#------------------------------------------------------------------------------
#$Date: 2016-03-25 16:22:33 +0200 (Fri, 25 Mar 2016) $
#$Revision: 179966 $
#$URL: svn://www.crystallography.net/cod/cif/7/02/60/7026074.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_7026074
loop_
_publ_author_name
'Sengupta, Oindrila'
'Gole, Bappaditya'
'Mukherjee, Sandip'
'Mukherjee, Partha Sarathi'
_publ_section_title
;
 A series of transition metal-azido extended complexes with various
 anionic and neutral co-ligands: synthesis, structure and their distinct
 magnetic behavior.
;
_journal_issue                   32
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              7451
_journal_page_last               7465
_journal_paper_doi               10.1039/c0dt00181c
_journal_volume                  39
_journal_year                    2010
_chemical_formula_moiety         'C7 H8 Mn N4 O3'
_chemical_formula_sum            'C7 H8 Mn N4 O3'
_chemical_formula_weight         251.11
_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                83.1980(10)
_cell_angle_beta                 73.1330(10)
_cell_angle_gamma                62.1050(10)
_cell_formula_units_Z            2
_cell_length_a                   7.4957(7)
_cell_length_b                   7.5942(7)
_cell_length_c                   9.4664(8)
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      28.33
_cell_volume                     455.67(7)
_computing_cell_refinement       'Bruker SMART'
_computing_data_collection       'Bruker SMART'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    'ORTEP-3 for Windows (Farrugia, 1999)'
_computing_publication_material  WinGX
_computing_structure_refinement  'SHELXL97 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.935
_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  0.0184
_diffrn_reflns_av_sigmaI/netI    0.0253
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_k_max       9
_diffrn_reflns_limit_k_min       -10
_diffrn_reflns_limit_l_max       12
_diffrn_reflns_limit_l_min       -12
_diffrn_reflns_number            5288
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         28.33
_diffrn_reflns_theta_min         2.25
_exptl_absorpt_coefficient_mu    1.440
_exptl_absorpt_correction_T_max  0.7333
_exptl_absorpt_correction_T_min  0.5691
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_process_details   SADABS
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    1.830
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             254
_exptl_crystal_size_max          0.34
_exptl_crystal_size_mid          0.28
_exptl_crystal_size_min          0.22
_refine_diff_density_max         0.305
_refine_diff_density_min         -0.239
_refine_diff_density_rms         0.058
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.048
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     147
_refine_ls_number_reflns         2122
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.048
_refine_ls_R_factor_all          0.0329
_refine_ls_R_factor_gt           0.0265
_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)+(0.0333P)²+0.1400P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0639
_refine_ls_wR_factor_ref         0.0674
_reflns_number_gt                1834
_reflns_number_total             2122
_reflns_threshold_expression     >2σ(I)
_cod_data_source_file            c0dt00181c.txt
_cod_data_source_block           complex3
_cod_database_code               7026074
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
Mn1 Mn 0.5000 0.0000 0.0000 0.01835(11) Uani 1 2 d S
Mn2 Mn 0.0000 0.5000 0.0000 0.01994(11) Uani 1 2 d S
O1 O 0.2920(2) 0.00815(19) -0.12959(14) 0.0280(3) Uani 1 1 d .
O2 O 0.1257(2) 0.3255(2) -0.19141(14) 0.0324(3) Uani 1 1 d .
N1 N 0.3004(2) 0.3183(2) 0.06429(17) 0.0227(3) Uani 1 1 d .
N2 N 0.3476(2) 0.4056(2) 0.13191(16) 0.0222(3) Uani 1 1 d .
N3 N 0.3919(3) 0.4914(3) 0.1972(2) 0.0378(4) Uani 1 1 d .
N4 N 0.2738(2) -0.0641(2) -0.79888(15) 0.0233(3) Uani 1 1 d .
H4A H 0.1453 0.0004 -0.8140 0.028 Uiso 1 1 calc R
H4B H 0.3121 -0.1952 -0.8024 0.028 Uiso 1 1 calc R
O1W O 0.1439(3) 0.7011(3) -0.1204(2) 0.0395(4) Uani 1 1 d .
C1 C 0.2127(3) 0.1414(3) -0.21817(18) 0.0207(3) Uani 1 1 d .
C2 C 0.2223(3) 0.0807(3) -0.36649(18) 0.0200(3) Uani 1 1 d .
C3 C 0.3514(3) -0.1127(3) -0.42249(18) 0.0213(4) Uani 1 1 d .
H3 H 0.4281 -0.2102 -0.3649 0.026 Uiso 1 1 calc R
C4 C 0.3665(3) -0.1613(3) -0.56335(19) 0.0228(4) Uani 1 1 d .
H4 H 0.4536 -0.2910 -0.6000 0.027 Uiso 1 1 calc R
C7 C 0.1068(3) 0.2241(3) -0.45412(19) 0.0244(4) Uani 1 1 d .
H7 H 0.0189 0.3537 -0.4174 0.029 Uiso 1 1 calc R
C6 C 0.1209(3) 0.1765(3) -0.59451(19) 0.0243(4) Uani 1 1 d .
H6 H 0.0429 0.2735 -0.6517 0.029 Uiso 1 1 calc R
C5 C 0.2519(3) -0.0166(3) -0.65011(18) 0.0199(3) Uani 1 1 d .
H1W H 0.271(6) 0.621(6) -0.164(4) 0.095(13) Uiso 1 1 d .
H2W H 0.148(5) 0.790(5) -0.091(3) 0.070(11) 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'
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
N1 Mn1 N1 180.0 . 2_655
N1 Mn1 O1 88.12(5) . 2_655
N1 Mn1 O1 91.88(5) 2_655 2_655
N1 Mn1 O1 91.88(5) . .
N1 Mn1 O1 88.12(5) 2_655 .
O1 Mn1 O1 180.00(8) 2_655 .
N1 Mn1 N4 86.37(6) . 1_556
N1 Mn1 N4 93.63(6) 2_655 1_556
O1 Mn1 N4 94.56(5) 2_655 1_556
O1 Mn1 N4 85.44(5) . 1_556
N1 Mn1 N4 93.63(6) . 2_654
N1 Mn1 N4 86.37(6) 2_655 2_654
O1 Mn1 N4 85.45(5) 2_655 2_654
O1 Mn1 N4 94.55(5) . 2_654
N4 Mn1 N4 180.0 1_556 2_654
O2 Mn2 O2 180.00(4) 2_565 .
O2 Mn2 N1 90.33(5) 2_565 .
O2 Mn2 N1 89.67(5) . .
O2 Mn2 N1 89.67(5) 2_565 2_565
O2 Mn2 N1 90.33(5) . 2_565
N1 Mn2 N1 180.0 . 2_565
O2 Mn2 O1W 90.42(6) 2_565 .
O2 Mn2 O1W 89.58(6) . .
N1 Mn2 O1W 86.83(6) . .
N1 Mn2 O1W 93.17(6) 2_565 .
O2 Mn2 O1W 89.58(6) 2_565 2_565
O2 Mn2 O1W 90.42(6) . 2_565
N1 Mn2 O1W 93.17(6) . 2_565
N1 Mn2 O1W 86.83(6) 2_565 2_565
O1W Mn2 O1W 180.0 . 2_565
C1 O1 Mn1 127.15(11) . .
C1 O2 Mn2 134.47(12) . .
N2 N1 Mn1 122.42(12) . .
N2 N1 Mn2 115.76(11) . .
Mn1 N1 Mn2 121.79(6) . .
N3 N2 N1 179.48(19) . .
C5 N4 Mn1 121.54(10) . 1_554
O2 C1 O1 124.35(16) . .
O2 C1 C2 116.28(15) . .
O1 C1 C2 119.37(15) . .
C3 C2 C7 118.79(15) . .
C3 C2 C1 121.86(15) . .
C7 C2 C1 119.28(16) . .
C4 C3 C2 120.52(16) . .
C3 C4 C5 120.16(16) . .
C6 C7 C2 120.96(16) . .
C7 C6 C5 119.85(16) . .
C6 C5 C4 119.72(15) . .
C6 C5 N4 119.83(15) . .
C4 C5 N4 120.42(16) . .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
Mn1 N1 2.2107(14) .
Mn1 N1 2.2107(14) 2_655
Mn1 O1 2.2230(12) 2_655
Mn1 O1 2.2230(12) .
Mn1 N4 2.3273(15) 1_556
Mn1 N4 2.3273(15) 2_654
Mn2 O2 2.0824(12) 2_565
Mn2 O2 2.0824(12) .
Mn2 N1 2.2438(14) .
Mn2 N1 2.2438(14) 2_565
Mn2 O1W 2.2828(16) .
Mn2 O1W 2.2828(16) 2_565
O1 C1 1.267(2) .
O2 C1 1.257(2) .
N1 N2 1.194(2) .
N2 N3 1.155(2) .
N4 C5 1.439(2) .
N4 Mn1 2.3273(15) 1_554
C1 C2 1.501(2) .
C2 C3 1.390(2) .
C2 C7 1.394(2) .
C3 C4 1.384(2) .
C4 C5 1.390(2) .
C7 C6 1.380(2) .
C6 C5 1.388(2) .
