#------------------------------------------------------------------------------
#$Date: 2016-03-23 01:25:27 +0200 (Wed, 23 Mar 2016) $
#$Revision: 179140 $
#$URL: svn://www.crystallography.net/cod/cif/4/31/01/4310114.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_4310114
loop_
_publ_author_name
'En-Qing Gao'
'Ai-Ling Cheng'
'Yan-Xia Xu'
'Ming-Yuan He'
'Chun-Hua Yan'
_publ_contact_author_address
;
Department of Chemistry,
East China Normal University,
Shanghai 200062, China.
;
_publ_contact_author_email       eqgao@chem.ecnu.edu.cn
_publ_contact_author_fax         86-21-62233424
_publ_contact_author_name        'Prof. Chun-Hua Yan'
_publ_contact_author_phone       86-21-62233404
_publ_section_title
;
From Low-Dimensional Manganese(II) Azido Motifs to Higher-Dimensional
Materials: Structure and Magnetic Properties
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              8822
_journal_page_last               8835
_journal_paper_doi               10.1021/ic0512328
_journal_volume                  44
_journal_year                    2005
_chemical_formula_sum            'C12 H12 Mn N10 O'
_chemical_formula_weight         367.26
_chemical_name_systematic
; 
 ? 
;
_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
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 103.6010(10)
_cell_angle_gamma                90.00
_cell_formula_units_Z            8
_cell_length_a                   27.8153(5)
_cell_length_b                   8.6615(2)
_cell_length_c                   15.2390(3)
_cell_measurement_reflns_used    11696
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      27.485
_cell_measurement_theta_min      3.395
_cell_volume                     3568.46(13)
_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 0.990
_diffrn_measured_fraction_theta_max 0.990
_diffrn_measurement_device_type  'NONIUS KappaCCD Diffractometer'
_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  0.0710
_diffrn_reflns_av_sigmaI/netI    0.0611
_diffrn_reflns_limit_h_max       35
_diffrn_reflns_limit_h_min       -35
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            27217
_diffrn_reflns_theta_full        27.43
_diffrn_reflns_theta_max         27.43
_diffrn_reflns_theta_min         3.43
_diffrn_standards_decay_%        0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.761
_exptl_absorpt_correction_T_max  0.920
_exptl_absorpt_correction_T_min  0.821
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_process_details   '(Blessing, 1995, 1997)'
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.367
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             1496
_exptl_crystal_size_max          0.2
_exptl_crystal_size_mid          0.15
_exptl_crystal_size_min          0.1
_refine_diff_density_max         0.738
_refine_diff_density_min         -0.440
_refine_diff_density_rms         0.084
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.065
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     223
_refine_ls_number_reflns         4027
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.065
_refine_ls_R_factor_all          0.1097
_refine_ls_R_factor_gt           0.0591
_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)+(0.0799P)²+8.8079P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1597
_refine_ls_wR_factor_ref         0.1813
_reflns_number_gt                2503
_reflns_number_total             4027
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic0512328si20050724_112622_2.cif
_cod_data_source_block           1
_cod_database_code               4310114
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_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 0.75326(2) 0.24496(6) 0.61615(4) 0.0331(2) Uani 1 1 d . . .
N1 N 0.69032(12) 0.4217(4) 0.6032(2) 0.0407(8) Uani 1 1 d . . .
N2 N 0.52533(13) 0.5359(5) 0.6224(3) 0.0580(10) Uani 1 1 d . . .
N3 N 0.48084(13) 0.4571(5) 0.6284(3) 0.0571(10) Uani 1 1 d . . .
N4 N 0.31488(11) 0.5636(4) 0.6430(2) 0.0369(8) Uani 1 1 d . . .
N5 N 0.78492(13) 0.3695(4) 0.5126(2) 0.0415(8) Uani 1 1 d . . .
N6 N 0.82576(15) 0.4243(4) 0.5241(2) 0.0466(9) Uani 1 1 d . . .
N7 N 0.86478(17) 0.4758(6) 0.5354(3) 0.0804(14) Uani 1 1 d . . .
N8 N 0.79839(14) 0.3927(5) 0.7196(2) 0.0538(10) Uani 1 1 d . . .
N9 N 0.79211(11) 0.4991(4) 0.7625(2) 0.0367(8) Uani 1 1 d . . .
N10 N 0.78720(14) 0.6064(5) 0.8044(3) 0.0597(11) Uani 1 1 d . . .
C1 C 0.64457(14) 0.3836(5) 0.6109(3) 0.0422(10) Uani 1 1 d . . .
H1A H 0.6377 0.2801 0.6189 0.051 Uiso 1 1 calc R . .
C2 C 0.69926(15) 0.5700(5) 0.5905(3) 0.0412(10) Uani 1 1 d . . .
H2A H 0.7304 0.5979 0.5836 0.049 Uiso 1 1 calc R . .
C3 C 0.66429(17) 0.6841(5) 0.5872(3) 0.0513(11) Uani 1 1 d . . .
H3A H 0.6721 0.7868 0.5793 0.062 Uiso 1 1 calc R . .
C4 C 0.61787(17) 0.6442(6) 0.5956(3) 0.0555(12) Uani 1 1 d . . .
H4A H 0.5937 0.7194 0.5933 0.067 Uiso 1 1 calc R . .
C5 C 0.60736(14) 0.4899(5) 0.6076(3) 0.0434(10) Uani 1 1 d . . .
C6 C 0.55880(15) 0.4369(6) 0.6169(3) 0.0505(11) Uani 1 1 d . . .
H6A H 0.5523 0.3319 0.6188 0.061 Uiso 1 1 calc R . .
C7 C 0.44749(15) 0.5549(6) 0.6363(3) 0.0496(11) Uani 1 1 d . . .
H7A H 0.4542 0.6602 0.6381 0.060 Uiso 1 1 calc R . .
C8 C 0.39871(14) 0.4986(5) 0.6423(3) 0.0411(10) Uani 1 1 d . . .
C9 C 0.38770(16) 0.3434(5) 0.6472(3) 0.0501(11) Uani 1 1 d . . .
H9A H 0.4119 0.2690 0.6477 0.060 Uiso 1 1 calc R . .
C10 C 0.34108(18) 0.3005(5) 0.6514(3) 0.0509(11) Uani 1 1 d . . .
H10A H 0.3332 0.1970 0.6566 0.061 Uiso 1 1 calc R . .
C11 C 0.30570(15) 0.4145(5) 0.6480(3) 0.0443(10) Uani 1 1 d . . .
H11A H 0.2738 0.3845 0.6491 0.053 Uiso 1 1 calc R . .
C12 C 0.36149(14) 0.6041(5) 0.6420(3) 0.0426(10) Uani 1 1 d . . .
H12A H 0.3690 0.7087 0.6411 0.051 Uiso 1 1 calc R . .
O1 O 0.5672(7) -0.020(2) 0.7181(14) 0.242(7) Uani 0.607(13) 1 d P . .
O2 O 0.5797(11) 0.026(4) 0.641(2) 0.242(7) Uani 0.393(13) 1 d P . .
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'
Mn Mn 0.3368 0.7283 '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
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
N8 Mn1 N10 101.83(16) . 4_646 ?
N8 Mn1 N5 165.69(14) . 7_656 ?
N10 Mn1 N5 92.42(15) 4_646 7_656 ?
N8 Mn1 N5 88.38(14) . . ?
N10 Mn1 N5 169.57(15) 4_646 . ?
N5 Mn1 N5 77.34(14) 7_656 . ?
N8 Mn1 N4 89.65(13) . 3_545 ?
N10 Mn1 N4 89.16(13) 4_646 3_545 ?
N5 Mn1 N4 91.95(12) 7_656 3_545 ?
N5 Mn1 N4 93.11(12) . 3_545 ?
N8 Mn1 N1 88.20(13) . . ?
N10 Mn1 N1 86.13(13) 4_646 . ?
N5 Mn1 N1 91.44(12) 7_656 . ?
N5 Mn1 N1 92.09(12) . . ?
N4 Mn1 N1 174.32(11) 3_545 . ?
C2 N1 C1 117.5(3) . . ?
C2 N1 Mn1 119.4(3) . . ?
C1 N1 Mn1 123.1(3) . . ?
C6 N2 N3 109.7(4) . . ?
C7 N3 N2 110.3(4) . . ?
C11 N4 C12 117.1(3) . . ?
C11 N4 Mn1 122.3(3) . 3_455 ?
C12 N4 Mn1 120.1(3) . 3_455 ?
N6 N5 Mn1 122.7(3) . 7_656 ?
N6 N5 Mn1 126.6(3) . . ?
Mn1 N5 Mn1 102.66(14) 7_656 . ?
N7 N6 N5 179.6(5) . . ?
N9 N8 Mn1 137.0(3) . . ?
N10 N9 N8 177.9(4) . . ?
N9 N10 Mn1 152.7(3) . 4_656 ?
N1 C1 C5 123.4(4) . . ?
N1 C2 C3 122.9(4) . . ?
C4 C3 C2 119.1(4) . . ?
C3 C4 C5 119.1(4) . . ?
C1 C5 C4 117.9(4) . . ?
C1 C5 C6 119.3(4) . . ?
C4 C5 C6 122.8(4) . . ?
N2 C6 C5 119.8(4) . . ?
N3 C7 C8 119.2(4) . . ?
C12 C8 C9 117.9(4) . . ?
C12 C8 C7 119.0(4) . . ?
C9 C8 C7 123.1(4) . . ?
C10 C9 C8 119.4(4) . . ?
C9 C10 C11 118.5(4) . . ?
N4 C11 C10 123.6(4) . . ?
N4 C12 C8 123.4(4) . . ?
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 N8 2.183(4) . ?
Mn1 N10 2.194(4) 4_646 ?
Mn1 N5 2.232(3) 7_656 ?
Mn1 N5 2.255(3) . ?
Mn1 N4 2.290(3) 3_545 ?
Mn1 N1 2.299(3) . ?
N1 C2 1.331(5) . ?
N1 C1 1.346(5) . ?
N2 C6 1.282(5) . ?
N2 N3 1.434(5) . ?
N3 C7 1.282(5) . ?
N4 C11 1.322(5) . ?
N4 C12 1.347(5) . ?
N4 Mn1 2.290(3) 3_455 ?
N5 N6 1.205(5) . ?
N5 Mn1 2.232(3) 7_656 ?
N6 N7 1.148(5) . ?
N8 N9 1.167(5) . ?
N9 N10 1.153(5) . ?
N10 Mn1 2.194(4) 4_656 ?
C1 C5 1.378(6) . ?
C2 C3 1.379(6) . ?
C3 C4 1.372(6) . ?
C4 C5 1.389(6) . ?
C5 C6 1.465(6) . ?
C7 C8 1.465(6) . ?
C8 C12 1.380(5) . ?
C8 C9 1.385(6) . ?
C9 C10 1.365(6) . ?
C10 C11 1.386(6) . ?
O1 O2 1.37(3) . ?
