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#$Date: 2023-02-06 10:51:06 +0200 (Mon, 06 Feb 2023) $
#$Revision: 280781 $
#$URL: file:///home/coder/svn-repositories/cod/cif/8/10/66/8106682.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_8106682
loop_
_publ_author_name
'Wu, Qiong'
'Pu, Qing'
'Liu, Dian'
'Ju, Hong-Ping'
'Qiao, Yong-Feng'
'Wang, Xiao-Yan'
'Wu, Yong-Mei'
'Zou, Tao-Yu'
'Wang, Hai'
_publ_section_title
;
 Crystal structure of
 diazido-dimethanolato-bis(μ2-2-(((3-oxidopropyl)imino)methyl)phenolato-κ4
 O:O,O′,N)dimanganese(III), C22H28Mn2N8O6
;
_journal_issue                   5
_journal_name_full
'Zeitschrift für Kristallographie - New Crystal Structures'
_journal_page_first              799
_journal_page_last               800
_journal_paper_doi               10.1515/ncrs-2017-0049
_journal_volume                  232
_journal_year                    2017
_chemical_formula_sum            'C22 H28 Mn2 N8 O6'
_chemical_formula_weight         610.40
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_symmetry_cell_setting           triclinic
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_cell_angle_alpha                98.58(3)
_cell_angle_beta                 96.15(3)
_cell_angle_gamma                107.67(3)
_cell_formula_units_Z            1
_cell_length_a                   7.2827(15)
_cell_length_b                   8.6433(17)
_cell_length_c                   11.410(2)
_cell_measurement_reflns_used    6593
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      54.977
_cell_measurement_theta_min      5.872
_cell_volume                     667.8(3)
_computing_cell_refinement       'RAPID AUTO'
_computing_data_collection       'RAPID AUTO'
_computing_data_reduction        'RAPID AUTO'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      293(2)
_diffrn_detector_area_resol_mean 0.01
_diffrn_measured_fraction_theta_full 0.991
_diffrn_measured_fraction_theta_max 0.991
_diffrn_measurement_device_type  'Rigaku RAXIS RAPID IP'
_diffrn_measurement_method       Oscillation
_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  0.0470
_diffrn_reflns_av_sigmaI/netI    0.0704
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_l_max       13
_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_number            6593
_diffrn_reflns_theta_full        27.48
_diffrn_reflns_theta_max         27.48
_diffrn_reflns_theta_min         3.21
_exptl_absorpt_coefficient_mu    0.988
_exptl_absorpt_correction_T_max  0.708
_exptl_absorpt_correction_T_min  0.435
_exptl_absorpt_correction_type   analytical
_exptl_absorpt_process_details   'ABSCOR by T.Higashi    8 March, 1995'
_exptl_crystal_colour            dark-green
_exptl_crystal_density_diffrn    1.568
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       pillar
_exptl_crystal_F_000             376
_exptl_crystal_size_max          0.35
_exptl_crystal_size_mid          0.18
_exptl_crystal_size_min          0.15
_refine_diff_density_max         0.547
_refine_diff_density_min         -0.738
_refine_diff_density_rms         0.122
_refine_ls_extinction_coef       0.041(3)
_refine_ls_extinction_method     SHELXL
_refine_ls_goodness_of_fit_ref   0.948
_refine_ls_hydrogen_treatment    empirical
_refine_ls_matrix_type           full
_refine_ls_number_parameters     172
_refine_ls_number_reflns         3041
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.948
_refine_ls_R_factor_all          0.0507
_refine_ls_R_factor_gt           0.0414
_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)+(0.1000P)²+0.0000P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1201
_refine_ls_wR_factor_ref         0.1376
_reflns_number_gt                2482
_reflns_number_total             3041
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            suppl_ncrs-2017-0049_suppl.cif
_cod_data_source_block           1
_cod_original_cell_volume        667.8(2)
_cod_original_sg_symbol_H-M      P-1
_cod_original_formula_sum        'C22 H28 Mn2 N8 O6 '
_cod_database_code               8106682
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 -0.00166(5) 0.91026(4) 0.87763(3) 0.03005(16) Uani 1 1 d . . .
O3 O -0.1103(3) 1.0652(2) 0.95540(15) 0.0329(4) Uani 1 1 d . . .
O2 O -0.2781(3) 0.7163(2) 0.91414(17) 0.0460(5) Uani 1 1 d . . .
O1 O 0.0933(3) 0.7421(2) 0.82476(15) 0.0435(4) Uani 1 1 d . . .
N1 N -0.1351(3) 0.8998(3) 0.71247(18) 0.0339(4) Uani 1 1 d . . .
N2 N 0.2557(3) 1.1140(3) 0.85423(19) 0.0446(6) Uani 1 1 d . . .
N3 N 0.2749(3) 1.1586(3) 0.7617(2) 0.0406(5) Uani 1 1 d . . .
C10 C -0.0749(4) 0.8426(3) 0.6183(2) 0.0392(6) Uani 1 1 d . . .
H10A H -0.1307 0.8551 0.5446 0.047 Uiso 1 1 calc R . .
C9 C -0.2508(4) 1.1358(4) 0.7785(2) 0.0443(6) Uani 1 1 d . . .
H9A H -0.1212 1.2065 0.7731 0.053 Uiso 1 1 calc R . .
H9B H -0.3438 1.1882 0.7516 0.053 Uiso 1 1 calc R . .
C1 C 0.1434(4) 0.7099(3) 0.7168(2) 0.0372(5) Uani 1 1 d . . .
C11 C -0.2614(4) 1.1202(4) 0.9075(2) 0.0479(7) Uani 1 1 d . . .
H11A H -0.2505 1.2267 0.9546 0.057 Uiso 1 1 calc R . .
H11B H -0.3870 1.0424 0.9126 0.057 Uiso 1 1 calc R . .
C8 C -0.2938(4) 0.9702(4) 0.6967(2) 0.0442(6) Uani 1 1 d . . .
H8A H -0.4126 0.8935 0.7125 0.053 Uiso 1 1 calc R . .
H8B H -0.3162 0.9831 0.6140 0.053 Uiso 1 1 calc R . .
C5 C 0.1300(5) 0.7225(4) 0.5069(2) 0.0518(7) Uani 1 1 d . . .
H5A H 0.0815 0.7553 0.4395 0.062 Uiso 1 1 calc R . .
C2 C 0.2687(4) 0.6169(3) 0.7056(3) 0.0464(6) Uani 1 1 d . . .
H2B H 0.3142 0.5793 0.7715 0.056 Uiso 1 1 calc R . .
N4 N 0.2960(5) 1.2001(4) 0.6714(3) 0.0702(9) Uani 1 1 d . . .
C6 C 0.0692(4) 0.7620(3) 0.6168(2) 0.0387(6) Uani 1 1 d . . .
C12 C -0.2869(7) 0.5494(4) 0.9100(4) 0.0817(13) Uani 1 1 d . . .
H12A H -0.4115 0.4870 0.9267 0.123 Uiso 1 1 calc R . .
H12B H -0.1852 0.5449 0.9690 0.123 Uiso 1 1 calc R . .
H12C H -0.2699 0.5034 0.8316 0.123 Uiso 1 1 calc R . .
C4 C 0.2579(6) 0.6376(4) 0.4969(3) 0.0602(9) Uani 1 1 d . . .
H4A H 0.3010 0.6173 0.4241 0.072 Uiso 1 1 calc R . .
C3 C 0.3252(5) 0.5805(4) 0.5953(3) 0.0564(8) Uani 1 1 d . . .
H3A H 0.4083 0.5178 0.5870 0.068 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'
O O 0.0106 0.0060 '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
O1 Mn1 O3 169.96(8) . .
O1 Mn1 O3 93.75(8) . 2_577
O3 Mn1 O3 78.76(8) . 2_577
O1 Mn1 N1 92.39(9) . .
O3 Mn1 N1 94.95(8) . .
O3 Mn1 N1 173.64(7) 2_577 .
O1 Mn1 N2 95.65(10) . .
O3 Mn1 N2 91.09(9) . .
O3 Mn1 N2 90.20(9) 2_577 .
N1 Mn1 N2 90.84(9) . .
O1 Mn1 O2 89.53(9) . .
O3 Mn1 O2 83.55(8) . .
O3 Mn1 O2 87.73(8) 2_577 .
N1 Mn1 O2 90.68(9) . .
N2 Mn1 O2 174.53(7) . .
O1 Mn1 Mn1 132.37(6) . 2_577
O3 Mn1 Mn1 39.81(5) . 2_577
O3 Mn1 Mn1 38.95(5) 2_577 2_577
N1 Mn1 Mn1 134.75(7) . 2_577
N2 Mn1 Mn1 90.83(7) . 2_577
O2 Mn1 Mn1 84.38(6) . 2_577
C11 O3 Mn1 128.68(16) . .
C11 O3 Mn1 128.95(16) . 2_577
Mn1 O3 Mn1 101.24(8) . 2_577
C12 O2 Mn1 120.8(2) . .
C1 O1 Mn1 125.92(18) . .
C10 N1 C8 118.7(2) . .
C10 N1 Mn1 121.04(19) . .
C8 N1 Mn1 120.06(16) . .
N3 N2 Mn1 123.13(18) . .
N4 N3 N2 178.6(3) . .
N1 C10 C6 126.0(2) . .
N1 C10 H10A 117.0 . .
C6 C10 H10A 117.0 . .
C11 C9 C8 112.3(3) . .
C11 C9 H9A 109.1 . .
C8 C9 H9A 109.1 . .
C11 C9 H9B 109.1 . .
C8 C9 H9B 109.1 . .
H9A C9 H9B 107.9 . .
O1 C1 C2 117.4(2) . .
O1 C1 C6 122.1(2) . .
C2 C1 C6 120.5(2) . .
O3 C11 C9 111.0(2) . .
O3 C11 H11A 109.4 . .
C9 C11 H11A 109.4 . .
O3 C11 H11B 109.4 . .
C9 C11 H11B 109.4 . .
H11A C11 H11B 108.0 . .
N1 C8 C9 112.8(2) . .
N1 C8 H8A 109.0 . .
C9 C8 H8A 109.0 . .
N1 C8 H8B 109.0 . .
C9 C8 H8B 109.0 . .
H8A C8 H8B 107.8 . .
C4 C5 C6 121.4(3) . .
C4 C5 H5A 119.3 . .
C6 C5 H5A 119.3 . .
C1 C2 C3 119.4(3) . .
C1 C2 H2B 120.3 . .
C3 C2 H2B 120.3 . .
C5 C6 C1 118.2(3) . .
C5 C6 C10 117.9(3) . .
C1 C6 C10 123.7(2) . .
O2 C12 H12A 109.5 . .
O2 C12 H12B 109.5 . .
H12A C12 H12B 109.5 . .
O2 C12 H12C 109.5 . .
H12A C12 H12C 109.5 . .
H12B C12 H12C 109.5 . .
C5 C4 C3 120.2(3) . .
C5 C4 H4A 119.9 . .
C3 C4 H4A 119.9 . .
C4 C3 C2 120.2(3) . .
C4 C3 H3A 119.9 . .
C2 C3 H3A 119.9 . .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
Mn1 O1 1.8417(19) .
Mn1 O3 1.9096(18) .
Mn1 O3 1.9446(18) 2_577
Mn1 N1 2.002(2) .
Mn1 N2 2.220(2) .
Mn1 O2 2.319(2) .
Mn1 Mn1 2.9793(11) 2_577
O3 C11 1.415(3) .
O3 Mn1 1.9446(18) 2_577
O2 C12 1.418(4) .
O1 C1 1.335(3) .
N1 C10 1.291(3) .
N1 C8 1.467(4) .
N2 N3 1.184(3) .
N3 N4 1.152(3) .
C10 C6 1.425(4) .
C10 H10A 0.9300 .
C9 C11 1.506(4) .
C9 C8 1.512(4) .
C9 H9A 0.9700 .
C9 H9B 0.9700 .
C1 C2 1.391(4) .
C1 C6 1.402(4) .
C11 H11A 0.9700 .
C11 H11B 0.9700 .
C8 H8A 0.9700 .
C8 H8B 0.9700 .
C5 C4 1.353(5) .
C5 C6 1.404(3) .
C5 H5A 0.9300 .
C2 C3 1.387(4) .
C2 H2B 0.9300 .
C12 H12A 0.9600 .
C12 H12B 0.9600 .
C12 H12C 0.9600 .
C4 C3 1.392(5) .
C4 H4A 0.9300 .
C3 H3A 0.9300 .
