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#$Date: 2016-03-23 14:48:36 +0200 (Wed, 23 Mar 2016) $
#$Revision: 179307 $
#$URL: svn://www.crystallography.net/cod/cif/4/32/04/4320435.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_4320435
loop_
_publ_author_name
'Tosha M. Barclay'
'Robin G. Hicks'
'Martin T. Lemaire'
'Laurence K. Thompson'
_publ_contact_author             'Prof. Robin G. Hicks'
_publ_contact_author_email       rhicks@uvic.ca
_publ_section_title
;
 Synthesis, Structure, and Magnetism of Bimetallic Manganese or Nickel
 Complexes of a Bridging Verdazyl Radical
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              5581
_journal_page_last               5584
_journal_paper_doi               10.1021/ic010542x
_journal_volume                  40
_journal_year                    2001
_chemical_formula_sum            'C30 H17 F24 Mn2 N6 O9'
_chemical_formula_weight         1171.38
_chemical_melting_point          483
_chemical_name_systematic
;
mu-1,5-dimethyl-3-(4,6-dimethyl-2-pyrimidinyl)-6-oxoverdazyl-
bis(bis(1,1,1,3,3,3-hexafluoroacetylacetonato)manganese(II))
;
_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                 123.748(3)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   20.047(3)
_cell_length_b                   17.143(3)
_cell_length_c                   16.276(3)
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      50
_cell_measurement_theta_min      4
_cell_volume                     4650.9(14)
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 0.992
_diffrn_measured_fraction_theta_max 0.992
_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  0.0228
_diffrn_reflns_av_sigmaI/netI    0.0255
_diffrn_reflns_limit_h_max       23
_diffrn_reflns_limit_h_min       -23
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_l_max       11
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            12256
_diffrn_reflns_theta_full        25.10
_diffrn_reflns_theta_max         25.10
_diffrn_reflns_theta_min         1.70
_exptl_absorpt_coefficient_mu    0.692
_exptl_crystal_density_diffrn    1.673
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             2308
_refine_diff_density_max         0.475
_refine_diff_density_min         -0.315
_refine_diff_density_rms         0.060
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.031
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     323
_refine_ls_number_reflns         4125
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.031
_refine_ls_R_factor_all          0.1042
_refine_ls_R_factor_gt           0.0673
_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)+(0.1592P)²+1.0310P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2166
_refine_ls_wR_factor_ref         0.2557
_reflns_number_gt                2341
_reflns_number_total             4125
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic010542x.cif
_cod_data_source_block           rhmag31a
_cod_original_cell_volume        4650.7(13)
_cod_database_code               4320435
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
_atom_site_disorder_assembly
_atom_site_disorder_group
Mn1 Mn 0.12080(4) 0.24307(4) 0.69697(6) 0.0933(4) Uani 1 1 d . . .
N1 N 0.0491(2) 0.3241(2) 0.7314(3) 0.0859(11) Uani 1 1 d . . .
N2 N 0.0243(2) 0.1694(2) 0.6990(3) 0.0887(11) Uani 1 1 d . . .
N3 N 0.0208(3) 0.0901(2) 0.6969(4) 0.1049(14) Uani 1 1 d . . .
O1 O 0.1561(3) 0.1647(3) 0.6267(3) 0.1286(15) Uani 1 1 d . . .
O2 O 0.0615(2) 0.2990(2) 0.5583(3) 0.1174(13) Uani 1 1 d . . .
O3 O 0.2283(3) 0.3073(2) 0.7604(4) 0.1468(18) Uani 1 1 d . . .
O4 O 0.1903(2) 0.1786(2) 0.8311(3) 0.1128(12) Uani 1 1 d . . .
O5 O 0.0000 -0.0226(3) 0.7500 0.162(3) Uani 1 2 d S . .
C1 C 0.0000 0.4427(4) 0.7500 0.103(2) Uani 1 2 d S . .
H1A H 0.0000 0.4970 0.7500 0.124 Uiso 1 2 calc SR . .
C2 C 0.0499(3) 0.4036(3) 0.7320(4) 0.0940(15) Uani 1 1 d . . .
C3 C 0.1059(4) 0.4451(3) 0.7143(5) 0.133(2) Uani 1 1 d . . .
H3A H 0.1001 0.5004 0.7177 0.200 Uiso 1 1 calc R . .
H3B H 0.0936 0.4317 0.6500 0.200 Uiso 1 1 calc R . .
H3C H 0.1600 0.4300 0.7636 0.200 Uiso 1 1 calc R . .
C4 C 0.0000 0.2895(3) 0.7500 0.0751(16) Uani 1 2 d S . .
C5 C 0.0000 0.2029(3) 0.7500 0.0755(16) Uani 1 2 d S . .
C6 C 0.0000 0.0459(4) 0.7500 0.106(2) Uani 1 2 d S . .
C7 C 0.0427(6) 0.0496(4) 0.6361(8) 0.180(4) Uani 1 1 d . . .
H7A H 0.0553 0.0872 0.6030 0.271 Uiso 1 1 calc R . .
H7B H -0.0015 0.0179 0.5881 0.271 Uiso 1 1 calc R . .
H7C H 0.0886 0.0171 0.6774 0.271 Uiso 1 1 calc R . .
C11 C 0.1569(4) 0.1759(4) 0.5538(6) 0.127(2) Uani 1 1 d . . .
C12 C 0.1212(5) 0.2358(5) 0.4860(6) 0.142(3) Uani 1 1 d . . .
H12A H 0.1264 0.2374 0.4327 0.170 Uiso 1 1 calc R . .
C13 C 0.0780(4) 0.2933(4) 0.4957(5) 0.124(2) Uani 1 1 d . . .
C14 C 0.2009(12) 0.1155(9) 0.5335(14) 0.202(5) Uani 1 1 d . . .
C15 C 0.0407(8) 0.3595(7) 0.4171(8) 0.175(4) Uani 1 1 d . . .
C31 C 0.2964(4) 0.2891(4) 0.8268(6) 0.145(3) Uani 1 1 d . . .
C32 C 0.3193(4) 0.2297(4) 0.8936(6) 0.141(3) Uani 1 1 d . . .
H32A H 0.3734 0.2236 0.9428 0.169 Uiso 1 1 calc R . .
C33 C 0.2648(4) 0.1785(4) 0.8906(4) 0.1165(19) Uani 1 1 d . . .
C34 C 0.3633(8) 0.3441(9) 0.845(2) 0.297(12) Uani 1 1 d . . .
C35 C 0.2939(7) 0.1131(9) 0.9635(7) 0.193(4) Uani 1 1 d . . .
F1 F 0.2133(6) 0.1280(6) 0.4697(7) 0.304(5) Uani 1 1 d . . .
F2 F 0.1674(8) 0.0473(7) 0.5196(12) 0.330(6) Uani 1 1 d . . .
F3 F 0.2675(7) 0.0982(9) 0.6089(8) 0.341(8) Uani 1 1 d . . .
F4 F 0.0628(7) 0.4269(5) 0.4604(6) 0.348(7) Uani 1 1 d . . .
F5 F 0.0641(5) 0.3646(6) 0.3633(6) 0.280(5) Uani 1 1 d . . .
F6 F -0.0335(4) 0.3560(5) 0.3666(5) 0.261(4) Uani 1 1 d . . .
F7 F 0.3626(10) 0.3425(14) 0.7632(13) 0.470(16) Uani 1 1 d . . .
F8 F 0.3427(6) 0.4140(5) 0.8448(14) 0.374(9) Uani 1 1 d . . .
F9 F 0.4287(4) 0.3347(5) 0.9055(9) 0.318(6) Uani 1 1 d . . .
F10 F 0.3695(5) 0.1052(5) 1.0183(7) 0.297(5) Uani 1 1 d . . .
F11 F 0.2761(9) 0.1228(9) 1.0244(9) 0.369(8) Uani 1 1 d . . .
F12 F 0.2662(7) 0.0485(4) 0.9263(7) 0.319(6) 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'
F F 0.0171 0.0103 '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 95.84(17) . . ?
O2 Mn1 O1 82.53(18) . . ?
O3 Mn1 O1 92.2(2) . . ?
O2 Mn1 O4 172.16(18) . . ?
O3 Mn1 O4 82.01(15) . . ?
O1 Mn1 O4 90.01(16) . . ?
O2 Mn1 N1 85.90(16) . . ?
O3 Mn1 N1 100.04(18) . . ?
O1 Mn1 N1 163.95(16) . . ?
O4 Mn1 N1 101.88(15) . . ?
O2 Mn1 N2 106.45(16) . . ?
O3 Mn1 N2 155.26(19) . . ?
O1 Mn1 N2 101.09(16) . . ?
O4 Mn1 N2 77.25(14) . . ?
N1 Mn1 N2 71.60(14) . . ?
C4 N1 C2 117.0(5) . . ?
C4 N1 Mn1 115.8(3) . . ?
C2 N1 Mn1 127.2(4) . . ?
C5 N2 N3 115.0(4) . . ?
C5 N2 Mn1 112.2(3) . . ?
N3 N2 Mn1 125.0(3) . . ?
N2 N3 C6 124.3(5) . . ?
N2 N3 C7 117.4(5) . . ?
C6 N3 C7 118.3(5) . . ?
C11 O1 Mn1 128.1(4) . . ?
C13 O2 Mn1 126.6(4) . . ?
C31 O3 Mn1 129.5(4) . . ?
C33 O4 Mn1 127.9(4) . . ?
C2 C1 C2 121.0(6) 2_556 . ?
N1 C2 C1 119.2(5) . . ?
N1 C2 C3 119.0(5) . . ?
C1 C2 C3 121.9(4) . . ?
N1 C4 N1 126.7(5) 2_556 . ?
N1 C4 C5 116.7(3) 2_556 . ?
N1 C4 C5 116.7(3) . . ?
N2 C5 N2 127.8(6) 2_556 . ?
N2 C5 C4 116.1(3) 2_556 . ?
N2 C5 C4 116.1(3) . . ?
O5 C6 N3 123.4(3) . 2_556 ?
O5 C6 N3 123.4(3) . . ?
N3 C6 N3 113.3(6) 2_556 . ?
O1 C11 C12 128.1(7) . . ?
O1 C11 C14 115.7(8) . . ?
C12 C11 C14 116.2(8) . . ?
C13 C12 C11 121.3(7) . . ?
O2 C13 C12 128.5(6) . . ?
O2 C13 C15 113.2(8) . . ?
C12 C13 C15 118.2(8) . . ?
F1 C14 F3 105.6(15) . . ?
F1 C14 F2 109.9(17) . . ?
F3 C14 F2 97.1(12) . . ?
F1 C14 C11 119.3(11) . . ?
F3 C14 C11 112.5(15) . . ?
F2 C14 C11 110.1(12) . . ?
F5 C15 F6 109.3(10) . . ?
F5 C15 F4 100.1(12) . . ?
F6 C15 F4 109.1(12) . . ?
F5 C15 C13 116.6(11) . . ?
F6 C15 C13 111.3(10) . . ?
F4 C15 C13 109.9(9) . . ?
O3 C31 C32 127.5(6) . . ?
O3 C31 C34 116.4(8) . . ?
C32 C31 C34 115.8(9) . . ?
C31 C32 C33 122.4(6) . . ?
O4 C33 C32 127.4(5) . . ?
O4 C33 C35 112.8(7) . . ?
C32 C33 C35 119.7(7) . . ?
F9 C34 F8 111(2) . . ?
F9 C34 F7 103(2) . . ?
F8 C34 F7 101.3(15) . . ?
F9 C34 C31 123.3(12) . . ?
F8 C34 C31 109.4(14) . . ?
F7 C34 C31 106(2) . . ?
F12 C35 F11 105.2(15) . . ?
F12 C35 F10 106.6(13) . . ?
F11 C35 F10 102.4(9) . . ?
F12 C35 C33 114.3(8) . . ?
F11 C35 C33 112.0(12) . . ?
F10 C35 C33 115.1(11) . . ?
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 2.108(4) . ?
Mn1 O3 2.110(4) . ?
Mn1 O1 2.124(5) . ?
Mn1 O4 2.133(3) . ?
Mn1 N1 2.281(4) . ?
Mn1 N2 2.326(4) . ?
N1 C4 1.321(5) . ?
N1 C2 1.363(6) . ?
N2 C5 1.305(5) . ?
N2 N3 1.361(5) . ?
N3 C6 1.376(6) . ?
N3 C7 1.460(8) . ?
O1 C11 1.212(7) . ?
O2 C13 1.238(8) . ?
O3 C31 1.220(7) . ?
O4 C33 1.250(7) . ?
O5 C6 1.175(8) . ?
C1 C2 1.365(6) 2_556 ?
C1 C2 1.365(6) . ?
C2 C3 1.486(8) . ?
C4 N1 1.321(5) 2_556 ?
C4 C5 1.485(8) . ?
C5 N2 1.305(5) 2_556 ?
C6 N3 1.376(6) 2_556 ?
C11 C12 1.382(9) . ?
C11 C14 1.510(13) . ?
C12 C13 1.379(10) . ?
C13 C15 1.556(10) . ?
C14 F1 1.213(11) . ?
C14 F3 1.247(17) . ?
C14 F2 1.305(16) . ?
C15 F5 1.204(12) . ?
C15 F6 1.238(13) . ?
C15 F4 1.297(12) . ?
C31 C32 1.371(10) . ?
C31 C34 1.527(13) . ?
C32 C33 1.381(9) . ?
C33 C35 1.495(11) . ?
C34 F9 1.132(15) . ?
C34 F8 1.267(19) . ?
C34 F7 1.32(3) . ?
C35 F12 1.235(13) . ?
C35 F11 1.238(14) . ?
C35 F10 1.267(13) . ?
