#------------------------------------------------------------------------------
#$Date: 2016-02-16 02:10:39 +0100 (mar 16 de feb de 2016) $
#$Revision: 176453 $
#$URL: svn://www.crystallography.net/cod/cif/7/01/13/7011380.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_7011380
loop_
_publ_author_name
'Hitoshi Miyasaka'
'Rodolphe Clérac'
'Tomohiko Ishii'
'Ho-Chol Chang'
'Susumu Kitagawa'
'Masahiro Yamashita'
_publ_section_title
;
 Out-of-plane dimers of Mn(III) quadridentate Schiff-base complexes
 with saltmen2− and naphtmen2− ligands: structure
 analysis and ferromagnetic exchange
;
_journal_issue                   7
_journal_name_full               'J. Chem. Soc., Dalton Trans.'
_journal_page_first              1528
_journal_page_last               1534
_journal_paper_doi               10.1039/b111094m
_journal_year                    2002
_chemical_formula_sum            'C58 H64 Cl2 Mn2 N4 O16'
_chemical_formula_weight         1253.94
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_symmetry_Int_Tables_number      2
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_cell_angle_alpha                101.76(7)
_cell_angle_beta                 94.45(7)
_cell_angle_gamma                112.93(5)
_cell_formula_units_Z            1
_cell_length_a                   13.360(8)
_cell_length_b                   13.76(1)
_cell_length_c                   8.463(6)
_cell_measurement_reflns_used    25
_cell_measurement_temperature    296.2
_cell_measurement_theta_max      14.9
_cell_measurement_theta_min      14.7
_cell_volume                     1381.3(18)
_computing_cell_refinement       'MSC/AFC Diffractometer Control'
_computing_data_collection       'MSC/AFC Diffractometer Control'
_computing_data_reduction        'teXsan Ver. 1.11'
_computing_publication_material  'teXsan Ver. 1.11'
_computing_structure_refinement  'teXsan Ver. 1.10'
_computing_structure_solution    'DIRDIF94 (PATTY)'
_diffrn_measured_fraction_theta_full 0.9949
_diffrn_measured_fraction_theta_max 0.9949
_diffrn_measurement_device_type  'Rigaku AFC7R'
_diffrn_measurement_method       ω-2θ
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.7107
_diffrn_reflns_av_R_equivalents  0.060
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       0
_diffrn_reflns_limit_l_min       -10
_diffrn_reflns_number            6726
_diffrn_reflns_theta_full        27.52
_diffrn_reflns_theta_max         27.52
_diffrn_standards_decay_%        0.92
_diffrn_standards_interval_count 150
_diffrn_standards_number         3
_exptl_absorpt_coefficient_mu    0.630
_exptl_absorpt_correction_T_max  0.999
_exptl_absorpt_correction_T_min  0.802
_exptl_absorpt_correction_type   psi-scan
_exptl_absorpt_process_details   '(North, Phillips & Mathews, 1968)'
_exptl_crystal_colour            brown
_exptl_crystal_density_diffrn    1.507
_exptl_crystal_density_meas      1.500
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prismatic
_exptl_crystal_F_000             652.00
_exptl_crystal_size_max          0.300
_exptl_crystal_size_mid          0.250
_exptl_crystal_size_min          0.230
_refine_diff_density_max         0.77
_refine_diff_density_min         -1.48
_refine_ls_extinction_coef       0.00000
_refine_ls_extinction_method     'Zachariasen(1967) type 2 Gaussian isotropic'
_refine_ls_goodness_of_fit_ref   1.947
_refine_ls_hydrogen_treatment    noref
_refine_ls_number_parameters     370
_refine_ls_number_reflns         6299
_refine_ls_R_factor_gt           0.0699
_refine_ls_shift/su_max          0.0007
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w = 1/[σ²(Fo²) + (0.05900(Max(Fo²,0) + 2Fc²)/3)²]'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_ref         0.2031
_reflns_number_gt                4408
_reflns_number_total             6299
_reflns_threshold_expression     F²>2.0σ(F²)
_cod_data_source_file            b111094m.txt
_cod_data_source_block           '[Mn(naphtmen)(H2O)]ClO4'
_cod_original_cell_volume        1381(1)
_cod_original_sg_symbol_H-M      'P -1         '
_cod_original_formula_sum        'C58 H64 Cl2 N4 Mn2 O16 '
_cod_database_code               7011380
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_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
Mn(1) Mn 0.04023(4) 0.13758(5) 0.10808(7) 0.0384(2) Uani 1.00 d . . .
Cl(1) Cl 0.80222(10) 0.3377(1) 0.4368(1) 0.0574(3) Uani 1.00 d . . .
O(1) O -0.0370(2) 0.0036(2) 0.1613(4) 0.0444(8) Uani 1.00 d . . .
O(2) O 0.1804(2) 0.1461(2) 0.1762(3) 0.0448(8) Uani 1.00 d . . .
O(3) O 0.0442(2) 0.2279(3) 0.3600(4) 0.0560(9) Uani 1.00 d . . .
O(4) O 0.2239(3) 0.4027(3) 0.5406(5) 0.080(1) Uani 1.00 d . . .
O(5) O 0.7017(7) 0.2646(7) 0.378(2) 0.332(6) Uani 1.00 d . . .
O(6) O 0.8036(8) 0.3842(7) 0.5911(7) 0.204(4) Uani 1.00 d . . .
O(7) O 0.8701(5) 0.2845(6) 0.4271(8) 0.146(3) Uani 1.00 d . . .
O(8) O 0.8154(7) 0.4100(6) 0.3381(8) 0.161(3) Uani 1.00 d . . .
N(1) N -0.0998(2) 0.1430(3) 0.0302(4) 0.0354(8) Uani 1.00 d . . .
N(2) N 0.1004(2) 0.2537(3) -0.0042(4) 0.0361(8) Uani 1.00 d . . .
C(1) C -0.1291(3) -0.0176(3) 0.2268(5) 0.0390(9) Uani 1.00 d . . .
C(2) C -0.1461(3) -0.0830(3) 0.3401(5) 0.044(1) Uani 1.00 d . . .
C(3) C -0.2433(3) -0.1187(3) 0.3961(5) 0.046(1) Uani 1.00 d . . .
C(4) C -0.3308(3) -0.0919(3) 0.3443(5) 0.0416(10) Uani 1.00 d . . .
C(5) C -0.4350(3) -0.1358(4) 0.3946(5) 0.052(1) Uani 1.00 d . . .
C(6) C -0.5177(3) -0.1082(4) 0.3475(6) 0.056(1) Uani 1.00 d . . .
C(7) C -0.5002(3) -0.0349(4) 0.2490(6) 0.055(1) Uani 1.00 d . . .
C(8) C -0.4007(3) 0.0090(4) 0.1962(6) 0.050(1) Uani 1.00 d . . .
C(9) C -0.3132(3) -0.0205(3) 0.2400(5) 0.0402(10) Uani 1.00 d . . .
C(10) C -0.2083(3) 0.0196(3) 0.1835(5) 0.0375(9) Uani 1.00 d . . .
C(11) C -0.1923(3) 0.0893(3) 0.0743(5) 0.0382(9) Uani 1.00 d . . .
C(12) C -0.0959(3) 0.2079(3) -0.0940(4) 0.0361(9) Uani 1.00 d . . .
C(13) C -0.1841(3) 0.2530(4) -0.0870(6) 0.049(1) Uani 1.00 d . . .
C(14) C -0.1169(3) 0.1298(4) -0.2616(5) 0.050(1) Uani 1.00 d . . .
C(15) C 0.0226(3) 0.3031(3) -0.0498(5) 0.0361(9) Uani 1.00 d . . .
C(16) C 0.0520(3) 0.3549(3) -0.1930(5) 0.046(1) Uani 1.00 d . . .
C(17) C 0.0337(3) 0.3909(3) 0.1016(5) 0.047(1) Uani 1.00 d . . .
C(18) C 0.2013(3) 0.2935(3) -0.0304(5) 0.0374(9) Uani 1.00 d . . .
C(19) C 0.2886(3) 0.2657(3) 0.0233(5) 0.0367(9) Uani 1.00 d . . .
C(20) C 0.3945(3) 0.3142(3) -0.0273(5) 0.0399(10) Uani 1.00 d . . .
C(21) C 0.4129(3) 0.3735(4) -0.1466(6) 0.048(1) Uani 1.00 d . . .
C(22) C 0.5158(4) 0.4161(4) -0.1908(6) 0.060(1) Uani 1.00 d . . .
C(23) C 0.6047(3) 0.4019(4) -0.1174(7) 0.062(1) Uani 1.00 d . . .
C(24) C 0.5895(3) 0.3444(4) -0.0025(6) 0.056(1) Uani 1.00 d . . .
C(25) C 0.4848(3) 0.2976(4) 0.0444(5) 0.046(1) Uani 1.00 d . . .
C(26) C 0.4674(3) 0.2314(4) 0.1574(5) 0.050(1) Uani 1.00 d . . .
C(27) C 0.3668(3) 0.1810(4) 0.1953(5) 0.048(1) Uani 1.00 d . . .
C(28) C 0.2745(3) 0.1972(3) 0.1288(5) 0.0382(9) Uani 1.00 d . . .
C(29) C 0.3172(5) 0.4399(6) 0.4696(8) 0.092(2) Uani 1.00 d . . .
H(1) H -0.0890 -0.1023 0.3767 0.0526 Uiso 1.00 calc . . .
H(2) H -0.2530 -0.1625 0.4720 0.0558 Uiso 1.00 calc . . .
H(3) H -0.4471 -0.1856 0.4619 0.0630 Uiso 1.00 calc . . .
H(4) H -0.5871 -0.1380 0.3818 0.0678 Uiso 1.00 calc . . .
H(5) H -0.5581 -0.0155 0.2169 0.0649 Uiso 1.00 calc . . .
H(6) H -0.3908 0.0594 0.1306 0.0593 Uiso 1.00 calc . . .
H(7) H -0.2554 0.0973 0.0302 0.0455 Uiso 1.00 calc . . .
H(8) H -0.1705 0.3022 0.0175 0.0594 Uiso 1.00 calc . . .
H(9) H -0.2549 0.1947 -0.1030 0.0594 Uiso 1.00 calc . . .
H(10) H -0.1817 0.2907 -0.1700 0.0594 Uiso 1.00 calc . . .
H(11) H -0.1875 0.0710 -0.2779 0.0598 Uiso 1.00 calc . . .
H(12) H -0.1150 0.1676 -0.3443 0.0598 Uiso 1.00 calc . . .
H(13) H -0.0618 0.1025 -0.2662 0.0598 Uiso 1.00 calc . . .
H(14) H 0.0040 0.3885 -0.2144 0.0551 Uiso 1.00 calc . . .
H(15) H 0.0443 0.3002 -0.2882 0.0551 Uiso 1.00 calc . . .
H(16) H 0.1262 0.4084 -0.1665 0.0551 Uiso 1.00 calc . . .
H(17) H -0.0145 0.4238 0.0791 0.0566 Uiso 1.00 calc . . .
H(18) H 0.1077 0.4445 0.1291 0.0566 Uiso 1.00 calc . . .
H(19) H 0.0150 0.3586 0.1902 0.0566 Uiso 1.00 calc . . .
H(20) H 0.2191 0.3472 -0.0911 0.0445 Uiso 1.00 calc . . .
H(21) H 0.3539 0.3848 -0.1985 0.0585 Uiso 1.00 calc . . .
H(22) H 0.5260 0.4556 -0.2725 0.0721 Uiso 1.00 calc . . .
H(23) H 0.6754 0.4326 -0.1478 0.0748 Uiso 1.00 calc . . .
H(24) H 0.6500 0.3350 0.0479 0.0675 Uiso 1.00 calc . . .
H(25) H 0.5283 0.2226 0.2075 0.0603 Uiso 1.00 calc . . .
H(26) H 0.3569 0.1341 0.2667 0.0566 Uiso 1.00 calc . . .
H(27) H 0.2979 0.4482 0.3647 0.1093 Uiso 1.00 calc . . .
H(28) H 0.3490 0.3879 0.4584 0.1093 Uiso 1.00 calc . . .
H(29) H 0.3701 0.5079 0.5369 0.1093 Uiso 1.00 calc . . .
H(30) H 0.1069 0.2505 0.4428 0.0668 Uiso 1.00 calc . . .
H(31) H -0.0166 0.2439 0.3854 0.0668 Uiso 1.00 calc . . .
H(32) H 0.2291 0.4286 0.6564 0.0950 Uiso 1.00 calc . . .
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.003 0.002
;International Tables for Crystallography
(1992, Vol. C, Tables 4.2.6.8 and 6.1.1.1)
;
H H 0.000 0.000
;International Tables for Crystallography
(1992, Vol. C, Table 6.1.1.2)
;
O O 0.011 0.006
;International Tables for Crystallography
(1992, Vol. C, Tables 4.2.6.8 and 6.1.1.1)
;
N N 0.006 0.003
;International Tables for Crystallography
(1992, Vol. C, Tables 4.2.6.8 and 6.1.1.1)
;
Cl Cl 0.148 0.159
;International Tables for Crystallography
(1992, Vol. C, Tables 4.2.6.8 and 6.1.1.1)
;
Mn Mn 0.337 0.728
;International Tables for Crystallography
(1992, Vol. C, Tables 4.2.6.8 and 6.1.1.1)
;
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_2
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
O(1) Mn(1) O(1) 79.4(1) . . 2_555 yes
O(1) Mn(1) O(2) 95.0(1) . . . yes
O(1) Mn(1) O(3) 89.9(1) . . . yes
O(1) Mn(1) N(1) 90.9(1) . . . yes
O(1) Mn(1) N(2) 165.2(1) . . . yes
O(1) Mn(1) O(2) 85.2(1) 2_555 . . yes
O(1) Mn(1) O(3) 167.46(10) 2_555 . . yes
O(1) Mn(1) N(1) 95.8(1) 2_555 . . yes
O(1) Mn(1) N(2) 88.1(1) 2_555 . . yes
O(2) Mn(1) O(3) 89.2(1) . . . yes
O(2) Mn(1) N(1) 174.1(1) . . . yes
O(2) Mn(1) N(2) 91.9(1) . . . yes
O(3) Mn(1) N(1) 90.8(1) . . . yes
O(3) Mn(1) N(2) 103.3(1) . . . yes
N(1) Mn(1) N(2) 82.3(1) . . . yes
O(5) Cl(1) O(6) 107.1(8) . . . yes
O(5) Cl(1) O(7) 107.4(6) . . . yes
O(5) Cl(1) O(8) 102.0(6) . . . yes
O(6) Cl(1) O(7) 111.5(4) . . . yes
O(6) Cl(1) O(8) 111.4(4) . . . yes
O(7) Cl(1) O(8) 116.5(4) . . . yes
Mn(1) O(1) Mn(1) 100.6(1) . . 2_555 yes
Mn(1) O(1) C(1) 122.9(2) . . . yes
Mn(1) O(1) C(1) 118.6(2) 2_555 . . yes
Mn(1) O(2) C(28) 129.5(2) . . . yes
Mn(1) N(1) C(11) 123.1(2) . . . yes
Mn(1) N(1) C(12) 116.0(2) . . . yes
C(11) N(1) C(12) 120.8(3) . . . yes
Mn(1) N(2) C(15) 115.0(2) . . . yes
Mn(1) N(2) C(18) 124.8(2) . . . yes
C(15) N(2) C(18) 120.0(3) . . . yes
O(1) C(1) C(2) 117.5(3) . . . yes
O(1) C(1) C(10) 122.4(3) . . . yes
C(2) C(1) C(10) 120.1(3) . . . yes
C(1) C(2) C(3) 120.6(3) . . . yes
C(2) C(3) C(4) 121.6(3) . . . yes
C(3) C(4) C(5) 121.2(3) . . . yes
C(3) C(4) C(9) 118.9(3) . . . yes
C(5) C(4) C(9) 119.9(4) . . . yes
C(4) C(5) C(6) 121.0(4) . . . yes
C(5) C(6) C(7) 119.6(4) . . . yes
C(6) C(7) C(8) 121.3(4) . . . yes
C(7) C(8) C(9) 120.4(4) . . . yes
C(4) C(9) C(8) 117.6(3) . . . yes
C(4) C(9) C(10) 119.3(3) . . . yes
C(8) C(9) C(10) 123.1(3) . . . yes
C(1) C(10) C(9) 119.1(3) . . . yes
C(1) C(10) C(11) 121.8(3) . . . yes
C(9) C(10) C(11) 118.9(3) . . . yes
N(1) C(11) C(10) 126.3(3) . . . yes
N(1) C(12) C(13) 111.8(3) . . . yes
N(1) C(12) C(14) 106.4(3) . . . yes
N(1) C(12) C(15) 105.3(3) . . . yes
C(13) C(12) C(14) 109.6(3) . . . yes
C(13) C(12) C(15) 110.7(3) . . . yes
C(14) C(12) C(15) 113.0(3) . . . yes
N(2) C(15) C(12) 106.2(3) . . . yes
N(2) C(15) C(16) 112.0(3) . . . yes
N(2) C(15) C(17) 106.3(3) . . . yes
C(12) C(15) C(16) 111.3(3) . . . yes
C(12) C(15) C(17) 111.7(3) . . . yes
C(16) C(15) C(17) 109.3(3) . . . yes
N(2) C(18) C(19) 126.9(3) . . . yes
C(18) C(19) C(20) 118.8(3) . . . yes
C(18) C(19) C(28) 121.0(3) . . . yes
C(20) C(19) C(28) 120.1(3) . . . yes
C(19) C(20) C(21) 124.1(3) . . . yes
C(19) C(20) C(25) 118.2(3) . . . yes
C(21) C(20) C(25) 117.6(3) . . . yes
C(20) C(21) C(22) 121.0(4) . . . yes
C(21) C(22) C(23) 121.1(4) . . . yes
C(22) C(23) C(24) 119.4(4) . . . yes
C(23) C(24) C(25) 121.3(4) . . . yes
C(20) C(25) C(24) 119.5(4) . . . yes
C(20) C(25) C(26) 119.4(3) . . . yes
C(24) C(25) C(26) 121.2(4) . . . yes
C(25) C(26) C(27) 121.8(3) . . . yes
C(26) C(27) C(28) 120.7(4) . . . yes
O(2) C(28) C(19) 124.4(3) . . . yes
O(2) C(28) C(27) 115.9(3) . . . yes
C(19) C(28) C(27) 119.6(3) . . . yes
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_1
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Mn(1) O(1) 1.896(3) . . yes
Mn(1) O(1) 2.662(3) . 2_555 yes
Mn(1) O(2) 1.867(3) . . yes
Mn(1) O(3) 2.224(3) . . yes
Mn(1) N(1) 1.969(3) . . yes
Mn(1) N(2) 1.959(3) . . yes
Cl(1) O(5) 1.306(7) . . yes
Cl(1) O(6) 1.327(6) . . yes
Cl(1) O(7) 1.367(4) . . yes
Cl(1) O(8) 1.393(5) . . yes
O(1) C(1) 1.342(4) . . yes
O(2) C(28) 1.319(4) . . yes
O(4) C(29) 1.387(7) . . yes
N(1) C(11) 1.299(4) . . yes
N(1) C(12) 1.503(4) . . yes
N(2) C(15) 1.513(4) . . yes
N(2) C(18) 1.299(4) . . yes
C(1) C(2) 1.417(5) . . yes
C(1) C(10) 1.398(5) . . yes
C(2) C(3) 1.359(5) . . yes
C(3) C(4) 1.420(6) . . yes
C(4) C(5) 1.423(5) . . yes
C(4) C(9) 1.416(5) . . yes
C(5) C(6) 1.360(6) . . yes
C(6) C(7) 1.398(6) . . yes
C(7) C(8) 1.382(5) . . yes
C(8) C(9) 1.425(5) . . yes
C(9) C(10) 1.452(4) . . yes
C(10) C(11) 1.432(5) . . yes
C(12) C(13) 1.532(5) . . yes
C(12) C(14) 1.526(6) . . yes
C(12) C(15) 1.566(5) . . yes
C(15) C(16) 1.530(5) . . yes
C(15) C(17) 1.524(6) . . yes
C(18) C(19) 1.431(4) . . yes
C(19) C(20) 1.451(5) . . yes
C(19) C(28) 1.397(5) . . yes
C(20) C(21) 1.401(5) . . yes
C(20) C(25) 1.426(5) . . yes
C(21) C(22) 1.384(5) . . yes
C(22) C(23) 1.396(6) . . yes
C(23) C(24) 1.353(7) . . yes
C(24) C(25) 1.420(5) . . yes
C(25) C(26) 1.423(6) . . yes
C(26) C(27) 1.350(6) . . yes
C(27) C(28) 1.429(5) . . yes
loop_
_geom_contact_atom_site_label_1
_geom_contact_atom_site_label_2
_geom_contact_distance
_geom_contact_site_symmetry_1
_geom_contact_site_symmetry_2
_geom_contact_publ_flag
Mn(1) O(1) 2.662(3) . 2_555 ?
O(3) O(4) 2.705(5) . . ?
O(3) O(7) 2.789(6) . 1_455 ?
O(3) C(29) 3.571(8) . . ?
O(4) O(8) 2.834(7) . 2_666 ?
O(4) C(16) 3.320(6) . 1_556 ?
O(4) O(6) 3.475(8) . 2_666 ?
O(5) C(8) 3.21(1) . 1_655 ?
O(5) C(26) 3.333(8) . . ?
O(6) C(17) 3.416(10) . 2_666 ?
O(6) C(29) 3.485(10) . 2_666 ?
O(6) C(13) 3.588(7) . 1_656 ?
O(7) C(11) 3.379(8) . 1_655 ?
O(7) C(10) 3.501(8) . 1_655 ?
O(7) C(16) 3.587(8) . 1_656 ?
O(8) C(29) 3.462(9) . 2_666 ?
O(8) C(16) 3.550(7) . 2_665 ?
C(6) C(6) 3.37(1) . 2_456 ?
C(6) C(7) 3.516(7) . 2_456 ?
C(20) C(22) 3.466(7) . 2_665 ?
C(21) C(22) 3.392(7) . 2_665 ?
C(21) C(23) 3.526(7) . 2_665 ?
