#------------------------------------------------------------------------------
#$Date: 2016-02-04 03:13:02 +0200 (Thu, 04 Feb 2016) $
#$Revision: 175642 $
#$URL: svn://www.crystallography.net/cod/cif/4/34/48/4344807.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_4344807
loop_
_publ_author_name
'Xu, Caixia'
'Zhang, Jianguo'
'Yin, Xin'
'Cheng, Zhenxuan'
_publ_section_title
;
 Structural Diversity and Properties of M(II) Coordination Compounds
 Constructed by 3-Hydrazino-4-amino-1,2,4-triazole Dihydrochloride as
 Starting Material.
;
_journal_issue                   1
_journal_name_full               'Inorganic chemistry'
_journal_page_first              322
_journal_paper_doi               10.1021/acs.inorgchem.5b02434
_journal_volume                  55
_journal_year                    2015
_chemical_formula_sum            'C6 H18 Cl2 Mn N18 O4'
_chemical_formula_weight         532.22
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           143
_symmetry_space_group_name_Hall  'P 3'
_symmetry_space_group_name_H-M   'P 3'
_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                120.00
_cell_formula_units_Z            1
_cell_length_a                   9.5156(2)
_cell_length_b                   9.5156(2)
_cell_length_c                   6.1577(3)
_cell_measurement_temperature    296(2)
_cell_volume                     482.86(3)
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      296(2)
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 1.000
_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  0.0163
_diffrn_reflns_av_sigmaI/netI    0.0264
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       6
_diffrn_reflns_limit_l_min       -8
_diffrn_reflns_number            4018
_diffrn_reflns_theta_full        28.32
_diffrn_reflns_theta_max         28.32
_diffrn_reflns_theta_min         2.47
_exptl_absorpt_coefficient_mu    1.023
_exptl_crystal_density_diffrn    1.830
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             271
_refine_diff_density_max         0.152
_refine_diff_density_min         -0.201
_refine_diff_density_rms         0.049
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   0.025(12)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.033
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     118
_refine_ls_number_reflns         1407
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.032
_refine_ls_R_factor_all          0.0176
_refine_ls_R_factor_gt           0.0174
_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)+(0.0289P)²+0.0000P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0446
_refine_ls_wR_factor_ref         0.0447
_reflns_number_gt                1392
_reflns_number_total             1407
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic5b02434_si_003.cif
_cod_data_source_block           1
_cod_original_sg_symbol_H-M      P3
_cod_database_code               4344807
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-y, x-y, z'
'-x+y, -x, 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
C1 C 0.98875(15) 0.36207(14) 0.2477(2) 0.0258(2) Uani 1 1 d .
C2 C 0.26539(18) -0.00114(18) -0.0663(3) 0.0345(3) Uani 1 1 d .
Cl1 Cl 0.0000 0.0000 0.44638(9) 0.02806(11) Uani 1 3 d S
Cl2 Cl 0.3333 0.6667 0.74378(9) 0.03346(12) Uani 1 3 d S
H1 H 0.200(2) -0.047(2) -0.183(3) 0.035(5) Uiso 1 1 d .
H2 H 0.947(3) 0.564(3) 0.521(4) 0.045(6) Uiso 1 1 d .
H3 H 0.884(3) 0.414(3) 0.671(4) 0.047(5) Uiso 1 1 d .
H4 H 1.121(4) 0.489(4) 0.475(5) 0.066(8) Uiso 1 1 d .
H5 H 1.271(3) 0.316(3) 0.146(4) 0.044(6) Uiso 1 1 d .
H6 H 1.307(3) 0.459(3) 0.041(4) 0.050(6) Uiso 1 1 d .
Mn1 Mn 0.6667 0.3333 0.32769(5) 0.02573(9) Uani 1 3 d S
N1 N 1.09173(13) 0.34652(14) 0.1124(2) 0.0293(2) Uani 1 1 d .
N2 N 1.25632(15) 0.40332(18) 0.1546(3) 0.0395(3) Uani 1 1 d .
N3 N 1.02471(15) 0.42690(15) 0.4494(2) 0.0315(2) Uani 1 1 d .
N4 N 0.90766(16) 0.46309(17) 0.5366(2) 0.0353(3) Uani 1 1 d .
N5 N 0.38455(16) 0.14721(16) -0.0467(2) 0.0355(3) Uani 1 1 d .
N6 N 0.45399(14) 0.15521(14) 0.15695(19) 0.0291(2) Uani 1 1 d .
O1 O 0.14696(13) 0.13619(14) 0.5253(2) 0.0473(3) Uani 1 1 d .
O2 O 0.0000 0.0000 0.2135(4) 0.0555(6) Uani 1 3 d S
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'
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'
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
N6 C1 N1 109.57(11) 2_655 .
N6 C1 N3 124.58(12) 2_655 .
N1 C1 N3 125.80(12) . .
N5 C2 N1 110.99(13) . 3_665
O2 Cl1 O1 109.79(6) . .
O2 Cl1 O1 109.79(6) . 3
O1 Cl1 O1 109.15(6) . 3
O2 Cl1 O1 109.79(6) . 2
O1 Cl1 O1 109.15(6) . 2
O1 Cl1 O1 109.15(6) 3 2
N6 Mn1 N6 98.22(4) 2_655 .
N6 Mn1 N6 98.22(4) 2_655 3_665
N6 Mn1 N6 98.22(4) . 3_665
N6 Mn1 N4 73.39(4) 2_655 .
N6 Mn1 N4 163.54(4) . .
N6 Mn1 N4 97.02(5) 3_665 .
N6 Mn1 N4 97.02(5) 2_655 3_665
N6 Mn1 N4 73.39(4) . 3_665
N6 Mn1 N4 163.53(4) 3_665 3_665
N4 Mn1 N4 93.27(5) . 3_665
N6 Mn1 N4 163.54(4) 2_655 2_655
N6 Mn1 N4 97.02(5) . 2_655
N6 Mn1 N4 73.39(4) 3_665 2_655
N4 Mn1 N4 93.27(5) . 2_655
N4 Mn1 N4 93.27(5) 3_665 2_655
C1 N1 C2 105.50(11) . 2_655
C1 N1 N2 125.15(12) . .
C2 N1 N2 129.35(13) 2_655 .
C1 N3 N4 113.97(11) . .
N3 N4 Mn1 109.84(8) . .
C2 N5 N6 105.86(12) . .
C1 N6 N5 108.06(11) 3_665 .
C1 N6 Mn1 116.23(9) 3_665 .
N5 N6 Mn1 135.32(9) . .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
C1 N6 1.3139(17) 2_655
C1 N1 1.3496(16) .
C1 N3 1.3527(18) .
C2 N5 1.3009(19) .
C2 N1 1.3703(19) 3_665
Cl1 O2 1.434(3) .
Cl1 O1 1.4349(11) .
Cl1 O1 1.4348(11) 3
Cl1 O1 1.4349(11) 2
Mn1 N6 2.1549(12) 2_655
Mn1 N6 2.1549(12) .
Mn1 N6 2.1549(12) 3_665
Mn1 N4 2.3680(13) .
Mn1 N4 2.3680(13) 3_665
Mn1 N4 2.3680(13) 2_655
N1 C2 1.3703(19) 2_655
N1 N2 1.4021(17) .
N3 N4 1.4251(17) .
N5 N6 1.4019(18) .
N6 C1 1.3139(17) 3_665
