N1 C1 . 1.334(5) ?
N1 C4 . 1.339(4) ?
N2 C3 . 1.325(5) ?
N2 C4 . 1.332(5) ?
N3 C5 . 1.315(5) ?
N3 C6 . 1.347(5) ?
N4 C8 . 1.332(5) ?
N4 C5 . 1.338(5) ?
C1 C2 . 1.383(5) ?
C1 H1 . 0.9500 ?
C2 C3 . 1.381(6) ?
C2 H2 . 0.9500 ?
C3 H3 . 0.9500 ?
C4 C5 2_655 1.498(5) ?
C5 C4 2_655 1.498(5) ?
C6 C7 . 1.361(6) ?
C6 H6 . 0.9500 ?
C7 C8 . 1.378(6) ?
C7 H7 . 0.9500 ?
C8 H8 . 0.9500 ?
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
C6 H6 N3 5_656 0.95 2.60 3.151(5) 117.2
C6 H6 N2 6_556 0.95 2.62 3.554(5) 166.3
C7 H7 I1 4_545 0.95 2.97 3.917(4) 172.5
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_site_symmetry_4
_geom_torsion
N4 Mn1 N1 C1 2_655 . 176.2(3)
N4 Mn1 N1 C1 . . 92.1(3)
N1 Mn1 N1 C1 2_655 . 132.8(3)
I1 Mn1 N1 C1 . . -100.1(3)
I1 Mn1 N1 C1 2_655 . 5.2(3)
N4 Mn1 N1 C4 2_655 . -1.6(2)
N4 Mn1 N1 C4 . . -85.6(3)
N1 Mn1 N1 C4 2_655 . -44.9(2)
I1 Mn1 N1 C4 . . 82.1(2)
I1 Mn1 N1 C4 2_655 . -172.6(2)
N4 Mn1 N4 C8 2_655 . -90.9(3)
N1 Mn1 N4 C8 . . -19.2(3)
N1 Mn1 N4 C8 2_655 . 176.6(3)
I1 Mn1 N4 C8 . . -148.0(3)
I1 Mn1 N4 C8 2_655 . 76.1(3)
N4 Mn1 N4 C5 2_655 . 98.8(3)
N1 Mn1 N4 C5 . . 170.5(3)
N1 Mn1 N4 C5 2_655 . 6.3(3)
I1 Mn1 N4 C5 . . 41.8(5)
I1 Mn1 N4 C5 2_655 . -94.2(3)
C4 N1 C1 C2 . . 0.2(5)
Mn1 N1 C1 C2 . . -177.5(3)
N1 C1 C2 C3 . . 0.3(6)
C4 N2 C3 C2 . . 0.5(6)
C1 C2 C3 N2 . . -0.7(6)
C3 N2 C4 N1 . . 0.1(6)
C3 N2 C4 C5 . 2_655 -179.7(3)
C1 N1 C4 N2 . . -0.5(5)
Mn1 N1 C4 N2 . . 177.4(3)
C1 N1 C4 C5 . 2_655 179.4(3)
Mn1 N1 C4 C5 . 2_655 -2.7(4)
C6 N3 C5 N4 . . 0.8(6)
C6 N3 C5 C4 . 2_655 -179.7(4)
C8 N4 C5 N3 . . -1.6(6)
Mn1 N4 C5 N3 . . 169.7(3)
C8 N4 C5 C4 . 2_655 178.9(3)
Mn1 N4 C5 C4 . 2_655 -9.8(4)
C5 N3 C6 C7 . . 1.2(7)
N3 C6 C7 C8 . . -2.3(7)
C5 N4 C8 C7 . . 0.3(6)
Mn1 N4 C8 C7 . . -170.1(3)
C6 C7 C8 N4 . . 1.5(7)
