#------------------------------------------------------------------------------
#$Date: 2016-03-22 11:44:04 +0200 (Tue, 22 Mar 2016) $
#$Revision: 178913 $
#$URL: svn://www.crystallography.net/cod/cif/4/11/42/4114220.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_4114220
loop_
_publ_author_name
'Claire Mantel'
'Alia K. Hassan'
'Jacques Pécaut'
'Alain Deronzier'
'Marie-Noëlle Collomb'
'Carole Duboc-Toia'
_publ_section_title
;
 A High-Frequency and High-Field EPR Study of New Azide and Fluoride
 Mononuclear Mn(III) Complexes
;
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              12337
_journal_page_last               12344
_journal_paper_doi               10.1021/ja034652+
_journal_volume                  125
_journal_year                    2003
_chemical_formula_sum            'C14 H17 Mn N12'
_chemical_formula_weight         408.34
_chemical_name_systematic
;
 ?
;
_space_group_IT_number           61
_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_Hall  '-P 2ac 2ab'
_symmetry_space_group_name_H-M   'P b c a'
_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                90.00
_cell_formula_units_Z            8
_cell_length_a                   8.5919(6)
_cell_length_b                   15.7208(11)
_cell_length_c                   27.2838(19)
_cell_measurement_temperature    223(2)
_cell_volume                     3685.3(4)
_computing_cell_refinement       'Bruker SMART'
_computing_data_collection       'Bruker SMART'
_computing_data_reduction        'Bruker SHELXTL'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      223(2)
_diffrn_measured_fraction_theta_full 0.857
_diffrn_measured_fraction_theta_max 0.857
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       'phi and omega 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  0.0277
_diffrn_reflns_av_sigmaI/netI    0.0536
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -2
_diffrn_reflns_limit_k_max       9
_diffrn_reflns_limit_k_min       -21
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_limit_l_min       -36
_diffrn_reflns_number            10138
_diffrn_reflns_theta_full        29.41
_diffrn_reflns_theta_max         29.41
_diffrn_reflns_theta_min         2.80
_exptl_absorpt_coefficient_mu    0.744
_exptl_absorpt_correction_type   none
_exptl_crystal_density_diffrn    1.472
_exptl_crystal_F_000             1680
_exptl_crystal_size_max          0.2
_exptl_crystal_size_mid          0.2
_exptl_crystal_size_min          0.4
_refine_diff_density_max         0.283
_refine_diff_density_min         -0.287
_refine_diff_density_rms         0.044
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.897
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     312
_refine_ls_number_reflns         4366
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.897
_refine_ls_R_factor_all          0.0603
_refine_ls_R_factor_gt           0.0303
_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)+(0.0349P)²+0.0000P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0645
_refine_ls_wR_factor_ref         0.0691
_reflns_number_gt                2842
_reflns_number_total             4366
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja0346522Bsi20030626_055518.cif
_cod_data_source_block           struc[Mn(bpea)(N3)3]
_cod_database_code               4114220
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x+1/2, -y, z+1/2'
'-x, y+1/2, -z+1/2'
'x+1/2, -y+1/2, -z'
'-x, -y, -z'
'x-1/2, y, -z-1/2'
'x, -y-1/2, z-1/2'
'-x-1/2, y-1/2, 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_symmetry_multiplicity
_atom_site_calc_flag
Mn Mn 0.81827(2) 0.099064(15) 0.621628(9) 0.02451(8) Uani 1 1 d
N1 N 0.59323(14) 0.17715(8) 0.62284(5) 0.0252(3) Uani 1 1 d
N2 N 0.64651(13) 0.01635(9) 0.58710(5) 0.0269(3) Uani 1 1 d
N3 N 0.88291(15) 0.21869(9) 0.65681(5) 0.0314(3) Uani 1 1 d
N4 N 1.02310(16) 0.03848(11) 0.62439(6) 0.0420(4) Uani 1 1 d
N5 N 0.87653(15) 0.14161(10) 0.55626(6) 0.0371(4) Uani 1 1 d
N6 N 0.75346(16) 0.05275(9) 0.68516(6) 0.0323(3) Uani 1 1 d
N7 N 1.06229(16) -0.00805(11) 0.65676(7) 0.0414(4) Uani 1 1 d
N8 N 1.1049(2) -0.05441(14) 0.68662(8) 0.0693(6) Uani 1 1 d
N9 N 1.00974(17) 0.15634(10) 0.54630(6) 0.0387(4) Uani 1 1 d
N10 N 1.13531(18) 0.17180(14) 0.53464(7) 0.0688(6) Uani 1 1 d
N11 N 0.8075(2) 0.07620(12) 0.72288(7) 0.0519(5) Uani 1 1 d
N12 N 0.8517(3) 0.0979(2) 0.75967(9) 0.1297(12) Uani 1 1 d
C1 C 1.0290(2) 0.24664(14) 0.66267(8) 0.0415(5) Uani 1 1 d
H1 H 1.107(2) 0.2066(12) 0.6513(7) 0.050(6) Uiso 1 1 d
C2 C 1.0621(2) 0.32438(14) 0.68320(8) 0.0486(6) Uani 1 1 d
H2 H 1.163(2) 0.3399(13) 0.6856(7) 0.055(6) Uiso 1 1 d
C3 C 0.9425(2) 0.37508(15) 0.69813(9) 0.0498(6) Uani 1 1 d
H3 H 0.965(2) 0.4292(14) 0.7117(7) 0.054(6) Uiso 1 1 d
C4 C 0.7905(2) 0.34649(13) 0.69287(8) 0.0419(5) Uani 1 1 d
H4 H 0.707(2) 0.3818(11) 0.7040(7) 0.044(5) Uiso 1 1 d
C5 C 0.76448(19) 0.26766(11) 0.67244(6) 0.0294(4) Uani 1 1 d
C6 C 0.60397(19) 0.22903(13) 0.66793(7) 0.0306(4) Uani 1 1 d
H6A H 0.5834(17) 0.1925(10) 0.6955(6) 0.023(4) Uiso 1 1 d
H6B H 0.5237(18) 0.2730(11) 0.6700(6) 0.029(4) Uiso 1 1 d
C7 C 0.5790(2) 0.23252(13) 0.57839(7) 0.0332(4) Uani 1 1 d
H7A H 0.5755(19) 0.1911(12) 0.5499(7) 0.045(5) Uiso 1 1 d
H7B H 0.6792(19) 0.2651(11) 0.5767(6) 0.037(5) Uiso 1 1 d
C8 C 0.4421(3) 0.29422(17) 0.57812(10) 0.0479(6) Uani 1 1 d
H8A H 0.438(2) 0.3269(13) 0.5461(9) 0.061(6) Uiso 1 1 d
H8B H 0.348(2) 0.2660(14) 0.5793(8) 0.066(7) Uiso 1 1 d
H8C H 0.454(3) 0.3407(17) 0.6053(11) 0.097(9) Uiso 1 1 d
C9 C 0.46469(19) 0.11385(12) 0.62480(8) 0.0316(4) Uani 1 1 d
H9A H 0.460(2) 0.0965(11) 0.6563(8) 0.040(6) Uiso 1 1 d
H9B H 0.364(2) 0.1425(12) 0.6164(7) 0.041(5) Uiso 1 1 d
C10 C 0.49676(17) 0.03805(10) 0.59275(6) 0.0264(4) Uani 1 1 d
C11 C 0.37863(19) -0.00998(12) 0.57211(7) 0.0334(4) Uani 1 1 d
H11 H 0.2789(18) 0.0076(10) 0.5765(6) 0.032(5) Uiso 1 1 d
C12 C 0.4154(2) -0.08219(12) 0.54620(7) 0.0374(5) Uani 1 1 d
H12 H 0.3422(18) -0.1156(11) 0.5328(7) 0.034(5) Uiso 1 1 d
C13 C 0.5691(2) -0.10489(13) 0.54078(8) 0.0383(5) Uani 1 1 d
H13 H 0.6005(19) -0.1534(12) 0.5239(7) 0.038(5) Uiso 1 1 d
C14 C 0.6814(2) -0.05378(12) 0.56122(7) 0.0337(4) Uani 1 1 d
H14 H 0.7910(19) -0.0665(11) 0.5597(7) 0.040(5) Uiso 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'
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
N6 Mn N5 177.22(6)
N6 Mn N4 92.28(6)
N5 Mn N4 88.40(6)
N6 Mn N2 88.19(6)
N5 Mn N2 89.04(6)
N4 Mn N2 109.11(6)
N6 Mn N3 90.19(6)
N5 Mn N3 92.35(6)
N4 Mn N3 99.76(6)
N2 Mn N3 151.12(5)
N6 Mn N1 86.93(5)
N5 Mn N1 92.61(5)
N4 Mn N1 175.02(6)
N2 Mn N1 75.79(5)
N3 Mn N1 75.33(5)
C6 N1 C9 112.66(14)
C6 N1 C7 110.98(14)
C9 N1 C7 110.93(14)
C6 N1 Mn 104.76(10)
C9 N1 Mn 105.59(10)
C7 N1 Mn 111.65(10)
C10 N2 C14 118.93(14)
C10 N2 Mn 116.63(11)
C14 N2 Mn 124.44(10)
C1 N3 C5 118.89(16)
C1 N3 Mn 124.99(13)
C5 N3 Mn 116.10(11)
N7 N4 Mn 124.50(12)
N9 N5 Mn 120.90(12)
N11 N6 Mn 122.67(13)
N8 N7 N4 177.0(2)
N10 N9 N5 176.82(19)
N12 N11 N6 176.6(3)
N3 C1 C2 122.28(19)
C3 C2 C1 119.11(19)
C2 C3 C4 119.3(2)
C5 C4 C3 119.08(18)
N3 C5 C4 121.36(16)
N3 C5 C6 115.73(15)
C4 C5 C6 122.86(15)
N1 C6 C5 110.26(14)
N1 C7 C8 115.90(16)
N1 C9 C10 111.91(13)
N2 C10 C11 121.21(16)
N2 C10 C9 116.40(14)
C11 C10 C9 122.30(15)
C12 C11 C10 119.42(16)
C11 C12 C13 119.35(17)
C14 C13 C12 118.60(19)
N2 C14 C13 122.47(16)
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
Mn N6 1.9609(15)
Mn N5 1.9695(15)
Mn N4 2.0025(14)
Mn N2 2.1808(13)
Mn N3 2.1832(14)
Mn N1 2.2905(12)
N1 C6 1.479(2)
N1 C9 1.487(2)
N1 C7 1.498(2)
N2 C10 1.3400(18)
N2 C14 1.343(2)
N3 C1 1.340(2)
N3 C5 1.345(2)
N4 N7 1.195(2)
N5 N9 1.1989(18)
N6 N11 1.188(2)
N7 N8 1.153(2)
N9 N10 1.1507(19)
N11 N12 1.126(3)
C1 C2 1.374(3)
C2 C3 1.363(3)
C3 C4 1.388(3)
C4 C5 1.377(2)
C5 C6 1.512(2)
C7 C8 1.524(3)
C9 C10 1.503(2)
C10 C11 1.385(2)
C11 C12 1.374(3)
C12 C13 1.376(2)
C13 C14 1.374(2)
