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#$Date: 2016-03-22 11:11:11 +0200 (Tue, 22 Mar 2016) $
#$Revision: 178888 $
#$URL: svn://www.crystallography.net/cod/cif/4/11/17/4111751.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_4111751
loop_
_publ_author_name
'Jianfang Chai'
'Hongping Zhu'
'A. Claudia Stückl'
'Herbert W. Roesky'
'Jörg Magull'
'Alessandro Bencini'
'Andrea Caneschi'
'Dante Gatteschi'
_publ_section_title
;
 Synthesis and Reaction of [{HC(CMeNAr)2}Mn]2 (Ar = 2,6-iPr2C6H3): The
 Complex Containing Three-Coordinate Manganese(I) with a Mn-Mn Bond
 Exhibiting Unusual Magnetic Properties and Electronic Structure
;
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              9201
_journal_page_last               9206
_journal_paper_doi               10.1021/ja042269e
_journal_volume                  127
_journal_year                    2005
_chemical_formula_sum            'C58 H82 Mn2 N4 O2'
_chemical_formula_weight         977.16
_chemical_name_systematic
;
?
;
_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                 90.802(6)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   15.4921(12)
_cell_length_b                   16.3958(9)
_cell_length_c                   21.3688(17)
_cell_measurement_temperature    133(2)
_cell_volume                     5427.3(7)
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      133(2)
_diffrn_measured_fraction_theta_full 0.993
_diffrn_measured_fraction_theta_max 0.993
_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  0.0637
_diffrn_reflns_av_sigmaI/netI    0.0447
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -18
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       25
_diffrn_reflns_limit_l_min       -25
_diffrn_reflns_number            18243
_diffrn_reflns_theta_full        24.77
_diffrn_reflns_theta_max         24.77
_diffrn_reflns_theta_min         1.81
_exptl_absorpt_coefficient_mu    0.509
_exptl_absorpt_correction_type   none
_exptl_crystal_density_diffrn    1.196
_exptl_crystal_density_method    none
_exptl_crystal_F_000             2096
_refine_diff_density_max         0.325
_refine_diff_density_min         -0.257
_refine_diff_density_rms         0.049
_refine_ls_extinction_coef       none
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.024
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     308
_refine_ls_number_reflns         4641
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.024
_refine_ls_R_factor_all          0.0664
_refine_ls_R_factor_gt           0.0421
_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)+(0.0396P)²+6.7507P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0873
_refine_ls_wR_factor_ref         0.0962
_reflns_number_gt                3473
_reflns_number_total             4641
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja042269esi20050426_115054.cif
_cod_data_source_block           compound3
_cod_database_code               4111751
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_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
Mn1 Mn 0.05872(2) 0.24958(2) 0.295956(15) 0.01844(11) Uani 1 1 d .
N1 N 0.06562(13) 0.30042(12) 0.38164(9) 0.0198(4) Uani 1 1 d .
N2 N 0.17924(13) 0.20552(12) 0.30696(9) 0.0212(4) Uani 1 1 d .
O1 O -0.05780(10) 0.24786(12) 0.28954(7) 0.0251(4) Uani 1 1 d .
C1 C 0.13860(18) 0.37409(17) 0.46833(13) 0.0312(6) Uani 1 1 d .
H1A H 0.1972 0.3787 0.4859 0.047 Uiso 1 1 calc R
H1B H 0.1004 0.3503 0.4996 0.047 Uiso 1 1 calc R
H1C H 0.1174 0.4284 0.4566 0.047 Uiso 1 1 calc R
C2 C 0.13989(17) 0.31996(15) 0.41107(11) 0.0233(5) Uani 1 1 d .
C3 C 0.22042(17) 0.29230(16) 0.39266(12) 0.0249(6) Uani 1 1 d .
H3A H 0.2690 0.3165 0.4130 0.030 Uiso 1 1 calc R
C4 C 0.23844(17) 0.23259(14) 0.34729(11) 0.0228(6) Uani 1 1 d .
C5 C 0.32908(18) 0.19913(18) 0.34814(13) 0.0331(6) Uani 1 1 d .
H5A H 0.3303 0.1474 0.3253 0.050 Uiso 1 1 calc R
H5B H 0.3480 0.1901 0.3915 0.050 Uiso 1 1 calc R
H5C H 0.3679 0.2382 0.3282 0.050 Uiso 1 1 calc R
C6 C -0.01263(16) 0.32108(15) 0.41463(11) 0.0208(5) Uani 1 1 d .
C7 C -0.04586(17) 0.26500(16) 0.45768(11) 0.0271(6) Uani 1 1 d .
C8 C -0.11601(19) 0.28805(18) 0.49340(12) 0.0334(6) Uani 1 1 d .
H8A H -0.1390 0.2506 0.5227 0.040 Uiso 1 1 calc R
C9 C -0.15297(19) 0.36427(18) 0.48717(12) 0.0338(7) Uani 1 1 d .
H9A H -0.1993 0.3800 0.5133 0.041 Uiso 1 1 calc R
C10 C -0.12207(18) 0.41731(17) 0.44276(12) 0.0292(6) Uani 1 1 d .
H10A H -0.1490 0.4690 0.4377 0.035 Uiso 1 1 calc R
C11 C -0.05259(17) 0.39732(15) 0.40517(11) 0.0240(6) Uani 1 1 d .
C12 C -0.00855(19) 0.17950(16) 0.46482(13) 0.0320(6) Uani 1 1 d .
H12A H 0.0375 0.1732 0.4328 0.038 Uiso 1 1 calc R
C13 C -0.0755(3) 0.1146(2) 0.4521(2) 0.0732(13) Uani 1 1 d .
H13A H -0.0487 0.0606 0.4558 0.110 Uiso 1 1 calc R
H13B H -0.0993 0.1215 0.4097 0.110 Uiso 1 1 calc R
H13C H -0.1220 0.1194 0.4825 0.110 Uiso 1 1 calc R
C14 C 0.0338(3) 0.1674(2) 0.52905(19) 0.0748(14) Uani 1 1 d .
H14A H 0.0595 0.1128 0.5314 0.112 Uiso 1 1 calc R
H14B H -0.0098 0.1730 0.5616 0.112 Uiso 1 1 calc R
H14C H 0.0789 0.2086 0.5355 0.112 Uiso 1 1 calc R
C15 C -0.02415(18) 0.45591(16) 0.35437(13) 0.0288(6) Uani 1 1 d .
H15A H 0.0286 0.4329 0.3345 0.035 Uiso 1 1 calc R
C16 C -0.0014(2) 0.54024(18) 0.38062(16) 0.0419(7) Uani 1 1 d .
H16A H 0.0461 0.5351 0.4111 0.063 Uiso 1 1 calc R
H16B H -0.0520 0.5634 0.4012 0.063 Uiso 1 1 calc R
H16C H 0.0161 0.5761 0.3464 0.063 Uiso 1 1 calc R
C17 C -0.0947(2) 0.46336(17) 0.30382(13) 0.0342(7) Uani 1 1 d .
H17A H -0.1073 0.4093 0.2863 0.051 Uiso 1 1 calc R
H17B H -0.0750 0.4996 0.2705 0.051 Uiso 1 1 calc R
H17C H -0.1471 0.4859 0.3223 0.051 Uiso 1 1 calc R
C18 C 0.19994(17) 0.13813(15) 0.26590(12) 0.0238(5) Uani 1 1 d .
C19 C 0.25099(18) 0.15063(16) 0.21284(12) 0.0273(6) Uani 1 1 d .
C20 C 0.26618(19) 0.08370(17) 0.17411(13) 0.0337(7) Uani 1 1 d .
H20A H 0.3001 0.0907 0.1378 0.040 Uiso 1 1 calc R
C21 C 0.2331(2) 0.00786(18) 0.18727(14) 0.0392(7) Uani 1 1 d .
H21A H 0.2445 -0.0368 0.1603 0.047 Uiso 1 1 calc R
C22 C 0.1831(2) -0.00329(17) 0.24005(15) 0.0371(7) Uani 1 1 d .
H22A H 0.1606 -0.0559 0.2488 0.045 Uiso 1 1 calc R
C23 C 0.16545(18) 0.06114(16) 0.28029(13) 0.0289(6) Uani 1 1 d .
C24 C 0.28913(19) 0.23331(16) 0.19669(13) 0.0323(7) Uani 1 1 d .
H24A H 0.2784 0.2710 0.2325 0.039 Uiso 1 1 calc R
C25 C 0.3880(2) 0.22910(18) 0.18679(15) 0.0396(7) Uani 1 1 d .
H25A H 0.4153 0.2005 0.2221 0.059 Uiso 1 1 calc R
H25B H 0.4114 0.2845 0.1840 0.059 Uiso 1 1 calc R
H25C H 0.3998 0.1996 0.1479 0.059 Uiso 1 1 calc R
C26 C 0.2448(2) 0.26898(19) 0.13864(14) 0.0417(8) Uani 1 1 d .
H26A H 0.1828 0.2742 0.1461 0.063 Uiso 1 1 calc R
H26B H 0.2540 0.2328 0.1029 0.063 Uiso 1 1 calc R
H26C H 0.2691 0.3228 0.1297 0.063 Uiso 1 1 calc R
C27 C 0.11191(19) 0.04814(17) 0.33911(13) 0.0340(7) Uani 1 1 d .
H27A H 0.0784 0.0994 0.3460 0.041 Uiso 1 1 calc R
C28 C 0.1696(3) 0.0362(3) 0.39622(16) 0.0611(10) Uani 1 1 d .
H28A H 0.1339 0.0300 0.4334 0.092 Uiso 1 1 calc R
H28B H 0.2075 0.0836 0.4014 0.092 Uiso 1 1 calc R
H28C H 0.2048 -0.0129 0.3908 0.092 Uiso 1 1 calc R
C29 C 0.0471(3) -0.0210(3) 0.3346(2) 0.0816(14) Uani 1 1 d .
H29A H 0.0117 -0.0216 0.3722 0.122 Uiso 1 1 calc R
H29B H 0.0778 -0.0730 0.3309 0.122 Uiso 1 1 calc R
H29C H 0.0098 -0.0130 0.2976 0.122 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'
O O 0.0106 0.0060 '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 O1 85.99(7) . 2
O1 Mn1 N2 157.90(9) . .
O1 Mn1 N2 96.06(8) 2 .
O1 Mn1 N1 96.64(8) . .
O1 Mn1 N1 156.26(8) 2 .
N2 Mn1 N1 90.28(8) . .
O1 Mn1 Mn1 43.28(5) . 2
O1 Mn1 Mn1 42.74(5) 2 2
N2 Mn1 Mn1 135.28(6) . 2
N1 Mn1 Mn1 134.34(6) . 2
C2 N1 C6 115.7(2) . .
C2 N1 Mn1 124.00(17) . .
C6 N1 Mn1 120.29(15) . .
C4 N2 C18 119.4(2) . .
C4 N2 Mn1 126.01(17) . .
C18 N2 Mn1 114.55(16) . .
Mn1 O1 Mn1 93.98(7) . 2
N1 C2 C3 123.8(2) . .
N1 C2 C1 119.9(2) . .
C3 C2 C1 116.3(2) . .
C2 C3 C4 127.5(2) . .
N2 C4 C3 122.5(2) . .
N2 C4 C5 121.5(2) . .
C3 C4 C5 116.0(2) . .
C7 C6 C11 120.7(2) . .
C7 C6 N1 118.8(2) . .
C11 C6 N1 120.4(2) . .
C8 C7 C6 118.6(2) . .
C8 C7 C12 119.6(2) . .
C6 C7 C12 121.8(2) . .
C9 C8 C7 121.3(3) . .
C10 C9 C8 119.3(3) . .
C9 C10 C11 121.9(3) . .
C10 C11 C6 117.9(2) . .
C10 C11 C15 119.9(2) . .
C6 C11 C15 122.2(2) . .
C13 C12 C7 111.9(3) . .
C13 C12 C14 110.9(3) . .
C7 C12 C14 111.6(2) . .
C11 C15 C17 110.1(2) . .
C11 C15 C16 112.1(2) . .
C17 C15 C16 110.2(2) . .
C23 C18 C19 121.8(2) . .
C23 C18 N2 117.6(2) . .
C19 C18 N2 120.6(2) . .
C20 C19 C18 117.7(3) . .
C20 C19 C24 119.8(2) . .
C18 C19 C24 122.5(2) . .
C21 C20 C19 121.5(3) . .
C20 C21 C22 119.9(3) . .
C21 C22 C23 121.2(3) . .
C22 C23 C18 117.9(3) . .
C22 C23 C27 121.0(2) . .
C18 C23 C27 121.1(2) . .
C19 C24 C26 110.7(2) . .
C19 C24 C25 112.3(2) . .
C26 C24 C25 109.9(2) . .
C28 C27 C29 109.7(3) . .
C28 C27 C23 111.0(3) . .
C29 C27 C23 114.7(3) . .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
Mn1 O1 1.8087(16) .
Mn1 O1 1.8269(16) 2
Mn1 N2 2.013(2) .
Mn1 N1 2.013(2) .
Mn1 Mn1 2.6585(7) 2
N1 C2 1.342(3) .
N1 C6 1.451(3) .
N2 C4 1.326(3) .
N2 C18 1.450(3) .
O1 Mn1 1.8269(16) 2
C1 C2 1.512(4) .
C2 C3 1.390(4) .
C3 C4 1.409(4) .
C4 C5 1.508(4) .
C6 C7 1.404(3) .
C6 C11 1.408(4) .
C7 C8 1.389(4) .
C7 C12 1.523(4) .
C8 C9 1.380(4) .
C9 C10 1.378(4) .
C10 C11 1.391(4) .
C11 C15 1.519(4) .
C12 C13 1.508(5) .
C12 C14 1.526(4) .
C15 C17 1.531(4) .
C15 C16 1.531(4) .
C18 C23 1.407(4) .
C18 C19 1.407(4) .
C19 C20 1.397(4) .
C19 C24 1.520(4) .
C20 C21 1.375(4) .
C21 C22 1.389(4) .
C22 C23 1.392(4) .
C23 C27 1.530(4) .
C24 C26 1.526(4) .
C24 C25 1.551(4) .
C27 C28 1.516(5) .
C27 C29 1.517(5) .
