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#$Date: 2019-03-05 10:52:05 +0200 (Tue, 05 Mar 2019) $
#$Revision: 213973 $
#$URL: file:///home/coder/svn-repositories/cod/cif/7/01/36/7013641.cif $
#------------------------------------------------------------------------------
#
# This file is available in the Crystallography Open Database (COD),
# http://www.crystallography.net/
#
# All data on this site have been placed in the public domain by the
# contributors.
#
data_7013641
loop_
_publ_author_name
'Armentano, Donatella'
'de Munno, Giovanni'
'Guerra, Francesca'
'Faus, Juan'
'Lloret, Francesc'
'Julve, Miguel'
_publ_section_title
;
 2,2?-Bipyrimidine- and 2,3-bis(2-pyridyl)pyrazine-containing
 manganese(ii) compounds: structural and magnetic properties
;
_journal_issue                   24
_journal_name_full               'Dalton Transactions'
_journal_page_first              4626
_journal_paper_doi               10.1039/b311007a
_journal_year                    2003
_chemical_formula_sum            'C28 H28 Cl4 Mn2 N8 O4'
_chemical_formula_weight         792.26
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 93.61(3)
_cell_angle_gamma                90.00
_cell_formula_units_Z            2
_cell_length_a                   9.891(2)
_cell_length_b                   11.031(2)
_cell_length_c                   15.067(3)
_cell_measurement_temperature    293(2)
_cell_volume                     1640.7(6)
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 1.000
_diffrn_measurement_device_type  'R3m/V automatic four-circle diffractometer'
_diffrn_measurement_method       omega/2-theta-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  0.0646
_diffrn_reflns_av_sigmaI/netI    0.1332
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       0
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            3083
_diffrn_reflns_theta_full        25.05
_diffrn_reflns_theta_max         25.05
_diffrn_reflns_theta_min         2.06
_diffrn_standards_decay_%        2.2
_exptl_absorpt_coefficient_mu    1.143
_exptl_absorpt_correction_T_max  0.9141
_exptl_absorpt_correction_T_min  0.6705
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_process_details   psi-scan
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.604
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       laminar
_exptl_crystal_F_000             804
_exptl_crystal_size_max          0.38
_exptl_crystal_size_mid          0.18
_exptl_crystal_size_min          0.08
_refine_diff_density_max         0.693
_refine_diff_density_min         -0.766
_refine_diff_density_rms         0.106
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.052
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     208
_refine_ls_number_reflns         2905
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.052
_refine_ls_R_factor_all          0.1277
_refine_ls_R_factor_gt           0.0595
_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)+(0.0500P)²+0.0000P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1377
_refine_ls_wR_factor_ref         0.1495
_reflns_number_gt                1361
_reflns_number_total             2905
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            b311007a.txt
_cod_data_source_block           2
_cod_original_cell_volume        1640.6(6)
_cod_original_sg_symbol_H-M      P2(1)/c
_cod_database_code               7013641
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, y+1/2, -z+1/2'
'-x, -y, -z'
'x, -y-1/2, z-1/2'
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
Mn1 Mn 0.50017(11) 0.50511(11) 0.37378(7) 0.0309(3) Uani 1 1 d . . .
Cl1 Cl 0.34650(19) 0.42607(17) 0.48807(12) 0.0376(5) Uani 1 1 d . . .
Cl2 Cl 0.3374(3) 0.4549(3) 0.25341(19) 0.0914(10) Uani 1 1 d . . .
O1 O 0.4332(5) 0.6885(4) 0.3553(3) 0.0401(13) Uani 1 1 d . . .
H1W H 0.3437 0.7132 0.3424 0.060 Uiso 1 1 d . . .
H2W H 0.4813 0.7552 0.3801 0.060 Uiso 1 1 d . . .
N1 N 0.6363(6) 0.3378(5) 0.3689(4) 0.0314(14) Uani 1 1 d . . .
C1 C 0.6310(9) 0.2481(7) 0.4272(5) 0.042(2) Uani 1 1 d . . .
H1 H 0.5505 0.2352 0.4545 0.050 Uiso 1 1 calc R . .
C2 C 0.7385(9) 0.1738(7) 0.4489(5) 0.045(2) Uani 1 1 d . . .
H2 H 0.7295 0.1105 0.4888 0.054 Uiso 1 1 calc R . .
C3 C 0.8560(10) 0.1920(8) 0.4130(6) 0.055(3) Uani 1 1 d . . .
H3 H 0.9304 0.1432 0.4287 0.066 Uiso 1 1 calc R . .
C4 C 0.8662(8) 0.2858(8) 0.3510(5) 0.047(2) Uani 1 1 d . . .
H4 H 0.9479 0.3026 0.3263 0.057 Uiso 1 1 calc R . .
C5 C 0.7519(7) 0.3523(6) 0.3278(4) 0.0295(17) Uani 1 1 d . . .
C6 C 0.7498(7) 0.4504(6) 0.2594(4) 0.0279(17) Uani 1 1 d . . .
N2 N 0.6631(6) 0.5412(5) 0.2745(4) 0.0299(15) Uani 1 1 d . . .
C7 C 0.6632(8) 0.6369(7) 0.2206(5) 0.043(2) Uani 1 1 d . . .
H7 H 0.6044 0.7011 0.2291 0.052 Uiso 1 1 calc R . .
C8 C 0.7510(8) 0.6419(8) 0.1514(5) 0.050(2) Uani 1 1 d . . .
H8 H 0.7525 0.7116 0.1167 0.060 Uiso 1 1 calc R . .
N3 N 0.8320(7) 0.5506(6) 0.1336(4) 0.0450(18) Uani 1 1 d . . .
C9 C 0.8277(7) 0.4528(6) 0.1846(5) 0.0323(18) Uani 1 1 d . . .
C10 C 0.9083(8) 0.3462(7) 0.1571(5) 0.0365(19) Uani 1 1 d . . .
N4 N 0.8453(6) 0.2383(6) 0.1527(4) 0.0381(17) Uani 1 1 d . . .
C11 C 0.9130(8) 0.1436(8) 0.1230(5) 0.046(2) Uani 1 1 d . . .
H11 H 0.8692 0.0691 0.1187 0.055 Uiso 1 1 calc R . .
C12 C 1.0461(8) 0.1506(8) 0.0979(5) 0.047(2) Uani 1 1 d . . .
H12 H 1.0890 0.0825 0.0767 0.056 Uiso 1 1 calc R . .
C13 C 1.1126(8) 0.2597(8) 0.1050(6) 0.053(3) Uani 1 1 d . . .
H13 H 1.2026 0.2671 0.0913 0.064 Uiso 1 1 calc R . .
C14 C 1.0393(8) 0.3593(8) 0.1339(5) 0.051(2) Uani 1 1 d . . .
H14 H 1.0801 0.4353 0.1374 0.062 Uiso 1 1 calc R . .
O2 O 0.4524(5) 0.4183(4) 0.0772(3) 0.0291(12) Uani 1 1 d . . .
H4W H 0.5439 0.4325 0.0827 0.060 Uiso 1 1 d . . .
H3W H 0.4155 0.4295 0.1309 0.060 Uiso 1 1 d . . .
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'
Cl Cl 0.1484 0.1585 '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
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
O1 Mn1 N1 159.3(2) . . ?
O1 Mn1 N2 88.60(19) . . ?
N1 Mn1 N2 71.4(2) . . ?
O1 Mn1 Cl2 86.16(15) . . ?
N1 Mn1 Cl2 99.02(16) . . ?
N2 Mn1 Cl2 90.73(16) . . ?
O1 Mn1 Cl1 102.74(14) . . ?
N1 Mn1 Cl1 97.14(16) . . ?
N2 Mn1 Cl1 168.52(16) . . ?
Cl2 Mn1 Cl1 91.81(9) . . ?
O1 Mn1 Cl1 89.32(15) . 3_666 ?
N1 Mn1 Cl1 86.95(15) . 3_666 ?
N2 Mn1 Cl1 94.14(15) . 3_666 ?
Cl2 Mn1 Cl1 173.27(10) . 3_666 ?
Cl1 Mn1 Cl1 84.32(7) . 3_666 ?
Mn1 Cl1 Mn1 95.68(7) . 3_666 ?
C1 N1 C5 117.7(6) . . ?
C1 N1 Mn1 122.1(5) . . ?
C5 N1 Mn1 116.0(5) . . ?
N1 C1 C2 122.8(7) . . ?
C3 C2 C1 120.1(8) . . ?
C2 C3 C4 118.9(8) . . ?
C5 C4 C3 118.1(8) . . ?
N1 C5 C4 122.0(7) . . ?
N1 C5 C6 115.4(6) . . ?
C4 C5 C6 122.5(7) . . ?
N2 C6 C9 120.5(6) . . ?
N2 C6 C5 113.8(6) . . ?
C9 C6 C5 125.6(6) . . ?
C7 N2 C6 117.5(6) . . ?
C7 N2 Mn1 124.1(5) . . ?
C6 N2 Mn1 117.4(4) . . ?
N2 C7 C8 120.6(7) . . ?
N3 C8 C7 122.2(7) . . ?
C8 N3 C9 117.3(6) . . ?
N3 C9 C6 121.3(6) . . ?
N3 C9 C10 116.2(6) . . ?
C6 C9 C10 122.4(7) . . ?
N4 C10 C14 121.6(7) . . ?
N4 C10 C9 117.2(6) . . ?
C14 C10 C9 121.1(8) . . ?
C11 N4 C10 118.0(7) . . ?
N4 C11 C12 123.4(8) . . ?
C13 C12 C11 118.9(8) . . ?
C12 C13 C14 117.2(8) . . ?
C10 C14 C13 120.8(8) . . ?
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Mn1 O1 2.141(5) . ?
Mn1 N1 2.289(6) . ?
Mn1 N2 2.302(6) . ?
Mn1 Cl2 2.412(3) . ?
Mn1 Cl1 2.523(2) . ?
Mn1 Cl1 2.610(2) 3_666 ?
Cl1 Mn1 2.610(2) 3_666 ?
N1 C1 1.327(9) . ?
N1 C5 1.344(8) . ?
C1 C2 1.366(10) . ?
C2 C3 1.328(10) . ?
C3 C4 1.402(11) . ?
C4 C5 1.374(9) . ?
C5 C6 1.493(9) . ?
C6 N2 1.347(8) . ?
C6 C9 1.406(9) . ?
N2 C7 1.332(8) . ?
C7 C8 1.400(10) . ?
C8 N3 1.325(9) . ?
N3 C9 1.326(8) . ?
C9 C10 1.494(10) . ?
C10 N4 1.343(9) . ?
C10 C14 1.371(10) . ?
N4 C11 1.333(9) . ?
C11 C12 1.394(10) . ?
C12 C13 1.372(11) . ?
C13 C14 1.401(11) . ?
loop_
_geom_hbond_atom_site_label_D
_geom_hbond_atom_site_label_H
_geom_hbond_atom_site_label_A
_geom_hbond_distance_DH
_geom_hbond_distance_HA
_geom_hbond_distance_DA
_geom_hbond_angle_DHA
_geom_hbond_site_symmetry_A
O1 H1W N4 0.93 1.90 2.805(8) 163.2 2_655
O2 H3W Cl2 0.92 2.07 2.981(5) 178.5 .
O1 H2W O2 0.94 2.01 2.932(6) 167.3 2_655
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
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
N1 C5 C6 N2 27.8(9) . . . . ?
N3 C9 C10 N4 -130.8(8) . . . . ?
C5 C6 C9 C10 9.6(11) . . . . ?
