#------------------------------------------------------------------------------
#$Date: 2016-02-16 22:30:59 +0200 (Tue, 16 Feb 2016) $
#$Revision: 176467 $
#$URL: svn://www.crystallography.net/cod/cif/4/31/10/4311041.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_4311041
loop_
_publ_author_name
'James D. Martin'
'Ryan F. Hess'
'Paul D. Boyle'
_publ_contact_author_address
;
   Dept. of Chemistry, NCSU
;
_publ_contact_author_name        'James D. Martin'
_publ_section_title
;
 Synthesis of [NH4]MnCl2(OAc) and [NH4]2MnCl4(H2O)2 by Solvothermal
 Dehydration and Structure/Property Correlations in a One-Dimensional
 Antiferromagnet
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              3242
_journal_page_last               3247
_journal_paper_doi               10.1021/ic049881r
_journal_volume                  43
_journal_year                    2004
_chemical_formula_moiety         'Mn Cl4 N2 O2 H12 '
_chemical_formula_sum            'Cl4 H12 Mn N2 O2'
_chemical_formula_weight         268.85
_chemical_name_systematic        ?
_space_group_IT_number           139
_symmetry_cell_setting           tetragonal
_symmetry_space_group_name_Hall  '-I 4 2'
_symmetry_space_group_name_H-M   'I 4/m m m'
_cell_angle_alpha                90.0
_cell_angle_beta                 90.0
_cell_angle_gamma                90.0
_cell_formula_units_Z            2
_cell_length_a                   7.5250(5)
_cell_length_b                   7.5250(5)
_cell_length_c                   8.2760(17)
_cell_measurement_reflns_used    24
_cell_measurement_temperature    293
_cell_measurement_theta_max      17.50
_cell_measurement_theta_min      11.50
_cell_volume                     468.63(11)
_computing_cell_refinement       'Nonius CAD4 Argus'
_computing_data_collection       'Nonius CAD4 Argus'
_computing_data_reduction        'NRCVAX DATRD2'
_computing_molecular_graphics    NRCVAX
_computing_publication_material  'NRCVAX TABLES Jan 94 Version'
_computing_structure_refinement  'NRCVAX LSTSQ'
_computing_structure_solution    'from literature'
_diffrn_ambient_temperature      293
_diffrn_measurement_device       'Nonius CAD4     '
_diffrn_measurement_method       'Omega scan b/P/b        '
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'xray tube'
_diffrn_radiation_type           'Molybdenum K\a'
_diffrn_radiation_wavelength     .71073
_diffrn_reflns_av_R_equivalents  .050
_diffrn_reflns_limit_h_max       8
_diffrn_reflns_limit_h_min       0
_diffrn_reflns_limit_k_max       6
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       9
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_number            250
_diffrn_reflns_theta_max         25.00
_diffrn_reflns_theta_min         0.00
_diffrn_standards_decay_%        3.7
_diffrn_standards_interval_time  80
_diffrn_standards_number         3
_exptl_absorpt_coefficient_mu    2.49
_exptl_absorpt_correction_type   none
_exptl_crystal_density_diffrn    1.905
_exptl_crystal_description       prism
_exptl_crystal_F_000             271.95
_exptl_crystal_size_max          .20
_exptl_crystal_size_mid          .15
_exptl_crystal_size_min          .10
_refine_diff_density_max         .70
_refine_diff_density_min         -.41
_refine_ls_goodness_of_fit_obs   1.47
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     12
_refine_ls_number_reflns         120
_refine_ls_R_factor_all          .055
_refine_ls_R_factor_obs          .040
_refine_ls_shift/esd_max         .000
_refine_ls_structure_factor_coef F
_refine_ls_weighting_details     '1/(σ²(F)+ .0005F²) '
_refine_ls_weighting_scheme      sigma
_refine_ls_wR_factor_all         .049
_refine_ls_wR_factor_obs         .049
_reflns_number_observed          120
_reflns_number_total             139
_reflns_observed_criterion       'Inet > 1.0\s(Inet)'
_cod_data_source_file            ic049881rsi20040128_044152.cif
_cod_data_source_block           x95018
_cod_original_cell_volume        468.63(10)
_cod_original_formula_sum        'Mn Cl4 N2 O2 H12 '
_cod_database_code               4311041
loop_
_symmetry_equiv_pos_as_xyz
x,y,z
-x,-y,-z
1/2+x,1/2+y,1/2+z
1/2-x,1/2-y,1/2-z
-y,x,z
y,-x,-z
1/2-y,1/2+x,1/2+z
1/2+y,1/2-x,1/2-z
-x,-y,z
x,y,-z
1/2-x,1/2-y,1/2+z
1/2+x,1/2+y,1/2-z
y,-x,z
-y,x,-z
1/2+y,1/2-x,1/2+z
1/2-y,1/2+x,1/2-z
-x,y,z
x,-y,-z
1/2-x,1/2+y,1/2+z
1/2+x,1/2-y,1/2-z
y,x,z
-y,-x,-z
1/2+y,1/2+x,1/2+z
1/2-y,1/2-x,1/2-z
x,-y,z
-x,y,-z
1/2+x,1/2-y,1/2+z
1/2-x,1/2+y,1/2-z
-y,-x,z
y,x,-z
1/2-y,1/2-x,1/2+z
1/2+y,1/2+x,1/2-z
loop_
_atom_site_label
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_type_symbol
_atom_site_occupancy
Mn .00000 .00000 .00000 .0300(10) Uani ? S Mn 1
Cl .2391(2) .23914 .00000 .0397(11) Uani ? S Cl 1
O .00000 .00000 .2658(10) .042(3) Uani ? S O 1
N .00000 .50000 .25000 .049(4) Uani ? S N 1
H1 .078 .078 .295 .0522 Uiso ? S H .500
H2 .093 .500 .310 .0592 Uiso ? S H 1
loop_
_atom_site_aniso_label
_atom_site_aniso_U_11
_atom_site_aniso_U_22
_atom_site_aniso_U_33
_atom_site_aniso_U_12
_atom_site_aniso_U_13
_atom_site_aniso_U_23
_atom_site_aniso_type_symbol
Mn .0336(12) .0336 .0226(15) .00000 .00000 .00000 Mn
Cl .0388(10) .0388 .0416(14) -.0035(10) .00000 .00000 Cl
O .050(4) .050 .027(5) .00000 .00000 .00000 O
N .062(5) .062 .024(6) .00000 .00000 .00000 N
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
Mn ? .337 .728 'International Tables Vol. IV Table 2.2B'
Cl ? .148 .159 'International Tables Vol. IV Table 2.2B'
N ? .006 .003 'International Tables Vol. IV Table 2.2B'
O ? .011 .006 'International Tables Vol. IV Table 2.2B'
H ? .000 .000 'International Tables Vol. IV Table 2.2B'
loop_
_diffrn_standard_refln_index_h
_diffrn_standard_refln_index_k
_diffrn_standard_refln_index_l
-4 0 -4
0 -4 -4
0 0 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_2
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
Cl Mn Cl 180.0 ? ? 2_555 ?
Cl Mn Cl 90.0 ? ? 5_555 ?
Cl Mn Cl 90.0 ? ? 6_555 ?
Cl Mn Cl 90.0 2_555 ? 5_555 ?
Cl Mn Cl 90.0 2_555 ? 6_555 ?
Cl Mn Cl 180.0 5_555 ? 6_555 ?
H1 O H1 85.6(3) ? ? 5_555 ?
H1 O H1 147.8(10) ? ? 9_555 ?
H1 O H1 85.6(3) ? ? 13_555 ?
H1 O H1 85.6(3) 5_555 ? 9_555 ?
H1 O H1 147.8(10) 5_555 ? 13_555 ?
H1 O H1 85.6(3) 9_555 ? 13_555 ?
H2 N H2 109.455(6) ? ? 8_455 ?
H2 N H2 109.503(12) ? ? 9_565 ?
H2 N H2 109.455(6) ? ? 16_555 ?
H2 N H2 109.455(6) 8_455 ? 9_565 ?
H2 N H2 109.503(12) 8_455 ? 16_555 ?
H2 N H2 109.455(6) 9_565 ? 16_555 ?
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_1
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Mn Cl 2.545(2) ? ? ?
Mn Cl 2.545(2) ? 2_555 ?
Mn Cl 2.545(2) ? 5_555 ?
Mn Cl 2.545(2) ? 6_555 ?
O H1 .860(2) ? ? ?
O H1 .860(2) ? 5_555 ?
O H1 .860(2) ? 9_555 ?
O H1 .860(2) ? 13_555 ?
N H2 .86000(7) ? ? ?
N H2 .86000(7) ? 8_455 ?
N H2 .86000(7) ? 9_565 ?
N H2 .86000(7) ? 16_555 ?
