#------------------------------------------------------------------------------
#$Date: 2019-07-31 07:41:55 +0300 (Wed, 31 Jul 2019) $
#$Revision: 217324 $
#$URL: file:///home/coder/svn-repositories/cod/cif/2/24/30/2243038.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_2243038
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)2 (H2 O)4], 2C6 H7 N O'
_chemical_formula_moiety         'C12 H22 Br4 Mn2 N2 O6, 2(C6 H7 N O)'
_chemical_formula_sum            'C24 H36 Br4 Mn2 N4 O8'
_chemical_formula_weight         938.09
_chemical_name_systematic
'Bis(μ-2-methylpyridine N-oxide)bis[diaquadibromidomanganese(II)]--2-methylpyridine N-oxide (1/2)'
_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                110.048(8)
_cell_angle_beta                 90.336(7)
_cell_angle_gamma                98.052(7)
_cell_formula_units_Z            1
_cell_length_a                   8.9560(8)
_cell_length_b                   9.7922(9)
_cell_length_c                   10.2945(8)
_cell_measurement_reflns_used    4291
_cell_measurement_temperature    170
_cell_measurement_theta_max      33.1600
_cell_measurement_theta_min      2.2600
_cell_volume                     838.34(13)
_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 0.997
_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  0.0534
_diffrn_reflns_av_unetI/netI     0.0621
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       13
_diffrn_reflns_limit_l_min       -13
_diffrn_reflns_number            8918
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.485
_diffrn_reflns_theta_min         2.109
_diffrn_source                   'fine-focus sealed X-ray tube'
_exptl_absorpt_coefficient_mu    5.568
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.57999
_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    1.858
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             462
_exptl_crystal_size_max          0.2
_exptl_crystal_size_mid          0.2
_exptl_crystal_size_min          0.1
_refine_diff_density_max         0.724
_refine_diff_density_min         -0.615
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.001
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     208
_refine_ls_number_reflns         3838
_refine_ls_number_restraints     4
_refine_ls_restrained_S_all      1.000
_refine_ls_R_factor_all          0.0584
_refine_ls_R_factor_gt           0.0374
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[σ²(Fo²)+(0.0319P)²] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0735
_refine_ls_wR_factor_ref         0.0800
_reflns_number_gt                2931
_reflns_number_total             3838
_reflns_threshold_expression     'I > 2σ(I)'
_cod_data_source_file            su5505sup1.cif
_cod_data_source_block           II
_cod_database_code               2243038
_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   0.402
_shelx_estimated_absorpt_t_max   0.606
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 0.97900(4) 0.80035(4) 0.74971(4) 0.02737(11) Uani d 1
O O1 1.0009(3) 0.4219(3) 0.5880(2) 0.0216(5) Uani d 1
C C1 0.9673(4) 0.2520(4) 0.7046(4) 0.0271(8) Uani d 1
Mn Mn1 0.82268(6) 0.55061(6) 0.56887(5) 0.02123(13) Uani d 1
N N1 1.0302(3) 0.3845(3) 0.6999(3) 0.0219(6) Uani d 1
Br Br2 0.62884(4) 0.49697(4) 0.74319(4) 0.03065(11) Uani d 1
C C2 1.0052(4) 0.2179(4) 0.8211(4) 0.0304(9) Uani d 1
H H2 0.962787 0.125920 0.827065 0.037 Uiso calc 1
O O3 0.7281(3) 0.3472(3) 0.3927(3) 0.0267(6) Uani d 1
H H3A 0.647(3) 0.288(4) 0.388(4) 0.043(13) Uiso d 1
H H3B 0.799(3) 0.297(4) 0.359(4) 0.036(12) Uiso d 1
C C3 1.1028(5) 0.3150(4) 0.9273(4) 0.0329(9) Uani d 1
H H3 1.127202 0.290351 1.005596 0.039 Uiso calc 1
C C4 1.1643(5) 0.4487(5) 0.9180(4) 0.0368(10) Uani d 1
H H4 1.231315 0.517477 0.990012 0.044 Uiso calc 1
O O4 0.6790(3) 0.6595(3) 0.4807(3) 0.0268(6) Uani d 1
H H4A 0.642(6) 0.726(4) 0.542(4) 0.09(2) Uiso d 1
H H4B 0.614(5) 0.614(6) 0.417(4) 0.10(2) Uiso d 1
C C5 1.1269(4) 0.4809(4) 0.8023(4) 0.0320(9) Uani d 1
H H5 1.169778 0.571996 0.794612 0.038 Uiso calc 1
C C6 0.8633(5) 0.1536(4) 0.5885(4) 0.0377(10) Uani d 1
H H6A 0.769395 0.194740 0.589890 0.057 Uiso calc 1
H H6B 0.840725 0.056545 0.597618 0.057 Uiso calc 1
H H6C 0.910470 0.144060 0.500794 0.057 Uiso calc 1
N N2 0.4507(3) 0.0303(3) 0.2438(3) 0.0262(7) Uani d 1
O O2 0.4865(3) 0.1344(3) 0.3682(3) 0.0288(6) Uani d 1
C C7 0.5133(4) -0.0960(4) 0.2104(4) 0.0292(9) Uani d 1
C C8 0.4748(6) -0.2028(5) 0.0806(4) 0.0455(12) Uani d 1
H H8 0.518213 -0.290783 0.054919 0.055 Uiso calc 1
C C9 0.3744(6) -0.1829(6) -0.0117(5) 0.0544(14) Uani d 1
H H9 0.349499 -0.256046 -0.100515 0.065 Uiso calc 1
C C10 0.3105(5) -0.0539(6) 0.0278(5) 0.0516(13) Uani d 1
H H10 0.238985 -0.039227 -0.032830 0.062 Uiso calc 1
C C11 0.3517(4) 0.0509(5) 0.1542(4) 0.0378(10) Uani d 1
H H11 0.310341 0.140125 0.180201 0.045 Uiso calc 1
C C12 0.6228(5) -0.1073(4) 0.3143(4) 0.0383(10) Uani d 1
H H12A 0.713697 -0.035107 0.324504 0.057 Uiso calc 1
H H12B 0.650204 -0.206492 0.283156 0.057 Uiso calc 1
H H12C 0.576598 -0.087782 0.403703 0.057 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
O1 Mn1 O1 . 2_766 74.40(9)
Mn1 O1 Mn1 . 2_766 105.60(9)
N1 O1 Mn1 . . 125.53(19)
N1 O1 Mn1 . 2_766 124.62(18)
N1 C1 C2 . . 117.5(3)
N1 C1 C6 . . 118.5(3)
C2 C1 C6 . . 124.1(3)
O1 Mn1 Br1 . . 91.54(6)
O1 Mn1 Br1 2_766 . 85.90(6)
O1 Mn1 Br2 . . 101.36(6)
O1 Mn1 Br2 2_766 . 175.09(6)
O1 Mn1 O3 . . 84.60(9)
Br2 Mn1 Br1 . . 96.79(2)
O3 Mn1 Br1 . . 169.21(8)
O3 Mn1 O1 . 2_766 83.36(9)
O3 Mn1 Br2 . . 93.85(7)
O4 Mn1 Br1 . . 95.42(8)
O4 Mn1 O1 . 2_766 87.70(9)
O4 Mn1 O1 . . 160.29(10)
O4 Mn1 Br2 . . 96.11(8)
O4 Mn1 O3 . . 85.19(10)
C1 N1 O1 . . 120.1(3)
C5 N1 O1 . . 117.8(3)
C5 N1 C1 . . 122.0(3)
C1 C2 H2 . . 119.2
C3 C2 C1 . . 121.5(3)
C3 C2 H2 . . 119.2
Mn1 O3 H3A . . 128(3)
Mn1 O3 H3B . . 110(3)
H3A O3 H3B . . 109(4)
C2 C3 H3 . . 120.5
C2 C3 C4 . . 119.0(3)
C4 C3 H3 . . 120.5
C3 C4 H4 . . 120.5
C5 C4 C3 . . 119.0(4)
C5 C4 H4 . . 120.5
Mn1 O4 H4A . . 112(4)
Mn1 O4 H4B . . 123(4)
H4A O4 H4B . . 110(5)
N1 C5 C4 . . 121.0(3)
N1 C5 H5 . . 119.5
C4 C5 H5 . . 119.5
C1 C6 H6A . . 109.5
C1 C6 H6B . . 109.5
C1 C6 H6C . . 109.5
H6A C6 H6B . . 109.5
H6A C6 H6C . . 109.5
H6B C6 H6C . . 109.5
O2 N2 C7 . . 119.0(3)
O2 N2 C11 . . 119.7(3)
C11 N2 C7 . . 121.3(3)
N2 C7 C8 . . 118.2(4)
N2 C7 C12 . . 117.4(3)
C8 C7 C12 . . 124.4(4)
C7 C8 H8 . . 119.5
C9 C8 C7 . . 121.1(5)
C9 C8 H8 . . 119.5
C8 C9 H9 . . 120.5
C8 C9 C10 . . 118.9(4)
C10 C9 H9 . . 120.5
C9 C10 H10 . . 120.4
C11 C10 C9 . . 119.3(4)
C11 C10 H10 . . 120.4
N2 C11 C10 . . 121.2(4)
N2 C11 H11 . . 119.4
C10 C11 H11 . . 119.4
C7 C12 H12A . . 109.5
C7 C12 H12B . . 109.5
C7 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 . 2.7009(7)
Mn1 O1 . 2.214(2)
O1 Mn1 2_766 2.321(2)
O1 N1 . 1.358(3)
C1 N1 . 1.357(4)
C1 C2 . 1.402(5)
C1 C6 . 1.473(5)
Mn1 Br2 . 2.6340(7)
Mn1 O3 . 2.237(3)
Mn1 O4 . 2.157(3)
N1 C5 . 1.353(5)
C2 H2 . 0.9500
C2 C3 . 1.381(5)
O3 H3A . 0.852(19)
O3 H3B . 0.857(19)
C3 H3 . 0.9500
C3 C4 . 1.383(5)
C4 H4 . 0.9500
C4 C5 . 1.382(5)
O4 H4A . 0.846(19)
O4 H4B . 0.83(2)
C5 H5 . 0.9500
C6 H6A . 0.9800
C6 H6B . 0.9800
C6 H6C . 0.9800
N2 O2 . 1.338(4)
N2 C7 . 1.366(5)
N2 C11 . 1.359(5)
C7 C8 . 1.390(5)
C7 C12 . 1.490(5)
C8 H8 . 0.9500
C8 C9 . 1.384(7)
C9 H9 . 0.9500
C9 C10 . 1.394(7)
C10 H10 . 0.9500
C10 C11 . 1.362(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 O2 . 0.85(2) 1.89(2) 2.731(4) 171(4) yes
O3 H3B Br1 2_766 0.86(2) 2.44(2) 3.282(3) 168(4) yes
O4 H4A O2 2_666 0.85(2) 1.91(3) 2.721(4) 161(5) yes
O4 H4B Br2 2_666 0.83(4) 2.59(4) 3.403(3) 167(4) yes

_cod_database_fobs_code 2243038
