#------------------------------------------------------------------------------
#$Date: 2016-02-20 05:06:23 +0200 (Sat, 20 Feb 2016) $
#$Revision: 176774 $
#$URL: svn://www.crystallography.net/cod/cif/2/20/71/2207105.cif $
#------------------------------------------------------------------------------
#
# This file is available in the Crystallography Open Database (COD),
# http://www.crystallography.net/. The original data for this entry
# were provided by IUCr Journals, http://journals.iucr.org/.
#
# The file may be used within the scientific community so long as
# proper attribution is given to the journal article from which the
# data were obtained.
#
data_2207105
loop_
_publ_author_name
'Chen, Zi-Lu'
'Li, Shi-Bing'
'Qiu, Zhi-Hui'
'Zeng, Qing-Fen'
'Liang, Fu-Pei'
_publ_section_title
;
 Hexaaquamanganese(II) dichloride bis(hexamethylenetetramine)
 tetrahydrate
;
_journal_coeditor_code           XU6047
_journal_issue                   10
_journal_name_full               'Acta Crystallographica Section E'
_journal_page_first              m1931
_journal_page_last               m1932
_journal_paper_doi               10.1107/S1600536805027571
_journal_volume                  61
_journal_year                    2005
_chemical_formula_iupac          '[Mn (H2 O)6] Cl2 , 2C6 H12 N4 , 4H2 O'
_chemical_formula_moiety         'H12 Mn O6 2+ , 2Cl - , 2C6 H12 N4 , 4H2 O'
_chemical_formula_sum            'C12 H44 Cl2 Mn N8 O10'
_chemical_formula_weight         586.39
_chemical_name_systematic
;
Hexaaquamanganese(II) dichloride bis(hexamethylenetetraamine) tetrahydrate
;
_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           SHELXL97
_cell_angle_alpha                119.477(4)
_cell_angle_beta                 101.018(5)
_cell_angle_gamma                94.140(5)
_cell_formula_units_Z            1
_cell_length_a                   9.337(3)
_cell_length_b                   9.531(2)
_cell_length_c                   9.538(2)
_cell_measurement_reflns_used    1215
_cell_measurement_temperature    294(2)
_cell_measurement_theta_max      24.6
_cell_measurement_theta_min      2.3
_cell_volume                     711.4(3)
_computing_cell_refinement       'SAINT (Bruker, 1998)'
_computing_data_collection       'SMART (Bruker, 1998)'
_computing_data_reduction        SAINT
_computing_molecular_graphics    'SHELXTL (Bruker, 1997)'
_computing_publication_material  SHELXTL
_computing_structure_refinement  'SHELXL97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS97 (Sheldrick, 1997)'
_diffrn_ambient_temperature      294(2)
_diffrn_measured_fraction_theta_full 0.99
_diffrn_measured_fraction_theta_max 0.99
_diffrn_measurement_device_type  'Bruker SMART CCD area-detector'
_diffrn_measurement_method       'φ and ω'
_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  0.025
_diffrn_reflns_av_sigmaI/netI    0.058
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_k_min       -10
_diffrn_reflns_limit_l_max       8
_diffrn_reflns_limit_l_min       -11
_diffrn_reflns_number            4034
_diffrn_reflns_theta_full        26.4
_diffrn_reflns_theta_max         26.4
_diffrn_reflns_theta_min         2.3
_diffrn_standards_decay_%        0
_diffrn_standards_interval_count 0
_diffrn_standards_interval_time  0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.706
_exptl_absorpt_correction_T_max  0.893
_exptl_absorpt_correction_T_min  0.840
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   '(SADABS; Bruker, 1998)'
_exptl_crystal_colour            'pale yellow'
_exptl_crystal_density_diffrn    1.369
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             311
_exptl_crystal_size_max          0.22
_exptl_crystal_size_mid          0.18
_exptl_crystal_size_min          0.16
_refine_diff_density_max         0.28
_refine_diff_density_min         -0.27
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.038
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     151
_refine_ls_number_reflns         2850
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.038
_refine_ls_R_factor_all          0.074
_refine_ls_R_factor_gt           0.042
_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)+(0.0517P)²] where P = (Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.096
_refine_ls_wR_factor_ref         0.111
_reflns_number_gt                1975
_reflns_number_total             2850
_reflns_threshold_expression     I>2σ(I)
_cod_data_source_file            xu6047.cif
_cod_data_source_block           I
_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.

Automatic conversion script
Id: cif_fix_enum 1527 2010-12-29 10:47:43Z saulius 

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.

Automatic conversion script
Id: cif_fix_values 1715 2011-07-08 13:25:40Z adriana 
;
_cod_original_cell_volume        711.5(3)
_cod_database_code               2207105
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, -y, -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_occupancy
_atom_site_type_symbol
Mn 0.5000 0.5000 0.5000 0.03063(18) Uani d S 1 Mn
Cl 0.81455(9) 0.06236(10) 0.32135(10) 0.0601(3) Uani d . 1 Cl
N1 0.6664(3) 0.0410(3) 0.8491(3) 0.0384(6) Uani d . 1 N
N2 0.6603(3) 0.3259(3) 1.0453(3) 0.0369(5) Uani d . 1 N
N3 0.6652(2) 0.2412(3) 0.7604(3) 0.0357(5) Uani d . 1 N
N4 0.8857(2) 0.2548(3) 0.9556(3) 0.0390(6) Uani d . 1 N
O1 0.6255(2) 0.5573(2) 0.3598(2) 0.0462(5) Uani d . 1 O
H1C 0.7148 0.6405 0.4000 0.069 Uiso d R 1 H
H1D 0.6341 0.4855 0.2575 0.069 Uiso d R 1 H
O2 0.6263(2) 0.7040(2) 0.7362(2) 0.0504(6) Uani d . 1 O
H2C 0.6201 0.8057 0.7599 0.076 Uiso d R 1 H
H2D 0.6795 0.7012 0.8204 0.076 Uiso d R 1 H
O3 0.6372(2) 0.3333(3) 0.5208(2) 0.0545(6) Uani d . 1 O
H3C 0.6914 0.2776 0.4647 0.082 Uiso d R 1 H
H3D 0.6393 0.2991 0.5866 0.082 Uiso d R 1 H
O4 0.8039(2) 0.7197(2) 1.0046(2) 0.0502(5) Uani d . 1 O
H4C 0.7856 0.8207 1.0842 0.075 Uiso d R 1 H
H4D 0.8979 0.7228 1.0016 0.075 Uiso d R 1 H
O5 0.8512(3) 0.8047(3) 0.4465(3) 0.0850(9) Uani d . 1 O
H5C 0.8409 0.8754 0.4055 0.127 Uiso d R 1 H
H5D 0.9363 0.8478 0.5201 0.127 Uiso d R 1 H
C1 0.6090(3) 0.1522(3) 0.9890(3) 0.0400(7) Uani d . 1 C
H1A 0.6415 0.1349 1.0812 0.048 Uiso calc R 1 H
H1B 0.5012 0.1265 0.9551 0.048 Uiso calc R 1 H
C2 0.6077(3) 0.3474(3) 0.9030(3) 0.0398(7) Uani d . 1 C
H2A 0.6394 0.4613 0.9371 0.048 Uiso calc R 1 H
H2B 0.4998 0.3220 0.8690 0.048 Uiso calc R 1 H
C3 0.6145(3) 0.0698(3) 0.7107(3) 0.0400(7) Uani d . 1 C
H3A 0.6517 -0.0022 0.6169 0.048 Uiso calc R 1 H
H3B 0.5067 0.0431 0.6750 0.048 Uiso calc R 1 H
C4 0.8232(3) 0.3615(4) 1.0938(3) 0.0428(7) Uani d . 1 C
H4A 0.8583 0.3464 1.1871 0.051 Uiso calc R 1 H
H4B 0.8584 0.4754 1.1303 0.051 Uiso calc R 1 H
C5 0.8291(3) 0.0828(3) 0.9014(4) 0.0438(7) Uani d . 1 C
H5A 0.8680 0.0107 0.8092 0.053 Uiso calc R 1 H
H5B 0.8647 0.0646 0.9924 0.053 Uiso calc R 1 H
C6 0.8291(3) 0.2793(4) 0.8161(3) 0.0425(7) Uani d . 1 C
H6A 0.8685 0.2097 0.7233 0.051 Uiso calc R 1 H
H6B 0.8641 0.3926 0.8502 0.051 Uiso calc R 1 H
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_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle
O2 Mn O2 2_666 . 180.0
O2 Mn O1 2_666 . 86.17(8)
O2 Mn O1 . . 93.83(8)
O2 Mn O1 2_666 2_666 93.83(8)
O2 Mn O1 . 2_666 86.17(8)
O1 Mn O1 . 2_666 180.0000(10)
O2 Mn O3 2_666 . 87.53(8)
O2 Mn O3 . . 92.47(8)
O1 Mn O3 . . 94.45(8)
O1 Mn O3 2_666 . 85.55(8)
O2 Mn O3 2_666 2_666 92.47(8)
O2 Mn O3 . 2_666 87.53(8)
O1 Mn O3 . 2_666 85.55(8)
O1 Mn O3 2_666 2_666 94.45(8)
O3 Mn O3 . 2_666 180.0000(10)
C5 N1 C1 . . 108.6(2)
C5 N1 C3 . . 108.3(2)
C1 N1 C3 . . 107.9(2)
C4 N2 C2 . . 108.9(2)
C4 N2 C1 . . 108.3(2)
C2 N2 C1 . . 107.6(2)
C3 N3 C2 . . 108.1(2)
C3 N3 C6 . . 108.2(2)
C2 N3 C6 . . 108.3(2)
C6 N4 C5 . . 108.0(2)
C6 N4 C4 . . 107.7(2)
C5 N4 C4 . . 108.0(2)
Mn O1 H1C . . 129.5
Mn O1 H1D . . 125.6
H1C O1 H1D . . 100.1
Mn O2 H2C . . 119.3
Mn O2 H2D . . 127.6
H2C O2 H2D . . 112.8
Mn O3 H3C . . 133.5
Mn O3 H3D . . 126.1
H3C O3 H3D . . 100.0
H4C O4 H4D . . 113.3
H5C O5 H5D . . 103.6
N1 C1 N2 . . 111.9(2)
N1 C1 H1A . . 109.2
N2 C1 H1A . . 109.2
N1 C1 H1B . . 109.2
N2 C1 H1B . . 109.2
H1A C1 H1B . . 107.9
N2 C2 N3 . . 111.8(2)
N2 C2 H2A . . 109.2
N3 C2 H2A . . 109.2
N2 C2 H2B . . 109.2
N3 C2 H2B . . 109.2
H2A C2 H2B . . 107.9
N3 C3 N1 . . 111.7(2)
N3 C3 H3A . . 109.3
N1 C3 H3A . . 109.3
N3 C3 H3B . . 109.3
N1 C3 H3B . . 109.3
H3A C3 H3B . . 107.9
N2 C4 N4 . . 112.2(2)
N2 C4 H4A . . 109.2
N4 C4 H4A . . 109.2
N2 C4 H4B . . 109.2
N4 C4 H4B . . 109.2
H4A C4 H4B . . 107.9
N1 C5 N4 . . 112.2(2)
N1 C5 H5A . . 109.2
N4 C5 H5A . . 109.2
N1 C5 H5B . . 109.2
N4 C5 H5B . . 109.2
H5A C5 H5B . . 107.9
N4 C6 N3 . . 112.3(2)
N4 C6 H6A . . 109.1
N3 C6 H6A . . 109.1
N4 C6 H6B . . 109.1
N3 C6 H6B . . 109.1
H6A C6 H6B . . 107.9
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_site_symmetry_2
_geom_bond_distance
_geom_bond_publ_flag
Mn O1 . 2.1642(17) y
Mn O1 2_666 2.1642(17) ?
Mn O2 2_666 2.1421(18) ?
Mn O2 . 2.1421(18) y
Mn O3 . 2.1707(19) y
Mn O3 2_666 2.1707(19) ?
N1 C5 . 1.464(4) ?
N1 C1 . 1.467(3) ?
N1 C3 . 1.478(3) ?
N2 C4 . 1.465(4) ?
N2 C2 . 1.470(3) ?
N2 C1 . 1.473(3) ?
N3 C3 . 1.469(3) ?
N3 C2 . 1.471(3) ?
N3 C6 . 1.475(3) ?
N4 C6 . 1.470(3) ?
N4 C5 . 1.473(4) ?
N4 C4 . 1.475(3) ?
O1 H1C . 0.9771 ?
O1 H1D . 0.8988 ?
O2 H2C . 0.8899 ?
O2 H2D . 0.8730 ?
O3 H3C . 0.8292 ?
O3 H3D . 0.8358 ?
O4 H4C . 0.9419 ?
O4 H4D . 0.8823 ?
O5 H5C . 0.9338 ?
O5 H5D . 0.8656 ?
C1 H1A . 0.9700 ?
C1 H1B . 0.9700 ?
C2 H2A . 0.9700 ?
C2 H2B . 0.9700 ?
C3 H3A . 0.9700 ?
C3 H3B . 0.9700 ?
C4 H4A . 0.9700 ?
C4 H4B . 0.9700 ?
C5 H5A . 0.9700 ?
C5 H5B . 0.9700 ?
C6 H6A . 0.9700 ?
C6 H6B . 0.9700 ?
loop_
_geom_hbond_atom_site_label_D
_geom_hbond_atom_site_label_H
_geom_hbond_atom_site_label_A
_geom_hbond_site_symmetry_A
_geom_hbond_distance_DH
_geom_hbond_distance_HA
_geom_hbond_distance_DA
_geom_hbond_angle_DHA
_geom_hbond_publ_flag
O1 H1C O5 . 0.98 1.75 2.717(4) 167 y
O1 H1D N2 1_554 0.90 1.92 2.817(3) 176 y
O2 H2C N1 1_565 0.89 1.94 2.808(4) 163 y
O2 H2D O4 . 0.87 1.83 2.700(3) 173 y
O3 H3C Cl . 0.83 2.36 3.165(3) 163 y
O3 H3D N3 . 0.84 1.97 2.800(4) 173 y
O4 H4C Cl 1_566 0.94 2.25 3.151(2) 161 y
O4 H4D N4 2_767 0.88 1.96 2.827(3) 168 y
O5 H5C Cl 1_565 0.93 2.30 3.228(3) 176 y
O5 H5D Cl 2_766 0.87 2.35 3.205(3) 170 y
loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
C5 N1 C1 N2 58.1(3)
C3 N1 C1 N2 -59.1(3)
C4 N2 C1 N1 -58.1(3)
C2 N2 C1 N1 59.4(3)
C4 N2 C2 N3 57.9(3)
C1 N2 C2 N3 -59.4(3)
C3 N3 C2 N2 59.4(3)
C6 N3 C2 N2 -57.6(3)
C2 N3 C3 N1 -58.8(3)
C6 N3 C3 N1 58.3(3)
C5 N1 C3 N3 -58.7(3)
C1 N1 C3 N3 58.7(3)
C2 N2 C4 N4 -58.3(3)
C1 N2 C4 N4 58.4(3)
C6 N4 C4 N2 58.3(3)
C5 N4 C4 N2 -58.2(3)
C1 N1 C5 N4 -58.2(3)
C3 N1 C5 N4 58.8(3)
C6 N4 C5 N1 -58.3(3)
C4 N4 C5 N1 58.0(3)
C5 N4 C6 N3 57.9(3)
C4 N4 C6 N3 -58.5(3)
C3 N3 C6 N4 -58.3(3)
C2 N3 C6 N4 58.6(3)
