#------------------------------------------------------------------------------
#$Date: 2016-03-23 00:06:12 +0200 (Wed, 23 Mar 2016) $
#$Revision: 179093 $
#$URL: svn://www.crystallography.net/cod/cif/4/30/55/4305568.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_4305568
loop_
_publ_author_name
'Christelle Hureau'
'Sihem Groni'
'Régis Guillot'
'Geneviève Blondin'
'Carole Duboc'
'Elodie Anxolabéhère-Mallart'
_publ_contact_author_address
;
"Institut de Chimie Moléculaire et des Matériaux d'Orsay,
 Univ Paris-Sud, UMR 8182 CNRS, Orsay, F- 91405"
;
_publ_contact_author_email       eanxolab@icmo.u-psud.fr
_publ_contact_author_name        'Elodie Anxolabéhère-Mallart'
_publ_contact_author_phone       '33 1 69 15 76 40'
_publ_section_title
;
Syntheses, X-ray Structures, Solid State High-Field Electron Paramagnetic
Resonance, and Density-Functional Theory Investigations on Chloro and Aqua
MnII Mononuclear Complexes with Amino-Pyridine Pentadentate Ligands
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              9238
_journal_page_last               9247
_journal_paper_doi               10.1021/ic800551u
_journal_volume                  47
_journal_year                    2008
_chemical_formula_moiety         'C21 H25 Cl Mn N5, F6 P '
_chemical_formula_sum            'C21 H25 Cl F6 Mn N5 P'
_chemical_formula_weight         582.82
_chemical_name_systematic
;
[N-methyl-N,N',N'-tris(2-pyridylmethylethane-1,2-diamine MnCl] (PF6) 
;
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_Int_Tables_number      14
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/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                 96.893(2)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   7.7305(4)
_cell_length_b                   17.8372(12)
_cell_length_c                   18.2266(12)
_cell_measurement_reflns_used    6041
_cell_measurement_temperature    273(2)
_cell_measurement_theta_max      28.60
_cell_measurement_theta_min      2.25
_cell_volume                     2495.1(3)
_computing_cell_refinement       'Bruker SMART'
_computing_data_collection       'Bruker SMART'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'Bruker SHELXTL'
_computing_structure_solution    'Bruker SHELXTL'
_diffrn_ambient_temperature      273(2)
_diffrn_measured_fraction_theta_full 0.802
_diffrn_measured_fraction_theta_max 0.802
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0182
_diffrn_reflns_av_sigmaI/netI    0.0255
_diffrn_reflns_limit_h_max       6
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -24
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_number            10559
_diffrn_reflns_theta_full        28.87
_diffrn_reflns_theta_max         28.87
_diffrn_reflns_theta_min         1.60
_diffrn_source                   'fine-focus sealed tube'
_exptl_absorpt_coefficient_mu    0.764
_exptl_absorpt_correction_T_max  0.94
_exptl_absorpt_correction_T_min  0.89
_exptl_absorpt_correction_type   psi-scan
_exptl_absorpt_process_details   SADABS
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.517
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             1188
_exptl_crystal_size_max          0.150
_exptl_crystal_size_mid          0.120
_exptl_crystal_size_min          0.080
_refine_diff_density_max         1.172
_refine_diff_density_min         -0.683
_refine_diff_density_rms         0.098
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.027
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     316
_refine_ls_number_reflns         5267
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.027
_refine_ls_R_factor_all          0.0696
_refine_ls_R_factor_gt           0.0554
_refine_ls_shift/su_max          0.062
_refine_ls_shift/su_mean         0.003
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[σ²(Fo²)+(0.0960P)²+3.2575P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1578
_refine_ls_wR_factor_ref         0.1722
_reflns_number_gt                4220
_reflns_number_total             5267
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic800551u_si_002_2.cif
_cod_data_source_block           149GuillotICMMO
_cod_original_sg_symbol_H-M      'P 21/c'
_cod_database_code               4305568
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, y+1/2, -z+1/2'
'-x, -y, -z'
'x, -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
F6 F -0.5233(5) -0.10290(18) -0.2134(2) 0.1164(14) Uani 1 1 d . . .
F5 F -0.4347(6) 0.06189(17) -0.1610(2) 0.1184(13) Uani 1 1 d . . .
C30 C 0.1654(6) 0.1666(2) -0.0077(2) 0.0561(10) Uani 1 1 d . . .
H30 H 0.2733 0.1898 -0.0068 0.067 Uiso 1 1 calc R . .
F4 F -0.6710(6) -0.0139(2) -0.1673(3) 0.1487(19) Uani 1 1 d . . .
C33 C -0.1493(7) 0.0990(3) -0.0114(2) 0.0729(13) Uani 1 1 d . . .
H33 H -0.2580 0.0765 -0.0120 0.087 Uiso 1 1 calc R . .
C31 C 0.1251(8) 0.1079(3) -0.0565(2) 0.0747(14) Uani 1 1 d . . .
H31 H 0.2047 0.0910 -0.0873 0.090 Uiso 1 1 calc R . .
F2 F -0.2933(6) -0.0286(2) -0.2034(5) 0.221(4) Uani 1 1 d . . .
F3 F -0.5338(11) 0.0124(3) -0.2629(2) 0.202(3) Uani 1 1 d . . .
F1 F -0.4365(9) -0.0497(3) -0.1079(3) 0.189(3) Uani 1 1 d . . .
C32 C -0.0369(9) 0.0753(3) -0.0581(3) 0.0858(16) Uani 1 1 d . . .
H32 H -0.0693 0.0368 -0.0914 0.103 Uiso 1 1 calc R . .
Cl1 Cl 0.34924(11) 0.34269(6) 0.06810(5) 0.0500(2) Uani 1 1 d . . .
C40 C 0.0119(6) 0.4051(3) 0.2421(2) 0.0650(12) Uani 1 1 d . . .
H40A H 0.0325 0.3631 0.2749 0.098 Uiso 1 1 calc R . .
H40B H -0.0642 0.4401 0.2622 0.098 Uiso 1 1 calc R . .
H40C H 0.1206 0.4292 0.2366 0.098 Uiso 1 1 calc R . .
Mn1 Mn 0.09229(6) 0.29342(3) 0.10941(2) 0.03387(17) Uani 1 1 d . . .
P3 P -0.47872(14) -0.02125(5) -0.18671(6) 0.0507(3) Uani 1 1 d . . .
N2 N -0.1119(4) 0.21697(16) 0.15672(16) 0.0425(6) Uani 1 1 d . . .
N6 N -0.0696(3) 0.37897(16) 0.16943(15) 0.0404(6) Uani 1 1 d . . .
N1 N 0.2181(4) 0.24987(16) 0.22042(15) 0.0411(6) Uani 1 1 d . . .
N3 N 0.0557(4) 0.19086(16) 0.03778(16) 0.0456(7) Uani 1 1 d . . .
C7 C -0.1011(5) 0.1567(2) 0.0369(2) 0.0506(9) Uani 1 1 d . . .
C4 C 0.1366(5) 0.19278(19) 0.24962(19) 0.0434(8) Uani 1 1 d . . .
C5 C -0.0143(5) 0.1586(2) 0.2009(2) 0.0513(9) Uani 1 1 d . . .
H5A H 0.0288 0.1218 0.1684 0.062 Uiso 1 1 calc R . .
H5B H -0.0909 0.1332 0.2313 0.062 Uiso 1 1 calc R . .
C21 C 0.3524(5) 0.2823(2) 0.2612(2) 0.0477(8) Uani 1 1 d . . .
H21 H 0.4085 0.3220 0.2409 0.057 Uiso 1 1 calc R . .
C14 C -0.1554(5) 0.4217(2) 0.0415(2) 0.0476(8) Uani 1 1 d . . .
C17 C -0.2157(5) 0.2625(2) 0.2035(2) 0.0528(9) Uani 1 1 d . . .
H17A H -0.1581 0.2630 0.2538 0.063 Uiso 1 1 calc R . .
H17B H -0.3294 0.2397 0.2040 0.063 Uiso 1 1 calc R . .
C3 C 0.1899(6) 0.1667(2) 0.3206(2) 0.0561(10) Uani 1 1 d . . .
H3 H 0.1331 0.1267 0.3400 0.067 Uiso 1 1 calc R . .
N4 N -0.0967(4) 0.35592(17) 0.01974(16) 0.0452(7) Uani 1 1 d . . .
C165 C -0.2383(5) 0.3419(2) 0.1758(2) 0.0499(8) Uani 1 1 d . . .
H16A H -0.3077 0.3417 0.1278 0.060 Uiso 1 1 calc R . .
H16B H -0.3010 0.3704 0.2094 0.060 Uiso 1 1 calc R . .
C2 C 0.3298(6) 0.2017(3) 0.3617(2) 0.0650(12) Uani 1 1 d . . .
H2 H 0.3674 0.1854 0.4094 0.078 Uiso 1 1 calc R . .
C10 C -0.1391(5) 0.3358(3) -0.0510(2) 0.0567(10) Uani 1 1 d . . .
H10 H -0.0967 0.2907 -0.0672 0.068 Uiso 1 1 calc R . .
C6 C -0.2174(5) 0.1858(2) 0.0914(2) 0.0549(9) Uani 1 1 d . . .
H6A H -0.2937 0.2244 0.0681 0.066 Uiso 1 1 calc R . .
H6B H -0.2895 0.1454 0.1063 0.066 Uiso 1 1 calc R . .
C11 C -0.2432(6) 0.3796(3) -0.1006(2) 0.0699(13) Uani 1 1 d . . .
H11 H -0.2740 0.3632 -0.1488 0.084 Uiso 1 1 calc R . .
C13 C -0.2588(6) 0.4679(3) -0.0060(3) 0.0663(12) Uani 1 1 d . . .
H13 H -0.2998 0.5129 0.0111 0.080 Uiso 1 1 calc R . .
C15 C -0.1006(5) 0.4441(2) 0.1205(2) 0.0549(9) Uani 1 1 d . . .
H15A H 0.0052 0.4737 0.1229 0.066 Uiso 1 1 calc R . .
H15B H -0.1906 0.4751 0.1375 0.066 Uiso 1 1 calc R . .
C1 C 0.4117(6) 0.2598(3) 0.3321(2) 0.0611(11) Uani 1 1 d . . .
H1 H 0.5055 0.2838 0.3591 0.073 Uiso 1 1 calc R . .
C12 C -0.3012(6) 0.4478(3) -0.0781(3) 0.0767(15) Uani 1 1 d . . .
H12 H -0.3674 0.4793 -0.1111 0.092 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'
N N 0.0061 0.0033 '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'
P P 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Cl Cl 0.1484 0.1585 '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'
H H 0.0000 0.0000 '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
N3 C30 C31 122.4(4) . . ?
C32 C33 C7 119.4(5) . . ?
C32 C31 C30 117.8(5) . . ?
C33 C32 C31 120.3(4) . . ?
N3 Mn1 N1 104.45(11) . . ?
N3 Mn1 N6 140.33(10) . . ?
N1 Mn1 N6 90.14(10) . . ?
N3 Mn1 N2 72.21(11) . . ?
N1 Mn1 N2 72.96(10) . . ?
N6 Mn1 N2 77.48(10) . . ?
N3 Mn1 N4 87.57(11) . . ?
N1 Mn1 N4 161.58(10) . . ?
N6 Mn1 N4 71.95(10) . . ?
N2 Mn1 N4 98.26(10) . . ?
N3 Mn1 Cl1 99.73(8) . . ?
N1 Mn1 Cl1 97.11(7) . . ?
N6 Mn1 Cl1 115.06(8) . . ?
N2 Mn1 Cl1 164.54(8) . . ?
N4 Mn1 Cl1 94.47(8) . . ?
F2 P3 F1 93.4(4) . . ?
F2 P3 F3 91.1(4) . . ?
F1 P3 F3 174.4(4) . . ?
F2 P3 F6 92.0(2) . . ?
F1 P3 F6 89.9(3) . . ?
F3 P3 F6 93.2(3) . . ?
F2 P3 F4 178.7(4) . . ?
F1 P3 F4 85.2(4) . . ?
F3 P3 F4 90.2(4) . . ?
F6 P3 F4 88.2(2) . . ?
F2 P3 F5 88.0(2) . . ?
F1 P3 F5 91.1(3) . . ?
F3 P3 F5 85.8(3) . . ?
F6 P3 F5 179.1(2) . . ?
F4 P3 F5 91.8(2) . . ?
C5 N2 C6 112.0(3) . . ?
C5 N2 C17 110.6(3) . . ?
C6 N2 C17 112.8(3) . . ?
C5 N2 Mn1 107.0(2) . . ?
C6 N2 Mn1 104.8(2) . . ?
C17 N2 Mn1 109.3(2) . . ?
C15 N6 C40 108.5(3) . . ?
C15 N6 C165 108.7(3) . . ?
C40 N6 C165 110.9(3) . . ?
C15 N6 Mn1 106.9(2) . . ?
C40 N6 Mn1 115.7(2) . . ?
C165 N6 Mn1 105.8(2) . . ?
C21 N1 C4 118.6(3) . . ?
C21 N1 Mn1 124.7(2) . . ?
C4 N1 Mn1 116.2(2) . . ?
C30 N3 C7 118.9(3) . . ?
C30 N3 Mn1 125.7(3) . . ?
C7 N3 Mn1 115.0(2) . . ?
N3 C7 C33 121.1(4) . . ?
N3 C7 C6 116.2(3) . . ?
C33 C7 C6 122.8(4) . . ?
N1 C4 C3 121.5(4) . . ?
N1 C4 C5 116.2(3) . . ?
C3 C4 C5 122.3(3) . . ?
N2 C5 C4 110.3(3) . . ?
N1 C21 C1 123.1(4) . . ?
N4 C14 C13 122.1(4) . . ?
N4 C14 C15 116.7(3) . . ?
C13 C14 C15 121.2(4) . . ?
N2 C17 C165 111.9(3) . . ?
C2 C3 C4 118.5(4) . . ?
C14 N4 C10 117.9(3) . . ?
C14 N4 Mn1 114.7(2) . . ?
C10 N4 Mn1 127.2(3) . . ?
N6 C165 C17 112.3(3) . . ?
C1 C2 C3 119.9(4) . . ?
N4 C10 C11 122.3(4) . . ?
N2 C6 C7 110.3(3) . . ?
C12 C11 C10 119.4(4) . . ?
C12 C13 C14 120.1(5) . . ?
N6 C15 C14 112.3(3) . . ?
C2 C1 C21 118.4(4) . . ?
C13 C12 C11 118.1(4) . . ?
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
F6 P3 1.561(3) . ?
F5 P3 1.580(3) . ?
C30 N3 1.329(5) . ?
C30 C31 1.385(6) . ?
F4 P3 1.574(4) . ?
C33 C32 1.355(8) . ?
C33 C7 1.377(6) . ?
C31 C32 1.378(8) . ?
F2 P3 1.506(4) . ?
F3 P3 1.526(4) . ?
F1 P3 1.522(4) . ?
Cl1 Mn1 2.3757(9) . ?
C40 N6 1.473(5) . ?
Mn1 N3 2.246(3) . ?
Mn1 N1 2.274(3) . ?
Mn1 N6 2.328(3) . ?
Mn1 N2 2.328(3) . ?
Mn1 N4 2.340(3) . ?
N2 C5 1.469(5) . ?
N2 C6 1.470(5) . ?
N2 C17 1.481(5) . ?
N6 C15 1.466(5) . ?
N6 C165 1.479(5) . ?
N1 C21 1.334(5) . ?
N1 C4 1.341(4) . ?
N3 C7 1.355(5) . ?
C7 C6 1.509(6) . ?
C4 C3 1.389(5) . ?
C4 C5 1.508(6) . ?
C21 C1 1.378(5) . ?
C14 N4 1.335(5) . ?
C14 C13 1.379(5) . ?
C14 C15 1.505(6) . ?
C17 C165 1.506(5) . ?
C3 C2 1.388(7) . ?
N4 C10 1.341(5) . ?
C2 C1 1.360(7) . ?
C10 C11 1.378(6) . ?
C11 C12 1.377(7) . ?
C13 C12 1.363(7) . ?
