#------------------------------------------------------------------------------
#$Date: 2019-07-31 07:41:55 +0300 (Wed, 31 Jul 2019) $
#$Revision: 217324 $
#$URL: file:///home/coder/svn-repositories/cod/cif/2/24/30/2243039.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_2243039
loop_
_publ_author_name
'Lynch, Sheridan'
'Lynch, Genevieve'
'Lynch, Will E.'
'Padgett, Clifford W.'
_publ_section_title
;
 Crystal structures of four dimeric manganese(II) bromide coordination
 complexes with various derivatives of pyridine N-oxide
;
_journal_coeditor_code           SU5505
_journal_issue                   8
_journal_name_full               'Acta Crystallographica Section E'
_journal_page_first              1284
_journal_page_last               1290
_journal_paper_doi               10.1107/S2056989019010557
_journal_volume                  75
_journal_year                    2019
_chemical_formula_iupac          '[Mn2 Br4 (C6 H7 N O)4 (H2 O)2]'
_chemical_formula_moiety         'C24 H32 Br4 Mn2 N4 O6'
_chemical_formula_sum            'C24 H32 Br4 Mn2 N4 O6'
_chemical_formula_weight         902.05
_chemical_name_systematic
;
Bis(μ-3-methylpyridine N-oxide)bis[aquadibromido(3-methylpyridine
N-oxide)manganese(II)]
;
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     dual
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_cell_angle_alpha                111.980(7)
_cell_angle_beta                 100.360(6)
_cell_angle_gamma                97.737(6)
_cell_formula_units_Z            1
_cell_length_a                   7.6354(5)
_cell_length_b                   9.9700(8)
_cell_length_c                   11.8980(10)
_cell_measurement_reflns_used    4991
_cell_measurement_temperature    170
_cell_measurement_theta_max      33.1210
_cell_measurement_theta_min      2.2340
_cell_volume                     805.71(12)
_computing_cell_refinement
;
CrysAlisPro (Rigaku Oxford Diffraction, 2018)
;
_computing_data_collection
;
CrysAlisPro (Rigaku Oxford Diffraction, 2018)
;
_computing_data_reduction
;
CrysAlisPro (Rigaku Oxford Diffraction, 2018)
;
_computing_molecular_graphics
;
OLEX2 (Dolomanov et al.,  2009) and Mercury (Macrae et
al.,  2008)
;
_computing_publication_material
;
OLEX2 (Dolomanov et al.,  2009)
;
_computing_structure_refinement
;
ShelXL (Sheldrick, 2015b)
;
_computing_structure_solution
;
ShelXT (Sheldrick, 2015a)
;
_diffrn_ambient_temperature      170
_diffrn_detector                 'Rigaku XtaLAB area detector'
_diffrn_detector_area_resol_mean 13.6612
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device       'abstract diffractometer'
_diffrn_measurement_device_type  'Rigaku XtaLAB mini'
_diffrn_measurement_method       'profile data from ω-scans'
_diffrn_radiation_monochromator  'Graphite Monochromator'
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0361
_diffrn_reflns_av_unetI/netI     0.0467
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_number            8460
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.483
_diffrn_reflns_theta_min         1.907
_diffrn_source                   'fine-focus sealed X-ray tube'
_exptl_absorpt_coefficient_mu    5.785
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.31906
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
(CrysAlisPro; Rigaku Oxford Diffraction, 2018)
;
_exptl_crystal_colour            'clear light yellow'
_exptl_crystal_density_diffrn    1.859
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             442
_exptl_crystal_size_max          0.45
_exptl_crystal_size_mid          0.4
_exptl_crystal_size_min          0.2
_refine_diff_density_max         1.657
_refine_diff_density_min         -0.844
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.015
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     191
_refine_ls_number_reflns         3672
_refine_ls_number_restraints     2
_refine_ls_restrained_S_all      1.015
_refine_ls_R_factor_all          0.0580
_refine_ls_R_factor_gt           0.0399
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[σ²(Fo²)+(0.0461P)²+0.5922P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0900
_refine_ls_wR_factor_ref         0.0977
_reflns_number_gt                2875
_reflns_number_total             3672
_reflns_threshold_expression     'I > 2σ(I)'
_cod_data_source_file            su5505sup1.cif
_cod_data_source_block           III
_cod_database_code               2243039
_shelx_space_group_comment
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;
_shelx_estimated_absorpt_t_min   0.181
_shelx_estimated_absorpt_t_max   0.391
loop_
_space_group_symop_operation_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_occupancy
Br Br1 0.36280(5) 0.42105(5) 0.13651(4) 0.03458(13) Uani d 1
C C1 0.4906(7) 0.7816(7) 0.4116(5) 0.0544(14) Uani d 1
H H1 0.509132 0.827435 0.356286 0.065 Uiso calc 1
N N1 0.3196(5) 0.7177(4) 0.4046(3) 0.0383(9) Uani d 1
Mn Mn1 0.04801(8) 0.51611(7) 0.16098(5) 0.02659(16) Uani d 1
O O1 0.1816(4) 0.7175(4) 0.3187(3) 0.0418(8) Uani d 1
O O2 0.0827(3) 0.6326(3) 0.0380(3) 0.0295(6) Uani d 1
C C2 0.6381(7) 0.7822(7) 0.4963(5) 0.0606(16) Uani d 1
Br Br2 -0.07392(6) 0.33641(5) 0.25163(4) 0.03571(14) Uani d 1
N N2 0.1876(4) 0.7681(4) 0.0757(3) 0.0254(7) Uani d 1
C C3 0.6062(7) 0.7148(6) 0.5770(5) 0.0520(13) Uani d 1
H H3 0.705412 0.710037 0.635284 0.062 Uiso calc 1
O O3 -0.2115(4) 0.5986(4) 0.1560(3) 0.0360(7) Uani d 1
H H3A -0.304(4) 0.546(5) 0.159(4) 0.045(15) Uiso d 1
H H3B -0.237(7) 0.594(6) 0.082(3) 0.065(18) Uiso d 1
C C4 0.4293(7) 0.6553(6) 0.5712(5) 0.0489(12) Uani d 1
H H4 0.406617 0.612501 0.627790 0.059 Uiso calc 1
C C5 0.2857(6) 0.6573(5) 0.4846(4) 0.0391(10) Uani d 1
H H5 0.163976 0.616659 0.481113 0.047 Uiso calc 1
C C6 0.8283(9) 0.8554(11) 0.5025(7) 0.110(3) Uani d 1
H H6A 0.848206 0.962978 0.548807 0.165 Uiso calc 1
H H6B 0.841882 0.833305 0.417405 0.165 Uiso calc 1
H H6C 0.918146 0.817490 0.545184 0.165 Uiso calc 1
C C7 0.3693(5) 0.7876(4) 0.1021(4) 0.0287(9) Uani d 1
H H7 0.422698 0.704972 0.095217 0.034 Uiso calc 1
C C8 0.4801(5) 0.9247(5) 0.1391(4) 0.0317(9) Uani d 1
C C9 0.3993(6) 1.0418(5) 0.1454(4) 0.0369(10) Uani d 1
H H9 0.472406 1.136963 0.166642 0.044 Uiso calc 1
C C10 0.2119(6) 1.0206(5) 0.1206(5) 0.0425(11) Uani d 1
H H10 0.155519 1.101679 0.127690 0.051 Uiso calc 1
C C11 0.1069(6) 0.8811(5) 0.0856(4) 0.0376(10) Uani d 1
H H11 -0.022312 0.865462 0.068630 0.045 Uiso calc 1
C C12 0.6838(6) 0.9463(6) 0.1743(6) 0.0583(15) Uani d 1
H H12A 0.727982 0.988271 0.265702 0.087 Uiso calc 1
H H12B 0.739282 1.014307 0.142149 0.087 Uiso calc 1
H H12C 0.717356 0.850553 0.138142 0.087 Uiso calc 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'
Br Br -0.2901 2.4595 '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_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle
N1 C1 H1 . . 119.2
N1 C1 C2 . . 121.6(5)
C2 C1 H1 . . 119.2
O1 N1 C1 . . 119.2(4)
O1 N1 C5 . . 119.5(4)
C5 N1 C1 . . 121.3(4)
O1 Mn1 Br1 . . 93.86(9)
O1 Mn1 O2 . 2_565 157.76(11)
O1 Mn1 O2 . . 88.94(11)
O1 Mn1 Br2 . . 105.48(9)
O1 Mn1 O3 . . 88.95(12)
O2 Mn1 Br1 . . 91.19(7)
O2 Mn1 Br1 2_565 . 89.84(8)
O2 Mn1 O2 . 2_565 69.05(11)
O2 Mn1 Br2 2_565 . 95.91(7)
O2 Mn1 Br2 . . 163.39(7)
O2 Mn1 O3 . . 81.25(11)
O2 Mn1 O3 2_565 . 84.75(11)
Br2 Mn1 Br1 . . 95.91(2)
O3 Mn1 Br1 . . 171.89(8)
O3 Mn1 Br2 . . 90.65(8)
N1 O1 Mn1 . . 119.7(3)
Mn1 O2 Mn1 . 2_565 110.95(11)
N2 O2 Mn1 . 2_565 123.8(2)
N2 O2 Mn1 . . 124.7(2)
C1 C2 C3 . . 117.8(5)
C1 C2 C6 . . 120.5(6)
C3 C2 C6 . . 121.7(5)
C7 N2 O2 . . 119.9(3)
C11 N2 O2 . . 118.7(3)
C11 N2 C7 . . 121.5(4)
C2 C3 H3 . . 120.3
C4 C3 C2 . . 119.4(5)
C4 C3 H3 . . 120.3
Mn1 O3 H3A . . 118(3)
Mn1 O3 H3B . . 101(4)
H3A O3 H3B . . 104(5)
C3 C4 H4 . . 119.7
C5 C4 C3 . . 120.7(5)
C5 C4 H4 . . 119.7
N1 C5 C4 . . 119.1(4)
N1 C5 H5 . . 120.4
C4 C5 H5 . . 120.4
C2 C6 H6A . . 109.5
C2 C6 H6B . . 109.5
C2 C6 H6C . . 109.5
H6A C6 H6B . . 109.5
H6A C6 H6C . . 109.5
H6B C6 H6C . . 109.5
N2 C7 H7 . . 119.4
N2 C7 C8 . . 121.2(4)
C8 C7 H7 . . 119.4
C7 C8 C9 . . 118.3(4)
C7 C8 C12 . . 120.6(4)
C9 C8 C12 . . 121.1(4)
C8 C9 H9 . . 120.1
C8 C9 C10 . . 119.8(4)
C10 C9 H9 . . 120.1
C9 C10 H10 . . 120.2
C11 C10 C9 . . 119.6(4)
C11 C10 H10 . . 120.2
N2 C11 C10 . . 119.6(4)
N2 C11 H11 . . 120.2
C10 C11 H11 . . 120.2
C8 C12 H12A . . 109.5
C8 C12 H12B . . 109.5
C8 C12 H12C . . 109.5
H12A C12 H12B . . 109.5
H12A C12 H12C . . 109.5
H12B C12 H12C . . 109.5
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_site_symmetry_2
_geom_bond_distance
Mn1 Br1 . 2.7237(7)
C1 H1 . 0.9500
C1 N1 . 1.347(6)
C1 C2 . 1.368(7)
N1 O1 . 1.328(4)
N1 C5 . 1.346(6)
Mn1 O1 . 2.129(3)
Mn1 O2 . 2.211(3)
Mn1 O2 2_565 2.219(3)
Mn1 Br2 . 2.5687(7)
Mn1 O3 . 2.245(3)
O2 N2 . 1.339(4)
C2 C3 . 1.399(8)
C2 C6 . 1.511(8)
N2 C7 . 1.336(5)
N2 C11 . 1.332(5)
C3 H3 . 0.9500
C3 C4 . 1.379(7)
O3 H3A . 0.834(19)
O3 H3B . 0.844(19)
C4 H4 . 0.9500
C4 C5 . 1.370(6)
C5 H5 . 0.9500
C6 H6A . 0.9800
C6 H6B . 0.9800
C6 H6C . 0.9800
C7 H7 . 0.9500
C7 C8 . 1.372(6)
C8 C9 . 1.377(6)
C8 C12 . 1.499(6)
C9 H9 . 0.9500
C9 C10 . 1.377(6)
C10 H10 . 0.9500
C10 C11 . 1.377(6)
C11 H11 . 0.9500
C12 H12A . 0.9800
C12 H12B . 0.9800
C12 H12C . 0.9800
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
O3 H3A Br1 1_455 0.83(2) 2.60(2) 3.410(3) 164(4) yes
O3 H3B Br1 2_565 0.84(2) 2.55(2) 3.386(3) 172(5) yes

_cod_database_fobs_code 2243039
