#------------------------------------------------------------------------------
#$Date: 2018-09-26 06:29:44 +0300 (Wed, 26 Sep 2018) $
#$Revision: 211175 $
#$URL: file:///home/coder/svn-repositories/cod/cif/8/10/23/8102376.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_8102376
loop_
_publ_author_name
'Hai-Mei Feng'
'Zhu-Jun Chen'
'Xian-Wei Pan'
'Ke-Wei Lei'
_publ_section_title
;
 Crystal structure of
 hexa(N-acyl-3-hydroxy-2-naphthalenecarbo-hydrazide)-hexa(N,N-dimethyl-
 formamide)hexamanganese(III) - N,N-dimethylformamide (1:6),
 [Mn6(C13H9N2O3)6(C3H7NO)6] · (C3H7NO)6
;
_journal_issue                   1
_journal_name_full
'Zeitschrift für Kristallographie - New Crystal Structures'
_journal_page_first              51
_journal_volume                  224
_journal_year                    2009
_chemical_formula_moiety         'C96 H96 Mn6 N18 O24, 6(C3 H7 N O)'
_chemical_formula_sum            'C114 H138 Mn6 N24 O30'
_chemical_formula_weight         2654.12
_space_group_IT_number           148
_symmetry_cell_setting           hexagonal
_symmetry_space_group_name_Hall  '-R 3'
_symmetry_space_group_name_H-M   'R -3 :H'
_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                 90.00
_cell_angle_gamma                120.00
_cell_formula_units_Z            3
_cell_length_a                   32.006(5)
_cell_length_b                   32.006(5)
_cell_length_c                   10.753(2)
_cell_measurement_reflns_used    4843
_cell_measurement_temperature    273(2)
_cell_measurement_theta_max      27.46
_cell_measurement_theta_min      3.26
_cell_volume                     9539(3)
_computing_cell_refinement       'SAINT-Plus (Bruker, 2001)'
_computing_data_collection       'APEX2 (Bruker, 2004)'
_computing_data_reduction        SAINT-Plus
_computing_molecular_graphics    'SHELXTL (Bruker, 2001)'
_computing_publication_material  SHELXTL
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1997)'
_diffrn_ambient_temperature      273(2)
_diffrn_measured_fraction_theta_full 0.996
_diffrn_measured_fraction_theta_max 0.996
_diffrn_measurement_device_type  'Bruker APEX II CCD area-detector'
_diffrn_measurement_method       'φ and ω scans'
_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  0.0488
_diffrn_reflns_av_sigmaI/netI    0.0326
_diffrn_reflns_limit_h_max       41
_diffrn_reflns_limit_h_min       -41
_diffrn_reflns_limit_k_max       41
_diffrn_reflns_limit_k_min       -41
_diffrn_reflns_limit_l_max       13
_diffrn_reflns_limit_l_min       -11
_diffrn_reflns_number            28630
_diffrn_reflns_theta_full        27.46
_diffrn_reflns_theta_max         27.46
_diffrn_reflns_theta_min         3.26
_diffrn_standards_decay_%        0
_diffrn_standards_interval_count 0
_diffrn_standards_interval_time  0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.659
_exptl_absorpt_correction_T_max  0.8685
_exptl_absorpt_correction_T_min  0.7647
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   '(SADABS; Bruker, 2001)'
_exptl_crystal_colour            black
_exptl_crystal_density_diffrn    1.386
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             4140
_exptl_crystal_size_max          0.43
_exptl_crystal_size_mid          0.28
_exptl_crystal_size_min          0.22
_refine_diff_density_max         0.903
_refine_diff_density_min         -0.659
_refine_diff_density_rms         0.180
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.998
_refine_ls_hydrogen_treatment    noref
_refine_ls_matrix_type           full
_refine_ls_number_parameters     283
_refine_ls_number_reflns         4843
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.998
_refine_ls_R_factor_all          0.0609
_refine_ls_R_factor_gt           0.0465
_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)+(0.0900P)²+7.9170P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1289
_refine_ls_wR_factor_ref         0.1388
_reflns_number_gt                3896
_reflns_number_total             4843
_reflns_threshold_expression     I>2σ(I)
_cod_data_source_file            1267-2465.cff
_cod_data_source_block           shx97
_cod_original_sg_symbol_H-M      'R -3'
_cod_database_code               8102376
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-y, x-y, z'
'-x+y, -x, z'
'x+2/3, y+1/3, z+1/3'
'-y+2/3, x-y+1/3, z+1/3'
'-x+y+2/3, -x+1/3, z+1/3'
'x+1/3, y+2/3, z+2/3'
'-y+1/3, x-y+2/3, z+2/3'
'-x+y+1/3, -x+2/3, z+2/3'
'-x, -y, -z'
'y, -x+y, -z'
'x-y, x, -z'
'-x+2/3, -y+1/3, -z+1/3'
'y+2/3, -x+y+1/3, -z+1/3'
'x-y+2/3, x+1/3, -z+1/3'
'-x+1/3, -y+2/3, -z+2/3'
'y+1/3, -x+y+2/3, -z+2/3'
'x-y+1/3, x+2/3, -z+2/3'
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 1.017767(10) 0.861005(11) 0.55349(3) 0.03186(13) Uani 1 1 d . . .
C1 C 0.74597(9) 0.65745(9) 0.8189(3) 0.0487(6) Uani 1 1 d . . .
H1 H 0.7158 0.6543 0.8056 0.045(7) Uiso 1 1 calc R . .
C2 C 0.79432(10) 0.62756(9) 0.9102(2) 0.0479(6) Uani 1 1 d . . .
H2 H 0.7962 0.6041 0.9570 0.066(9) Uiso 1 1 calc R . .
C3 C 0.83547(9) 0.66605(8) 0.8641(2) 0.0441(5) Uani 1 1 d . . .
H3 H 0.8652 0.6688 0.8808 0.054(8) Uiso 1 1 calc R . .
C4 C 0.74947(9) 0.62348(8) 0.8868(3) 0.0494(6) Uani 1 1 d . . .
H4 H 0.7216 0.5972 0.9181 0.045(7) Uiso 1 1 calc R . .
C5 C 0.78753(8) 0.69765(8) 0.7681(2) 0.0385(5) Uani 1 1 d . . .
C6 C 0.83321(8) 0.70175(8) 0.7913(2) 0.0368(5) Uani 1 1 d . . .
C7 C 0.87404(8) 0.74004(8) 0.7366(2) 0.0373(5) Uani 1 1 d . . .
H7 H 0.9041 0.7432 0.7524 0.052(7) Uiso 1 1 calc R . .
C8 C 0.87156(7) 0.77324(7) 0.6602(2) 0.0314(4) Uani 1 1 d . . .
C9 C 0.91628(7) 0.80944(7) 0.59887(19) 0.0295(4) Uani 1 1 d . . .
C10 C 1.05591(7) 0.82577(7) 0.3621(2) 0.0346(5) Uani 1 1 d . . .
C11 C 1.05295(8) 0.78529(8) 0.3079(2) 0.0416(5) Uani 1 1 d . . .
H11 H 1.0256 0.7555 0.3222 0.049(7) Uiso 1 1 calc R . .
C12 C 1.0902(2) 0.7956(2) 0.8540(7) 0.144(3) Uani 1 1 d . . .
H12A H 1.1079 0.8281 0.8233 0.16(2) Uiso 1 1 calc R . .
H12B H 1.1107 0.7817 0.8541 0.28(4) Uiso 1 1 calc R . .
H12C H 1.0794 0.7958 0.9372 0.21(4) Uiso 1 1 calc R . .
C13 C 1.0227(3) 0.7150(2) 0.7908(7) 0.145(2) Uani 1 1 d . . .
H13A H 1.0114 0.7071 0.8749 0.17(3) Uiso 1 1 calc R . .
H13B H 1.0437 0.7024 0.7727 0.23(4) Uiso 1 1 calc R . .
H13C H 0.9957 0.7010 0.7349 0.58(12) Uiso 1 1 calc R . .
N3 N 1.04914(12) 0.76752(12) 0.7752(3) 0.0852(9) Uani 1 1 d . . .
C15 C 1.06227(8) 0.95350(8) 0.6373(2) 0.0409(5) Uani 1 1 d . . .
C16 C 1.07041(12) 0.99629(11) 0.7113(3) 0.0704(10) Uani 1 1 d . . .
H16A H 1.1029 1.0127 0.7424 0.132(18) Uiso 1 1 calc R . .
H16B H 1.0482 0.9859 0.7798 0.103(13) Uiso 1 1 calc R . .
H16C H 1.0654 1.0178 0.6594 0.20(3) Uiso 1 1 calc R . .
C17 C 0.9738(4) 0.7909(7) -0.0370(9) 0.246(7) Uani 1 1 d . . .
H17 H 0.9915 0.8053 -0.1087 0.296 Uiso 1 1 calc R . .
C18 C 0.9512(5) 0.8496(4) -0.0337(10) 0.297(7) Uani 1 1 d . . .
H18A H 0.9509 0.8459 -0.1224 0.446 Uiso 1 1 calc R . .
H18B H 0.9784 0.8799 -0.0102 0.446 Uiso 1 1 calc R . .
H18C H 0.9220 0.8486 -0.0079 0.446 Uiso 1 1 calc R . .
C19 C 0.9385(4) 0.7956(4) 0.1502(8) 0.259(6) Uani 1 1 d . . .
H19A H 0.9326 0.7634 0.1624 0.389 Uiso 1 1 calc R . .
H19B H 0.9092 0.7962 0.1643 0.389 Uiso 1 1 calc R . .
H19C H 0.9628 0.8170 0.2074 0.389 Uiso 1 1 calc R . .
N1 N 0.95932(6) 0.86830(6) 0.45461(18) 0.0358(4) Uani 1 1 d . . .
N2 N 1.07728(6) 0.91424(6) 0.48942(17) 0.0314(4) Uani 1 1 d . . .
C14 C 1.03294(11) 0.78855(12) 0.7006(3) 0.0619(7) Uani 1 1 d . . .
H14 H 1.0061 0.7688 0.6522 0.091(12) Uiso 1 1 calc R . .
N4 N 0.95456(18) 0.8105(2) 0.0260(4) 0.1278(16) Uani 1 1 d . . .
O1 O 1.05052(6) 0.83258(7) 0.68940(19) 0.0556(5) Uani 1 1 d . . .
O2 O 1.01902(5) 0.82063(5) 0.43171(17) 0.0429(4) Uani 1 1 d . . .
O3 O 1.02625(6) 0.91140(6) 0.66713(16) 0.0433(4) Uani 1 1 d . . .
O4 O 0.95640(5) 0.81248(5) 0.63070(15) 0.0366(3) Uani 1 1 d . . .
O5 O 0.9675(4) 0.7494(4) 0.0037(10) 0.279(5) 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'
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 O3 170.33(7) . . ?
O2 Mn1 N2 90.43(7) . . ?
O3 Mn1 N2 79.91(7) . . ?
O2 Mn1 O4 96.21(7) . . ?
O3 Mn1 O4 93.44(7) . . ?
N2 Mn1 O4 173.21(7) . . ?
O2 Mn1 O1 90.01(8) . . ?
O3 Mn1 O1 91.57(8) . . ?
N2 Mn1 O1 97.77(7) . . ?
O4 Mn1 O1 83.67(6) . . ?
O2 Mn1 N1 92.70(7) . . ?
O3 Mn1 N1 89.40(7) . . ?
N2 Mn1 N1 104.00(7) . . ?
O4 Mn1 N1 74.37(6) . . ?
O1 Mn1 N1 158.04(7) . . ?
C4 C1 C5 121.2(2) . . ?
C4 C1 H1 119.4 . . ?
C5 C1 H1 119.4 . . ?
C3 C2 C4 120.0(2) . . ?
C3 C2 H2 120.0 . . ?
C4 C2 H2 120.0 . . ?
C2 C3 C6 120.8(2) . . ?
C2 C3 H3 119.6 . . ?
C6 C3 H3 119.6 . . ?
C1 C4 C2 120.9(2) . . ?
C1 C4 H4 119.6 . . ?
C2 C4 H4 119.6 . . ?
C11 C5 C1 123.0(2) 11_566 . ?
C11 C5 C6 118.95(19) 11_566 . ?
C1 C5 C6 118.0(2) . . ?
C7 C6 C3 122.5(2) . . ?
C7 C6 C5 118.3(2) . . ?
C3 C6 C5 119.2(2) . . ?
C8 C7 C6 122.59(19) . . ?
C8 C7 H7 118.7 . . ?
C6 C7 H7 118.7 . . ?
C7 C8 C10 119.49(19) . 11_566 ?
C7 C8 C9 117.79(18) . . ?
C10 C8 C9 122.63(18) 11_566 . ?
O4 C9 N2 121.52(18) . 11_566 ?
O4 C9 C8 118.81(18) . . ?
N2 C9 C8 119.65(17) 11_566 . ?
O2 C10 C11 118.63(19) . . ?
O2 C10 C8 123.04(18) . 12_656 ?
C11 C10 C8 118.33(19) . 12_656 ?
C10 C11 C5 122.3(2) . 12_656 ?
C10 C11 H11 118.8 . . ?
C5 C11 H11 118.8 12_656 . ?
N3 C12 H12A 109.5 . . ?
N3 C12 H12B 109.5 . . ?
H12A C12 H12B 109.5 . . ?
N3 C12 H12C 109.5 . . ?
H12A C12 H12C 109.5 . . ?
H12B C12 H12C 109.5 . . ?
N3 C13 H13A 109.5 . . ?
N3 C13 H13B 109.4 . . ?
H13A C13 H13B 109.5 . . ?
N3 C13 H13C 109.5 . . ?
H13A C13 H13C 109.5 . . ?
H13B C13 H13C 109.5 . . ?
C14 N3 C12 120.8(4) . . ?
C14 N3 C13 120.6(4) . . ?
C12 N3 C13 118.2(4) . . ?
N1 C15 O3 122.2(2) 12_656 . ?
N1 C15 C16 119.3(2) 12_656 . ?
O3 C15 C16 118.5(2) . . ?
C15 C16 H16A 109.5 . . ?
C15 C16 H16B 109.5 . . ?
H16A C16 H16B 109.5 . . ?
C15 C16 H16C 109.5 . . ?
H16A C16 H16C 109.5 . . ?
H16B C16 H16C 109.5 . . ?
N4 C17 O5 117.0(10) . . ?
N4 C17 H17 121.5 . . ?
O5 C17 H17 121.6 . . ?
N4 C18 H18A 109.5 . . ?
N4 C18 H18B 109.5 . . ?
H18A C18 H18B 109.5 . . ?
N4 C18 H18C 109.5 . . ?
H18A C18 H18C 109.5 . . ?
H18B C18 H18C 109.5 . . ?
N4 C19 H19A 109.5 . . ?
N4 C19 H19B 109.5 . . ?
H19A C19 H19B 109.5 . . ?
N4 C19 H19C 109.5 . . ?
H19A C19 H19C 109.5 . . ?
H19B C19 H19C 109.5 . . ?
C15 N1 N2 109.91(17) 11_566 11_566 ?
C15 N1 Mn1 140.84(15) 11_566 . ?
N2 N1 Mn1 109.24(12) 11_566 . ?
C9 N2 N1 113.96(16) 12_656 12_656 ?
C9 N2 Mn1 131.64(14) 12_656 . ?
N1 N2 Mn1 114.38(12) 12_656 . ?
O1 C14 N3 125.1(3) . . ?
O1 C14 H14 117.5 . . ?
N3 C14 H14 117.5 . . ?
C17 N4 C19 121.1(9) . . ?
C17 N4 C18 116.7(9) . . ?
C19 N4 C18 122.2(7) . . ?
C14 O1 Mn1 119.25(19) . . ?
C10 O2 Mn1 129.44(13) . . ?
C15 O3 Mn1 112.98(14) . . ?
C9 O4 Mn1 120.68(13) . . ?
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 1.8542(16) . ?
Mn1 O3 1.9313(16) . ?
Mn1 N2 1.9391(17) . ?
Mn1 O4 1.9770(14) . ?
Mn1 O1 2.2396(18) . ?
Mn1 N1 2.2630(18) . ?
C1 C4 1.360(4) . ?
C1 C5 1.419(3) . ?
C1 H1 0.9300 . ?
C2 C3 1.369(3) . ?
C2 C4 1.398(4) . ?
C2 H2 0.9300 . ?
C3 C6 1.416(3) . ?
C3 H3 0.9300 . ?
C4 H4 0.9300 . ?
C5 C11 1.409(3) 11_566 ?
C5 C6 1.423(3) . ?
C6 C7 1.398(3) . ?
C7 C8 1.376(3) . ?
C7 H7 0.9300 . ?
C8 C10 1.435(3) 11_566 ?
C8 C9 1.472(3) . ?
C9 O4 1.285(2) . ?
C9 N2 1.319(3) 11_566 ?
C10 O2 1.337(3) . ?
C10 C11 1.380(3) . ?
C10 C8 1.435(3) 12_656 ?
C11 C5 1.409(3) 12_656 ?
C11 H11 0.9300 . ?
C12 N3 1.439(6) . ?
C12 H12A 0.9600 . ?
C12 H12B 0.9600 . ?
C12 H12C 0.9600 . ?
C13 N3 1.466(6) . ?
C13 H13A 0.9600 . ?
C13 H13B 0.9600 . ?
C13 H13C 0.9600 . ?
N3 C14 1.310(4) . ?
C15 N1 1.298(3) 12_656 ?
C15 O3 1.302(3) . ?
C15 C16 1.490(3) . ?
C16 H16A 0.9600 . ?
C16 H16B 0.9600 . ?
C16 H16C 0.9600 . ?
C17 N4 1.272(12) . ?
C17 O5 1.317(15) . ?
C17 H17 0.9300 . ?
C18 N4 1.456(10) . ?
C18 H18A 0.9600 . ?
C18 H18B 0.9600 . ?
C18 H18C 0.9600 . ?
C19 N4 1.424(8) . ?
C19 H19A 0.9600 . ?
C19 H19B 0.9600 . ?
C19 H19C 0.9600 . ?
N1 C15 1.298(3) 11_566 ?
N1 N2 1.415(2) 11_566 ?
N2 C9 1.319(3) 12_656 ?
N2 N1 1.415(2) 12_656 ?
C14 O1 1.235(4) . ?
C14 H14 0.9300 . ?
