#------------------------------------------------------------------------------
#$Date: 2016-02-20 18:35:30 +0200 (Sat, 20 Feb 2016) $
#$Revision: 176787 $
#$URL: svn://www.crystallography.net/cod/cif/2/21/89/2218985.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_2218985
loop_
_publ_author_name
'Yang, Gui-Bin'
'Sun, Zhen-Hai'
_publ_section_title
;
 Diazidobis{2-[3-(dimethylamino)propyliminomethyl]phenol}manganese(III)
 perchlorate
;
_journal_coeditor_code           EZ2129
_journal_issue                   8
_journal_name_full               'Acta Crystallographica Section E'
_journal_page_first              m1080
_journal_paper_doi               10.1107/S1600536808023349
_journal_volume                  64
_journal_year                    2008
_chemical_formula_iupac          '[Mn (N3)2 (C12 H18 N2 O)2] Cl O4'
_chemical_formula_moiety         'C24 H36 Mn N10 O2 +, Cl O4 -'
_chemical_formula_sum            'C24 H36 Cl Mn N10 O6'
_chemical_formula_weight         651.02
_chemical_name_systematic
;
Diazidobis{2-[3-(dimethylamino)propyliminomethyl]phenol}manganese(III)
perchlorate
;
_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                 121.121(8)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   16.8115(17)
_cell_length_b                   16.4456(18)
_cell_length_c                   12.9059(14)
_cell_measurement_reflns_used    2842
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      25.50
_cell_measurement_theta_min      1.88
_cell_volume                     3054.6(6)
_computing_cell_refinement       'SAINT-Plus (Bruker, 2001)'
_computing_data_collection       'APEX2 (Bruker, 2004)'
_computing_data_reduction        'SAINT-Plus (Bruker, 2001)'
_computing_molecular_graphics    'SHELXTL (Sheldrick, 2008)'
_computing_publication_material  'SHELXTL (Sheldrick, 2008)'
_computing_structure_refinement  'SHELXL97 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 1.000
_diffrn_measurement_device_type  'Bruker APEXII CCD area-detector'
_diffrn_measurement_method       'φ and ω'
_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  0.0439
_diffrn_reflns_av_sigmaI/netI    0.0414
_diffrn_reflns_limit_h_max       1
_diffrn_reflns_limit_h_min       -20
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       -1
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_limit_l_min       -13
_diffrn_reflns_number            3388
_diffrn_reflns_theta_full        25.50
_diffrn_reflns_theta_max         25.50
_diffrn_reflns_theta_min         1.88
_diffrn_standards_decay_%        0
_diffrn_standards_interval_count 0
_diffrn_standards_interval_time  0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.575
_exptl_absorpt_correction_T_max  0.8840
_exptl_absorpt_correction_T_min  0.7902
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   '(SADABS; Bruker, 2001)'
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.416
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             1360
_exptl_crystal_size_max          0.43
_exptl_crystal_size_mid          0.28
_exptl_crystal_size_min          0.22
_refine_diff_density_max         0.484
_refine_diff_density_min         -0.482
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.003
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     195
_refine_ls_number_reflns         2842
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.003
_refine_ls_R_factor_all          0.0555
_refine_ls_R_factor_gt           0.0435
_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)+(0.0843P)²+2.1116P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1323
_refine_ls_wR_factor_ref         0.1442
_reflns_number_gt                2216
_reflns_number_total             2842
_reflns_threshold_expression     I>2σ(I)
_cod_data_source_file            ez2129.cif
_cod_data_source_block           I
_cod_original_sg_symbol_H-M      'C 2/c'
_cod_database_code               2218985
_cod_database_fobs_code          2218985
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_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_refinement_flags
_atom_site_occupancy
Mn Mn1 0.2500 0.2500 0.5000 0.0467(2) Uani d SD 1
Cl Cl1 0.0000 0.15323(8) 0.7500 0.0711(3) Uani d S 1
O O1 0.28801(14) 0.20397(12) 0.40192(19) 0.0626(5) Uani d D 1
O O2 0.0690(2) 0.2006(3) 0.7580(4) 0.1579(17) Uani d . 1
O O3 0.0340(3) 0.1044(2) 0.8529(3) 0.1482(15) Uani d . 1
N N1 0.13856(14) 0.16698(13) 0.43275(19) 0.0481(5) Uani d . 1
N N2 -0.12645(16) 0.32706(14) 0.3901(2) 0.0576(6) Uani d . 1
N N3 0.33339(17) 0.16169(15) 0.6490(2) 0.0603(6) Uani d . 1
N N4 0.36786(18) 0.10586(17) 0.6266(2) 0.0649(6) Uani d . 1
N N5 0.4004(3) 0.0528(2) 0.6034(4) 0.0980(10) Uani d . 1
C C1 0.25785(18) 0.14208(15) 0.3267(2) 0.0497(6) Uani d D 1
C C2 0.18274(18) 0.09312(16) 0.3069(2) 0.0523(6) Uani d . 1
C C3 0.1561(2) 0.0279(2) 0.2252(3) 0.0730(9) Uani d . 1
H H3A 0.1071 -0.0055 0.2123 0.088 Uiso calc R 1
C C4 0.2015(3) 0.0129(2) 0.1639(4) 0.0896(11) Uani d . 1
H H4A 0.1828 -0.0300 0.1092 0.108 Uiso calc R 1
C C5 0.2746(3) 0.0614(2) 0.1835(3) 0.0791(10) Uani d . 1
H H5A 0.3050 0.0512 0.1417 0.095 Uiso calc R 1
C C6 0.3033(2) 0.12473(19) 0.2640(3) 0.0633(7) Uani d . 1
H H6A 0.3534 0.1565 0.2771 0.076 Uiso calc R 1
C C7 0.12924(18) 0.10820(16) 0.3631(2) 0.0513(6) Uani d . 1
H H7A 0.0826 0.0708 0.3467 0.062 Uiso calc R 1
C C8 0.06994(18) 0.17367(16) 0.4719(3) 0.0532(6) Uani d . 1
H H8A 0.1022 0.1806 0.5590 0.064 Uiso calc R 1
H H8B 0.0336 0.1241 0.4513 0.064 Uiso calc R 1
C C9 0.0061(2) 0.24542(17) 0.4104(3) 0.0572(7) Uani d . 1
H H9A -0.0247 0.2389 0.3233 0.069 Uiso calc R 1
H H9B 0.0427 0.2949 0.4322 0.069 Uiso calc R 1
C C10 -0.0665(2) 0.25332(17) 0.4460(3) 0.0583(7) Uani d . 1
H H10A -0.1053 0.2051 0.4203 0.070 Uiso calc R 1
H H10B -0.0358 0.2570 0.5335 0.070 Uiso calc R 1
C C11 -0.0775(3) 0.4036(2) 0.4465(4) 0.0850(10) Uani d . 1
H H11A -0.0216 0.4066 0.4438 0.127 Uiso calc R 1
H H11B -0.0621 0.4052 0.5292 0.127 Uiso calc R 1
H H11C -0.1169 0.4488 0.4033 0.127 Uiso calc R 1
C C12 -0.2131(2) 0.3213(2) 0.3943(4) 0.0844(11) Uani d . 1
H H12A -0.2501 0.3691 0.3585 0.127 Uiso calc R 1
H H12B -0.1974 0.3170 0.4770 0.127 Uiso calc R 1
H H12C -0.2477 0.2742 0.3502 0.127 Uiso calc R 1
H H1A 0.313(2) 0.2343(11) 0.376(3) 0.080 Uiso d D 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'
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_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle
O1 Mn1 O1 . 7_556 180.00(8)
O1 Mn1 N1 . 7_556 89.94(8)
O1 Mn1 N1 7_556 7_556 90.06(8)
O1 Mn1 N1 . . 90.06(8)
O1 Mn1 N1 7_556 . 89.94(8)
N1 Mn1 N1 7_556 . 180.00(13)
O1 Mn1 N3 . 7_556 87.82(10)
O1 Mn1 N3 7_556 7_556 92.18(10)
N1 Mn1 N3 7_556 7_556 87.83(8)
N1 Mn1 N3 . 7_556 92.17(8)
O1 Mn1 N3 . . 92.18(10)
O1 Mn1 N3 7_556 . 87.82(10)
N1 Mn1 N3 7_556 . 92.17(8)
N1 Mn1 N3 . . 87.83(8)
N3 Mn1 N3 7_556 . 180.0
O2 Cl1 O2 . 2_556 109.9(5)
O2 Cl1 O3 . 2_556 108.4(3)
O2 Cl1 O3 2_556 2_556 110.1(2)
O2 Cl1 O3 . . 110.1(2)
O2 Cl1 O3 2_556 . 108.4(3)
O3 Cl1 O3 2_556 . 109.8(3)
C1 O1 Mn1 . . 133.21(18)
C1 O1 H1A . . 104.7(14)
Mn1 O1 H1A . . 117.3(13)
C7 N1 C8 . . 117.6(2)
C7 N1 Mn1 . . 122.76(18)
C8 N1 Mn1 . . 119.59(17)
C11 N2 C12 . . 110.1(3)
C11 N2 C10 . . 112.8(2)
C12 N2 C10 . . 111.0(3)
N4 N3 Mn1 . . 117.2(2)
N5 N4 N3 . . 179.0(3)
O1 C1 C6 . . 117.9(3)
O1 C1 C2 . . 123.1(2)
C6 C1 C2 . . 119.0(3)
C1 C2 C3 . . 118.8(3)
C1 C2 C7 . . 123.1(2)
C3 C2 C7 . . 118.0(3)
C4 C3 C2 . . 120.7(3)
C4 C3 H3A . . 119.6
C2 C3 H3A . . 119.6
C5 C4 C3 . . 119.9(3)
C5 C4 H4A . . 120.0
C3 C4 H4A . . 120.0
C6 C5 C4 . . 120.8(3)
C6 C5 H5A . . 119.6
C4 C5 H5A . . 119.6
C5 C6 C1 . . 120.7(3)
C5 C6 H6A . . 119.7
C1 C6 H6A . . 119.7
N1 C7 C2 . . 127.3(2)
N1 C7 H7A . . 116.4
C2 C7 H7A . . 116.4
N1 C8 C9 . . 110.2(2)
N1 C8 H8A . . 109.6
C9 C8 H8A . . 109.6
N1 C8 H8B . . 109.6
C9 C8 H8B . . 109.6
H8A C8 H8B . . 108.1
C8 C9 C10 . . 111.8(2)
C8 C9 H9A . . 109.2
C10 C9 H9A . . 109.2
C8 C9 H9B . . 109.3
C10 C9 H9B . . 109.3
H9A C9 H9B . . 107.9
N2 C10 C9 . . 111.7(2)
N2 C10 H10A . . 109.3
C9 C10 H10A . . 109.3
N2 C10 H10B . . 109.3
C9 C10 H10B . . 109.3
H10A C10 H10B . . 107.9
N2 C11 H11A . . 109.5
N2 C11 H11B . . 109.5
H11A C11 H11B . . 109.5
N2 C11 H11C . . 109.5
H11A C11 H11C . . 109.5
H11B C11 H11C . . 109.5
N2 C12 H12A . . 109.5
N2 C12 H12B . . 109.5
H12A C12 H12B . . 109.5
N2 C12 H12C . . 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 O1 . 1.8493(18)
Mn1 O1 7_556 1.8493(18)
Mn1 N1 7_556 2.109(2)
Mn1 N1 . 2.109(2)
Mn1 N3 7_556 2.233(2)
Mn1 N3 . 2.233(2)
Cl1 O2 . 1.357(3)
Cl1 O2 2_556 1.357(3)
Cl1 O3 2_556 1.397(3)
Cl1 O3 . 1.397(3)
O1 C1 . 1.314(3)
O1 H1A . 0.828(9)
N1 C7 . 1.273(3)
N1 C8 . 1.483(3)
N2 C11 . 1.474(4)
N2 C12 . 1.489(4)
N2 C10 . 1.502(4)
N3 N4 . 1.199(4)
N4 N5 . 1.149(4)
C1 C6 . 1.400(4)
C1 C2 . 1.405(4)
C2 C3 . 1.405(4)
C2 C7 . 1.439(4)
C3 C4 . 1.377(5)
C3 H3A . 0.9300
C4 C5 . 1.374(5)
C4 H4A . 0.9300
C5 C6 . 1.370(4)
C5 H5A . 0.9300
C6 H6A . 0.9300
C7 H7A . 0.9300
C8 C9 . 1.515(4)
C8 H8A . 0.9700
C8 H8B . 0.9700
C9 C10 . 1.516(4)
C9 H9A . 0.9700
C9 H9B . 0.9700
C10 H10A . 0.9700
C10 H10B . 0.9700
C11 H11A . 0.9600
C11 H11B . 0.9600
C11 H11C . 0.9600
C12 H12A . 0.9600
C12 H12B . 0.9600
C12 H12C . 0.9600
