#------------------------------------------------------------------------------
#$Date: 2016-03-25 23:12:50 +0100 (vie 25 de mar de 2016) $
#$Revision: 180065 $
#$URL: svn://www.crystallography.net/cod/cif/7/05/11/7051193.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_7051193
loop_
_publ_author_name
'Iwayan Dasna'
'Stéphane Golhen'
'Lahcène Ouahab'
'Nathalie Daro'
'Jean-Pascal Sutter'
_publ_section_title
;
 Synthesis, X-ray crystal structures and magnetic properties of CuII
 and MnII complexes containing imino nitroxide radicals and a
 dicyanamide anion
;
_journal_issue                   12
_journal_name_full               'New J. Chem.'
_journal_page_first              1572
_journal_page_last               1576
_journal_paper_doi               10.1039/b104773f
_journal_volume                  25
_journal_year                    2001
_chemical_formula_sum            'C28 H36 Mn N12 O4'
_chemical_formula_weight         659.63
_chemical_name_systematic
; 
? 
;
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                69.3961(14)
_cell_angle_beta                 88.9996(14)
_cell_angle_gamma                71.461(2)
_cell_formula_units_Z            1
_cell_length_a                   7.1089(2)
_cell_length_b                   9.9495(3)
_cell_length_c                   13.2518(6)
_cell_measurement_reflns_used    3591
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      27.485
_cell_measurement_theta_min      0.998
_cell_volume                     827.10(5)
_computing_cell_refinement       'HKL Scalepack (Otwinowski & Minor 1997)'
_computing_data_collection       'Collect (Nonius BV, 1997-2000)'
_computing_data_reduction
'HKL Denzo and Scalepack (Otwinowski & Minor 1997)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      293(2)
_diffrn_detector_area_resol_mean 9
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measurement_device       '95mm CCD camera on κ-goniostat'
_diffrn_measurement_device_type  KappaCCD
_diffrn_measurement_method       CCD
_diffrn_radiation_monochromator  'horizonally mounted graphite crystal'
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0289
_diffrn_reflns_av_sigmaI/netI    0.0557
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_h_min       -8
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            6724
_diffrn_reflns_theta_full        27.49
_diffrn_reflns_theta_max         27.49
_diffrn_reflns_theta_min         1.65
_exptl_absorpt_coefficient_mu    0.451
_exptl_absorpt_correction_type   none
_exptl_crystal_density_diffrn    1.324
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             345
_refine_diff_density_max         0.486
_refine_diff_density_min         -0.434
_refine_diff_density_rms         0.057
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.029
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     216
_refine_ls_number_reflns         3787
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.030
_refine_ls_R_factor_all          0.0672
_refine_ls_R_factor_gt           0.0462
_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)+(0.0753P)²+0.1378P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1201
_refine_ls_wR_factor_ref         0.1378
_reflns_number_gt                2924
_reflns_number_total             3787
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            b104773f.txt
_cod_data_source_block           2
_cod_depositor_comments
;
The following automatic conversions were performed:
'_symmetry_cell_setting' value 'Triclinic' changed to 'triclinic'
according to '/home/saulius/struct/CIF-dictionaries/cif_core.dic'
dictionary named 'cif_core.dic' version 2.4.1 from
2010-06-29.

'_exptl_absorpt_correction_type' value 'None' changed to
'none' according to '/home/saulius/struct/CIF-dictionaries/cif_core.dic'
dictionary named 'cif_core.dic' version 2.4.1 from 2010-06-29.

Automatic conversion script
Id: cif_fix_enum 1527 2010-12-29 10:47:43Z saulius 
;
_cod_original_cell_volume        827.09(5)
_cod_original_sg_symbol_H-M      P-1
_cod_database_code               7051193
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_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
Mn Mn 0.0000 0.0000 0.0000 0.03234(16) Uani 1 2 d S . .
OW1 O 0.0646(2) 0.17547(18) 0.04029(15) 0.0457(4) Uani 1 1 d . . .
O1A O 0.5940(4) 0.1782(5) -0.4534(3) 0.0891(16) Uani 0.700(7) 1 d P . .
O1B O -0.0492(10) 0.3988(10) -0.5854(6) 0.096(4) Uani 0.335(7) 1 d P . .
N4 N 0.3095(3) -0.1530(2) 0.05661(18) 0.0454(5) Uani 1 1 d . . .
N1 N 0.0938(3) 0.0811(2) -0.17075(15) 0.0393(4) Uani 1 1 d . . .
C13 C 0.4558(3) -0.2344(3) 0.0435(2) 0.0394(5) Uani 1 1 d . . .
C1 C 0.2634(3) 0.1129(3) -0.18832(19) 0.0448(5) Uani 1 1 d . . .
H1 H 0.3473 0.0950 -0.1286 0.054 Uiso 1 1 calc R . .
C3 C 0.1991(3) 0.1967(3) -0.38040(19) 0.0424(5) Uani 1 1 d . . .
C2 C 0.3205(4) 0.1707(3) -0.2900(2) 0.0475(6) Uani 1 1 d . . .
H2 H 0.4393 0.1921 -0.2979 0.057 Uiso 1 1 calc R . .
C6 C 0.2520(4) 0.2542(3) -0.4914(2) 0.0481(6) Uani 1 1 d . . .
C4 C 0.0232(3) 0.1625(3) -0.3627(2) 0.0497(6) Uani 1 1 d . . .
H4 H -0.0624 0.1776 -0.4209 0.060 Uiso 1 1 calc R . .
N2 N 0.4416(3) 0.2420(3) -0.51475(18) 0.0546(6) Uani 1 1 d . . .
N5 N 0.6293(3) -0.3087(3) 0.0263(3) 0.0673(8) Uani 1 1 d . . .
C14 C 0.6880(3) -0.4538(3) 0.0422(2) 0.0474(6) Uani 1 1 d . . .
N3 N 0.1206(4) 0.3212(3) -0.57746(19) 0.0688(7) Uani 1 1 d . . .
N6 N 0.7575(3) -0.5790(3) 0.0533(2) 0.0672(7) Uani 1 1 d . . .
C5 C -0.0226(3) 0.1062(3) -0.2583(2) 0.0463(6) Uani 1 1 d . . .
H5 H -0.1409 0.0844 -0.2479 0.056 Uiso 1 1 calc R . .
C7 C 0.4402(4) 0.3248(3) -0.6327(2) 0.0553(6) Uani 1 1 d . . .
C8 C 0.2281(4) 0.3434(3) -0.6755(2) 0.0575(7) Uani 1 1 d . . .
C11 C 0.1141(7) 0.4986(4) -0.7603(3) 0.0994(13) Uani 1 1 d . . .
H11A H 0.1159 0.5771 -0.7345 0.149 Uiso 1 1 calc R . .
H11B H -0.0214 0.5050 -0.7735 0.149 Uiso 1 1 calc R . .
H11C H 0.1759 0.5115 -0.8265 0.149 Uiso 1 1 calc R . .
C10 C 0.6150(6) 0.2320(5) -0.6745(3) 0.0962(13) Uani 1 1 d . . .
H10A H 0.5963 0.1383 -0.6690 0.144 Uiso 1 1 calc R . .
H10B H 0.7365 0.2100 -0.6320 0.144 Uiso 1 1 calc R . .
H10C H 0.6226 0.2889 -0.7490 0.144 Uiso 1 1 calc R . .
C12 C 0.2224(6) 0.2201(5) -0.7153(3) 0.0841(10) Uani 1 1 d . . .
H12A H 0.2932 0.1222 -0.6614 0.126 Uiso 1 1 calc R . .
H12B H 0.2842 0.2317 -0.7814 0.126 Uiso 1 1 calc R . .
H12C H 0.0863 0.2277 -0.7282 0.126 Uiso 1 1 calc R . .
C9 C 0.4703(7) 0.4742(5) -0.6416(3) 0.0925(12) Uani 1 1 d . . .
H9A H 0.3599 0.5329 -0.6152 0.139 Uiso 1 1 calc R . .
H9B H 0.4779 0.5312 -0.7160 0.139 Uiso 1 1 calc R . .
H9C H 0.5918 0.4522 -0.5991 0.139 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'
O O 0.0106 0.0060 '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
OW1 Mn OW1 180.00(8) 2 . ?
OW1 Mn N4 90.54(7) 2 2 ?
OW1 Mn N4 89.46(7) . 2 ?
OW1 Mn N4 89.46(7) 2 . ?
OW1 Mn N4 90.54(7) . . ?
N4 Mn N4 180.0(2) 2 . ?
OW1 Mn N1 87.04(7) 2 . ?
OW1 Mn N1 92.96(7) . . ?
N4 Mn N1 91.49(7) 2 . ?
N4 Mn N1 88.51(7) . . ?
OW1 Mn N1 92.96(7) 2 2 ?
OW1 Mn N1 87.04(7) . 2 ?
N4 Mn N1 88.51(7) 2 2 ?
N4 Mn N1 91.49(7) . 2 ?
N1 Mn N1 180.00(13) . 2 ?
C13 N4 Mn 150.59(19) . . ?
C1 N1 C5 116.78(19) . . ?
C1 N1 Mn 121.44(15) . . ?
C5 N1 Mn 121.70(14) . . ?
N4 C13 N5 171.4(2) . . ?
N1 C1 C2 123.6(2) . . ?
C2 C3 C4 117.4(2) . . ?
C2 C3 C6 122.7(2) . . ?
C4 C3 C6 119.9(2) . . ?
C1 C2 C3 119.3(2) . . ?
N3 C6 N2 113.6(2) . . ?
N3 C6 C3 123.3(2) . . ?
N2 C6 C3 123.1(2) . . ?
C5 C4 C3 119.3(2) . . ?
O1A N2 C6 128.4(3) . . ?
O1A N2 C7 122.3(2) . . ?
C6 N2 C7 109.2(2) . . ?
C13 N5 C14 123.8(2) . . ?
N6 C14 N5 173.0(3) . . ?
O1B N3 C6 128.2(5) . . ?
O1B N3 C8 118.7(4) . . ?
C6 N3 C8 108.7(2) . . ?
N1 C5 C4 123.6(2) . . ?
N2 C7 C10 109.0(3) . . ?
N2 C7 C9 105.2(3) . . ?
C10 C7 C9 109.4(3) . . ?
N2 C7 C8 100.8(2) . . ?
C10 C7 C8 116.8(3) . . ?
C9 C7 C8 114.4(3) . . ?
N3 C8 C12 105.4(3) . . ?
N3 C8 C11 108.4(3) . . ?
C12 C8 C11 109.5(3) . . ?
N3 C8 C7 103.6(2) . . ?
C12 C8 C7 113.8(3) . . ?
C11 C8 C7 115.4(3) . . ?
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
Mn OW1 2.1722(15) 2 ?
Mn OW1 2.1722(15) . ?
Mn N4 2.2012(18) 2 ?
Mn N4 2.2012(18) . ?
Mn N1 2.2847(19) . ?
Mn N1 2.2847(19) 2 ?
O1A N2 1.211(4) . ?
O1B N3 1.191(7) . ?
N4 C13 1.151(3) . ?
N1 C1 1.337(3) . ?
N1 C5 1.338(3) . ?
C13 N5 1.284(3) . ?
C1 C2 1.376(3) . ?
C3 C2 1.387(3) . ?
C3 C4 1.393(3) . ?
C3 C6 1.469(3) . ?
C6 N3 1.313(3) . ?
C6 N2 1.355(3) . ?
C4 C5 1.374(3) . ?
N2 C7 1.487(3) . ?
N5 C14 1.307(3) . ?
C14 N6 1.140(3) . ?
N3 C8 1.481(4) . ?
C7 C10 1.520(4) . ?
C7 C9 1.532(5) . ?
C7 C8 1.551(4) . ?
C8 C12 1.508(5) . ?
C8 C11 1.522(4) . ?
