#------------------------------------------------------------------------------
#$Date: 2016-03-23 01:25:27 +0200 (Wed, 23 Mar 2016) $
#$Revision: 179140 $
#$URL: svn://www.crystallography.net/cod/cif/4/31/01/4310115.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_4310115
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            'C14 H14 Mn N10'
_chemical_formula_weight         377.29
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                104.866(4)
_cell_angle_beta                 104.968(4)
_cell_angle_gamma                94.773(4)
_cell_formula_units_Z            2
_cell_length_a                   8.6051(7)
_cell_length_b                   8.6212(8)
_cell_length_c                   11.8163(11)
_cell_measurement_reflns_used    23137
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      27.485
_cell_measurement_theta_min      3.395
_cell_volume                     807.96(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 0.960
_diffrn_measured_fraction_theta_max 0.960
_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  0.0614
_diffrn_reflns_av_sigmaI/netI    0.0871
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       10
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_number            11240
_diffrn_reflns_theta_full        27.50
_diffrn_reflns_theta_max         27.50
_diffrn_reflns_theta_min         3.50
_diffrn_standards_decay_%        0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.838
_exptl_absorpt_correction_T_max  0.977
_exptl_absorpt_correction_T_min  0.902
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_process_details   '(Blessing, 1995, 1997)'
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.551
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             386
_exptl_crystal_size_max          0.2
_exptl_crystal_size_mid          0.15
_exptl_crystal_size_min          0.04
_refine_diff_density_max         0.378
_refine_diff_density_min         -0.527
_refine_diff_density_rms         0.136
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.035
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     228
_refine_ls_number_reflns         3570
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.035
_refine_ls_R_factor_all          0.0978
_refine_ls_R_factor_gt           0.0427
_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)+(0.0547P)²+0.0000P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0907
_refine_ls_wR_factor_ref         0.1220
_reflns_number_gt                2226
_reflns_number_total             3570
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic0512328si20050724_112622_3.cif
_cod_data_source_block           2
_cod_original_cell_volume        807.96(12)
_cod_database_code               4310115
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, -y, -z'
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 0.30214(5) 0.48182(6) 0.00897(4) 0.03569(18) Uani 1 1 d . . .
N1 N 0.3391(3) 0.3297(3) 0.1469(2) 0.0388(6) Uani 1 1 d . . .
N2 N 0.7132(3) 0.4785(3) 0.4684(2) 0.0459(7) Uani 1 1 d . . .
N3 N 0.8398(3) 0.5264(3) 0.5782(2) 0.0440(7) Uani 1 1 d . . .
N4 N 1.2274(3) 0.6525(3) 0.8876(2) 0.0395(6) Uani 1 1 d . . .
N5 N 0.5450(3) 0.6355(3) 0.1015(2) 0.0389(6) Uani 1 1 d . . .
N6 N 0.5827(3) 0.7402(3) 0.1985(2) 0.0374(6) Uani 1 1 d . . .
N7 N 0.6164(4) 0.8401(4) 0.2900(3) 0.0593(8) Uani 1 1 d . . .
N8 N 0.0801(3) 0.3081(3) -0.1059(2) 0.0475(7) Uani 1 1 d . . .
N9 N -0.0549(3) 0.3344(3) -0.1186(2) 0.0356(6) Uani 1 1 d . . .
N10 N -0.1900(3) 0.3562(3) -0.1347(2) 0.0483(7) Uani 1 1 d . . .
C1 C 0.4602(4) 0.3742(4) 0.2523(3) 0.0393(7) Uani 1 1 d . . .
H1A H 0.5301 0.4711 0.2704 0.047 Uiso 1 1 calc R . .
C2 C 0.2372(4) 0.1910(4) 0.1243(3) 0.0467(8) Uani 1 1 d . . .
H2A H 0.1499 0.1598 0.0534 0.056 Uiso 1 1 calc R . .
C3 C 0.2554(5) 0.0935(4) 0.2002(3) 0.0545(9) Uani 1 1 d . . .
H3A H 0.1831 -0.0023 0.1805 0.065 Uiso 1 1 calc R . .
C4 C 0.3831(4) 0.1402(4) 0.3066(3) 0.0479(8) Uani 1 1 d . . .
H4A H 0.3990 0.0745 0.3586 0.057 Uiso 1 1 calc R . .
C5 C 0.4876(4) 0.2849(4) 0.3359(2) 0.0361(7) Uani 1 1 d . . .
C6 C 0.6242(4) 0.3433(4) 0.4514(3) 0.0385(7) Uani 1 1 d . . .
C7 C 0.6451(5) 0.2402(5) 0.5374(3) 0.0692(12) Uani 1 1 d . . .
H7A H 0.7390 0.2890 0.6064 0.104 Uiso 1 1 calc R . .
H7B H 0.6598 0.1336 0.4958 0.104 Uiso 1 1 calc R . .
H7C H 0.5500 0.2320 0.5650 0.104 Uiso 1 1 calc R . .
C8 C 0.9095(5) 0.7645(5) 0.5091(3) 0.0613(10) Uani 1 1 d . . .
H8A H 0.8280 0.7071 0.4339 0.092 Uiso 1 1 calc R . .
H8B H 1.0112 0.7880 0.4928 0.092 Uiso 1 1 calc R . .
H8C H 0.8764 0.8643 0.5456 0.092 Uiso 1 1 calc R . .
C9 C 0.9298(4) 0.6611(4) 0.5953(3) 0.0410(8) Uani 1 1 d . . .
C10 C 1.0644(4) 0.7169(4) 0.7113(3) 0.0387(7) Uani 1 1 d . . .
C11 C 1.1467(4) 0.8751(4) 0.7574(3) 0.0482(8) Uani 1 1 d . . .
H11A H 1.1225 0.9499 0.7136 0.058 Uiso 1 1 calc R . .
C12 C 1.2652(4) 0.9208(4) 0.8695(3) 0.0514(9) Uani 1 1 d . . .
H12A H 1.3199 1.0271 0.9026 0.062 Uiso 1 1 calc R . .
C13 C 1.3009(4) 0.8078(4) 0.9308(3) 0.0458(8) Uani 1 1 d . . .
H13A H 1.3800 0.8403 1.0064 0.055 Uiso 1 1 calc R . .
C14 C 1.1121(4) 0.6093(4) 0.7797(3) 0.0381(7) Uani 1 1 d . . .
H14A H 1.0607 0.5017 0.7483 0.046 Uiso 1 1 calc R . .
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'
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 N5 93.05(10) . 2_665 ?
N8 Mn1 N5 170.39(9) . . ?
N5 Mn1 N5 77.39(10) 2_665 . ?
N8 Mn1 N10 98.29(11) . 2_565 ?
N5 Mn1 N10 168.09(10) 2_665 2_565 ?
N5 Mn1 N10 91.19(10) . 2_565 ?
N8 Mn1 N1 89.31(9) . . ?
N5 Mn1 N1 97.58(9) 2_665 . ?
N5 Mn1 N1 92.82(9) . . ?
N10 Mn1 N1 86.23(9) 2_565 . ?
N8 Mn1 N4 88.28(9) . 1_454 ?
N5 Mn1 N4 93.18(9) 2_665 1_454 ?
N5 Mn1 N4 91.32(9) . 1_454 ?
N10 Mn1 N4 83.59(9) 2_565 1_454 ?
N1 Mn1 N4 169.08(9) . 1_454 ?
C1 N1 C2 116.7(3) . . ?
C1 N1 Mn1 122.6(2) . . ?
C2 N1 Mn1 120.66(19) . . ?
C6 N2 N3 113.8(2) . . ?
C9 N3 N2 114.0(2) . . ?
C14 N4 C13 117.3(2) . . ?
C14 N4 Mn1 125.1(2) . 1_656 ?
C13 N4 Mn1 117.61(18) . 1_656 ?
N6 N5 Mn1 130.4(2) . 2_665 ?
N6 N5 Mn1 126.1(2) . . ?
Mn1 N5 Mn1 102.61(10) 2_665 . ?
N7 N6 N5 179.1(3) . . ?
N9 N8 Mn1 125.5(2) . . ?
N10 N9 N8 177.7(3) . . ?
N9 N10 Mn1 129.1(2) . 2_565 ?
N1 C1 C5 124.2(3) . . ?
N1 C2 C3 123.4(3) . . ?
C2 C3 C4 118.7(3) . . ?
C3 C4 C5 119.9(3) . . ?
C4 C5 C1 117.0(3) . . ?
C4 C5 C6 122.1(3) . . ?
C1 C5 C6 120.9(3) . . ?
N2 C6 C5 116.5(3) . . ?
N2 C6 C7 125.8(3) . . ?
C5 C6 C7 117.7(3) . . ?
N3 C9 C10 115.6(3) . . ?
N3 C9 C8 125.7(3) . . ?
C10 C9 C8 118.6(3) . . ?
C11 C10 C14 117.1(3) . . ?
C11 C10 C9 122.5(3) . . ?
C14 C10 C9 120.3(3) . . ?
C10 C11 C12 119.3(3) . . ?
C13 C12 C11 119.3(3) . . ?
N4 C13 C12 123.2(3) . . ?
N4 C14 C10 123.8(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 N8 2.208(3) . ?
Mn1 N5 2.211(2) 2_665 ?
Mn1 N5 2.221(3) . ?
Mn1 N10 2.233(3) 2_565 ?
Mn1 N1 2.319(2) . ?
Mn1 N4 2.324(2) 1_454 ?
N1 C1 1.342(4) . ?
N1 C2 1.345(4) . ?
N2 C6 1.279(4) . ?
N2 N3 1.400(3) . ?
N3 C9 1.280(4) . ?
N4 C14 1.338(3) . ?
N4 C13 1.340(4) . ?
N4 Mn1 2.324(2) 1_656 ?
N5 N6 1.209(3) . ?
N5 Mn1 2.211(2) 2_665 ?
N6 N7 1.146(3) . ?
N8 N9 1.181(4) . ?
N9 N10 1.168(3) . ?
N10 Mn1 2.233(3) 2_565 ?
C1 C5 1.387(4) . ?
C2 C3 1.368(5) . ?
C3 C4 1.380(4) . ?
C4 C5 1.384(4) . ?
C5 C6 1.489(4) . ?
C6 C7 1.501(4) . ?
C8 C9 1.504(4) . ?
C9 C10 1.483(4) . ?
C10 C11 1.384(4) . ?
C10 C14 1.400(4) . ?
C11 C12 1.385(4) . ?
C12 C13 1.365(4) . ?
