#------------------------------------------------------------------------------
#$Date: 2016-03-23 01:54:03 +0200 (Wed, 23 Mar 2016) $
#$Revision: 179160 $
#$URL: svn://www.crystallography.net/cod/cif/4/31/21/4312199.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_4312199
loop_
_publ_author_name
'Mei Yuan'
'Song Gao'
'Hao-Ling Sun'
'Gang Su'
_publ_section_title
;
 An Antiferromagnetic Mn(III) Chain Bridged by Hydrogencyanamide:
 [MnIII(5-Brsalen)(μ1,3-NCNH)]n
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              8221
_journal_page_last               8223
_journal_paper_doi               10.1021/ic048547s
_journal_volume                  43
_journal_year                    2004
_chemical_formula_sum            'C17 H13 Br2 Mn N4 O2'
_chemical_formula_weight         520.07
_chemical_name_systematic
; 
 ? 
;
_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                 105.978(2)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   13.3699(4)
_cell_length_b                   11.7277(4)
_cell_length_c                   11.5495(3)
_cell_measurement_reflns_used    36580
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      27.485
_cell_measurement_theta_min      3.395
_cell_volume                     1740.98(9)
_computing_cell_refinement       'HKL Scalepack (Otwinowski & Minor, 1997)'
_computing_data_collection       'KappaCCD (Nonius B. V., 1998)'
_computing_data_reduction
'HKL Denzo (Otwinowski & Minor, 1997) & maXus (Mackay et al., 1998)'
_computing_molecular_graphics    'Bruker SHELXTL V5.1 (Sheldrick, 1998)'
_computing_publication_material  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1997)'
_diffrn_ambient_temperature      293(2)
_diffrn_detector_area_resol_mean 0.76
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device_type  'NONIUS KappaCCD'
_diffrn_measurement_method       CCD
_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  0.0715
_diffrn_reflns_av_sigmaI/netI    0.0446
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       14
_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_number            32779
_diffrn_reflns_theta_full        27.50
_diffrn_reflns_theta_max         27.50
_diffrn_reflns_theta_min         3.47
_exptl_absorpt_coefficient_mu    5.369
_exptl_absorpt_correction_T_max  0.659
_exptl_absorpt_correction_T_min  0.555
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_process_details   '(Blessing, 1995, 1997)'
_exptl_crystal_colour            'deep red'
_exptl_crystal_density_diffrn    1.984
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             1016
_exptl_crystal_size_max          0.08
_exptl_crystal_size_mid          0.08
_exptl_crystal_size_min          0.05
_refine_diff_density_max         0.354
_refine_diff_density_min         -0.449
_refine_diff_density_rms         0.077
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.979
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     235
_refine_ls_number_reflns         3984
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.979
_refine_ls_R_factor_all          0.0632
_refine_ls_R_factor_gt           0.0326
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[σ²(Fo²)+(0.0382P)²+0.0000P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0670
_refine_ls_wR_factor_ref         0.0733
_reflns_number_gt                2703
_reflns_number_total             3984
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic048547ssi20041017_045829.cif
_cod_data_source_block           MnNCNH
_cod_database_code               4312199
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 1.09617(3) 0.29667(4) 0.54734(4) 0.03452(12) Uani 1 1 d . . .
Br1 Br 0.54324(2) 0.13907(3) 0.43866(3) 0.05740(12) Uani 1 1 d . . .
Br2 Br 1.60856(2) 0.58533(3) 0.71176(3) 0.05124(11) Uani 1 1 d . . .
O1 O 1.17166(14) 0.41355(16) 0.64480(16) 0.0398(5) Uani 1 1 d . . .
O2 O 0.97276(14) 0.34164(16) 0.58252(17) 0.0388(5) Uani 1 1 d . . .
N1 N 1.22212(17) 0.23744(19) 0.51005(18) 0.0337(5) Uani 1 1 d . . .
N2 N 1.02764(17) 0.16698(19) 0.44461(19) 0.0339(5) Uani 1 1 d . . .
N3 N 1.0647(2) 0.3980(2) 0.3762(2) 0.0461(6) Uani 1 1 d . . .
H3A H 1.0281 0.4589 0.3721 0.055 Uiso 1 1 calc R . .
N4 N 1.1311(2) 0.3440(2) 0.2051(2) 0.0473(6) Uani 1 1 d . . .
C1 C 1.2658(2) 0.4511(2) 0.6509(2) 0.0358(6) Uani 1 1 d . . .
C2 C 1.3007(2) 0.5516(3) 0.7157(2) 0.0419(7) Uani 1 1 d . . .
H2A H 1.2556 0.5916 0.7495 0.050 Uiso 1 1 calc R . .
C3 C 1.3999(2) 0.5923(3) 0.7305(3) 0.0435(7) Uani 1 1 d . . .
H3B H 1.4212 0.6588 0.7741 0.052 Uiso 1 1 calc R . .
C4 C 1.4683(2) 0.5340(3) 0.6802(2) 0.0408(7) Uani 1 1 d . . .
C5 C 1.4370(2) 0.4369(3) 0.6156(2) 0.0408(7) Uani 1 1 d . . .
H5A H 1.4833 0.3987 0.5820 0.049 Uiso 1 1 calc R . .
C6 C 1.3363(2) 0.3934(2) 0.5988(2) 0.0350(6) Uani 1 1 d . . .
C7 C 1.3104(2) 0.2871(2) 0.5345(2) 0.0378(7) Uani 1 1 d . . .
H7A H 1.3627 0.2518 0.5086 0.045 Uiso 1 1 calc R . .
C8 C 1.2079(2) 0.1224(2) 0.4562(3) 0.0455(7) Uani 1 1 d . . .
H8A H 1.2259 0.0653 0.5193 0.055 Uiso 1 1 calc R . .
H8B H 1.2535 0.1126 0.4045 0.055 Uiso 1 1 calc R . .
C9 C 1.0960(2) 0.1069(2) 0.3834(3) 0.0395(7) Uani 1 1 d . . .
H9A H 1.0861 0.1378 0.3031 0.047 Uiso 1 1 calc R . .
H9B H 1.0787 0.0265 0.3762 0.047 Uiso 1 1 calc R . .
C10 C 0.9310(2) 0.1408(2) 0.4216(2) 0.0364(6) Uani 1 1 d . . .
H10A H 0.9074 0.0799 0.3697 0.044 Uiso 1 1 calc R . .
C11 C 0.8558(2) 0.1984(2) 0.4701(2) 0.0347(6) Uani 1 1 d . . .
C12 C 0.8802(2) 0.2937(2) 0.5486(2) 0.0350(6) Uani 1 1 d . . .
C13 C 0.8001(2) 0.3388(2) 0.5921(3) 0.0409(7) Uani 1 1 d . . .
H13A H 0.8141 0.4016 0.6432 0.049 Uiso 1 1 calc R . .
C14 C 0.7027(2) 0.2934(3) 0.5616(3) 0.0431(7) Uani 1 1 d . . .
H14A H 0.6517 0.3240 0.5934 0.052 Uiso 1 1 calc R . .
C15 C 0.6794(2) 0.2013(3) 0.4831(3) 0.0407(7) Uani 1 1 d . . .
C16 C 0.7537(2) 0.1564(2) 0.4361(3) 0.0381(7) Uani 1 1 d . . .
H16A H 0.7365 0.0971 0.3807 0.046 Uiso 1 1 calc R . .
C17 C 1.0966(2) 0.3730(2) 0.2832(3) 0.0393(7) Uani 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'
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'
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
O2 Mn1 O1 91.40(8) . . ?
O2 Mn1 N1 175.69(9) . . ?
O1 Mn1 N1 92.15(9) . . ?
O2 Mn1 N2 93.20(9) . . ?
O1 Mn1 N2 175.21(9) . . ?
N1 Mn1 N2 83.20(9) . . ?
O2 Mn1 N3 94.52(9) . . ?
O1 Mn1 N3 94.64(9) . . ?
N1 Mn1 N3 87.63(9) . . ?
N2 Mn1 N3 86.31(9) . . ?
O2 Mn1 N4 91.59(9) . 4_566 ?
O1 Mn1 N4 94.94(9) . 4_566 ?
N1 Mn1 N4 85.67(9) . 4_566 ?
N2 Mn1 N4 83.63(9) . 4_566 ?
N3 Mn1 N4 168.50(9) . 4_566 ?
C1 O1 Mn1 128.54(16) . . ?
C12 O2 Mn1 128.67(17) . . ?
C7 N1 C8 121.0(2) . . ?
C7 N1 Mn1 125.7(2) . . ?
C8 N1 Mn1 113.24(17) . . ?
C10 N2 C9 120.5(2) . . ?
C10 N2 Mn1 125.35(19) . . ?
C9 N2 Mn1 113.89(17) . . ?
C17 N3 Mn1 125.9(2) . . ?
C17 N4 Mn1 138.3(2) . 4_565 ?
O1 C1 C2 118.8(2) . . ?
O1 C1 C6 123.6(3) . . ?
C2 C1 C6 117.6(3) . . ?
C3 C2 C1 121.6(3) . . ?
C2 C3 C4 120.0(3) . . ?
C5 C4 C3 120.1(3) . . ?
C5 C4 Br2 120.4(2) . . ?
C3 C4 Br2 119.3(2) . . ?
C4 C5 C6 121.2(3) . . ?
C5 C6 C1 119.5(3) . . ?
C5 C6 C7 118.0(2) . . ?
C1 C6 C7 122.4(3) . . ?
N1 C7 C6 125.7(3) . . ?
N1 C8 C9 109.7(2) . . ?
N2 C9 C8 109.0(2) . . ?
N2 C10 C11 125.2(3) . . ?
C16 C11 C12 119.4(2) . . ?
C16 C11 C10 117.0(2) . . ?
C12 C11 C10 123.6(3) . . ?
O2 C12 C13 118.6(2) . . ?
O2 C12 C11 123.9(2) . . ?
C13 C12 C11 117.5(3) . . ?
C14 C13 C12 122.0(3) . . ?
C13 C14 C15 120.0(3) . . ?
C16 C15 C14 120.3(3) . . ?
C16 C15 Br1 119.6(2) . . ?
C14 C15 Br1 120.1(2) . . ?
C15 C16 C11 120.8(3) . . ?
N4 C17 N3 174.3(3) . . ?
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 O2 1.8801(18) . ?
Mn1 O1 1.8812(19) . ?
Mn1 N1 1.976(2) . ?
Mn1 N2 1.991(2) . ?
Mn1 N3 2.245(2) . ?
Mn1 N4 2.407(3) 4_566 ?
Br1 C15 1.896(3) . ?
Br2 C4 1.907(3) . ?
O1 C1 1.317(3) . ?
O2 C12 1.317(3) . ?
N1 C7 1.277(3) . ?
N1 C8 1.476(4) . ?
N2 C10 1.283(3) . ?
N2 C9 1.479(3) . ?
N3 C17 1.294(4) . ?
N4 C17 1.171(4) . ?
N4 Mn1 2.407(3) 4_565 ?
C1 C2 1.406(4) . ?
C1 C6 1.422(4) . ?
C2 C3 1.375(4) . ?
C3 C4 1.391(4) . ?
C4 C5 1.363(4) . ?
C5 C6 1.403(4) . ?
C6 C7 1.443(4) . ?
C8 C9 1.511(4) . ?
C10 C11 1.446(4) . ?
C11 C16 1.401(4) . ?
C11 C12 1.419(4) . ?
C12 C13 1.405(4) . ?
C13 C14 1.361(4) . ?
C14 C15 1.390(4) . ?
C15 C16 1.363(4) . ?
