#------------------------------------------------------------------------------
#$Date: 2016-02-20 05:06:23 +0200 (Sat, 20 Feb 2016) $
#$Revision: 176774 $
#$URL: svn://www.crystallography.net/cod/cif/2/20/27/2202706.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_2202706
loop_
_publ_author_name
'Zhu, Hai-Liang'
'You, Zhong-Lu'
'Qu, Yang'
'Liu, Wei-Sheng'
'Tan, Min-Yu'
'Ma, Ji-Long'
_publ_section_title
;
 Hexaaquanickel(II) dichloride bis(hexamethylenetetramine) tetrahydrate
;
_journal_issue                   10
_journal_name_full               'Acta Crystallographica Section E'
_journal_page_first              m924
_journal_page_last               m925
_journal_paper_doi               10.1107/S1600536803020269
_journal_volume                  59
_journal_year                    2003
_chemical_formula_iupac          '[Ni (H2 O)6] Cl2, 2C6 H12 N4, 4H2 O'
_chemical_formula_moiety         'H12 Ni O6 2+, Cl2 1-, 2C6 H12 N4, 4H2 O'
_chemical_formula_sum            'C12 H44 Cl2 N8 Ni O10'
_chemical_formula_weight         590.14
_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                119.551(7)
_cell_angle_beta                 94.192(8)
_cell_angle_gamma                100.990(8)
_cell_formula_units_Z            1
_cell_length_a                   9.330(6)
_cell_length_b                   9.411(6)
_cell_length_c                   9.446(6)
_cell_measurement_reflns_used    2777
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      26.3
_cell_measurement_theta_min      2.5
_cell_volume                     694.6(8)
_computing_cell_refinement       SMART
_computing_data_collection       'SMART (Siemens, 1996)'
_computing_data_reduction        'SAINT (Siemens, 1996)'
_computing_molecular_graphics    'SHELXTL (Sheldrick, 1997b)'
_computing_publication_material  SHELXTL
_computing_structure_refinement  'SHELXL97 (Sheldrick, 1997a)'
_computing_structure_solution    'SHELXS97 (Sheldrick, 1997a)'
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 0.983
_diffrn_measured_fraction_theta_max 0.983
_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  0.0196
_diffrn_reflns_av_sigmaI/netI    0.0239
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_k_min       -10
_diffrn_reflns_limit_l_max       10
_diffrn_reflns_limit_l_min       -11
_diffrn_reflns_number            3644
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         25.02
_diffrn_reflns_theta_min         2.27
_diffrn_standards_decay_%        0
_diffrn_standards_interval_count 0
_diffrn_standards_interval_time  0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.946
_exptl_absorpt_correction_T_max  0.8481
_exptl_absorpt_correction_T_min  0.6700
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   '(SADABS; Sheldrick, 1996)'
_exptl_crystal_colour            blue
_exptl_crystal_density_diffrn    1.411
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             314
_exptl_crystal_size_max          0.46
_exptl_crystal_size_mid          0.32
_exptl_crystal_size_min          0.18
_refine_diff_density_max         0.351
_refine_diff_density_min         -0.492
_refine_ls_extinction_coef       0.059(5)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4^
_refine_ls_extinction_method     'SHELXTL (Sheldrick, 1997)'
_refine_ls_goodness_of_fit_ref   1.049
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     204
_refine_ls_number_reflns         2418
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.049
_refine_ls_R_factor_all          0.0338
_refine_ls_R_factor_gt           0.0308
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w = 1/[σ²(Fo²)+(0.0606P)²+0.0662P] where P = (Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0860
_refine_ls_wR_factor_ref         0.0887
_reflns_number_gt                2216
_reflns_number_total             2418
_reflns_threshold_expression     I>2σ(I)
_cod_data_source_file            lh6108.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_database_code               2202706
_cod_database_fobs_code          2202706
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_disorder_assembly
_atom_site_disorder_group
_atom_site_type_symbol
Ni1 0.5000 0.5000 0.5000 0.02892(16) Uani d S 1 . . Ni
O1 0.3831(2) 0.6342(2) 0.4429(2) 0.0450(4) Uani d . 1 . . O
H1 0.380(3) 0.723(4) 0.510(4) 0.053(8) Uiso d . 1 . . H
H2 0.305(3) 0.595(3) 0.369(4) 0.059(8) Uiso d . 1 . . H
O2 0.6415(2) 0.5275(2) 0.3532(2) 0.0520(4) Uani d . 1 . . O
H3 0.632(4) 0.579(4) 0.314(4) 0.076(10) Uiso d . 1 . . H
H4 0.684(4) 0.456(4) 0.288(4) 0.080(10) Uiso d . 1 . . H
O3 0.6186(2) 0.7235(2) 0.69897(19) 0.0515(4) Uani d . 1 . . O
H5 0.613(3) 0.746(4) 0.797(4) 0.065(8) Uiso d . 1 . . H
H6 0.671(3) 0.790(4) 0.699(4) 0.059(9) Uiso d . 1 . . H
N1 0.6580(2) 1.0478(2) 0.3272(2) 0.0379(4) Uani d . 1 . . N
N2 0.6660(2) 0.7597(2) 0.2449(2) 0.0391(4) Uani d . 1 . . N
N3 0.88469(19) 0.9576(2) 0.2560(2) 0.0402(4) Uani d . 1 . . N
N4 0.6640(2) 0.8457(2) 0.0398(2) 0.0390(4) Uani d . 1 . . N
C1 0.6077(2) 0.9045(3) 0.3516(3) 0.0411(5) Uani d . 1 . . C
H11 0.4998 0.8690 0.3268 0.041(6) Uiso calc R 1 . . H
H12 0.6407 0.9410 0.4669 0.049(6) Uiso calc R 1 . . H
C2 0.8220(2) 1.0986(3) 0.3625(3) 0.0435(5) Uani d . 1 . . C
H13 0.8582 1.1379 0.4780 0.055(7) Uiso calc R 1 . . H
H14 0.8561 1.1918 0.3451 0.044(6) Uiso calc R 1 . . H
C3 0.6057(2) 0.9880(3) 0.1507(3) 0.0403(5) Uani d . 1 . . C
H15 0.4977 0.9528 0.1249 0.041(6) Uiso calc R 1 . . H
H16 0.6374 1.0805 0.1317 0.036(5) Uiso calc R 1 . . H
C4 0.8296(2) 0.8163(3) 0.2823(3) 0.0433(5) Uani d . 1 . . C
H17 0.8691 0.7222 0.2120 0.048(6) Uiso calc R 1 . . H
H18 0.8656 0.8519 0.3968 0.038(6) Uiso calc R 1 . . H
C5 0.8272(2) 0.9006(3) 0.0816(3) 0.0435(5) Uani d . 1 . . C
H19 0.8614 0.9925 0.0623 0.046(6) Uiso calc R 1 . . H
H20 0.8668 0.8075 0.0093 0.042(6) Uiso calc R 1 . . H
C6 0.6137(2) 0.7066(3) 0.0710(3) 0.0410(5) Uani d . 1 . . C
H21 0.5057 0.6698 0.0448 0.045(6) Uiso calc R 1 . . H
H22 0.6510 0.6113 -0.0013 0.050(6) Uiso calc R 1 . . H
Cl1 0.81052(7) 0.32527(8) 0.06497(8) 0.0593(2) Uani d . 1 . . Cl
O4 0.1488(3) 0.5523(4) 0.2005(3) 0.0813(7) Uani d . 1 . . O
H7 0.165(5) 0.585(5) 0.129(6) 0.114(15) Uiso d . 1 . . H
H8 0.068(5) 0.496(6) 0.174(5) 0.106(16) Uiso d . 1 . . H
O5 0.8033(2) 0.9976(2) 0.7221(2) 0.0518(4) Uani d . 1 . . O
H9 0.889(4) 1.002(4) 0.732(4) 0.061(9) Uiso d . 1 . . H
H10 0.800(4) 1.078(5) 0.812(5) 0.089(12) Uiso d . 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'
Cl Cl 0.1484 0.1585 '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'
Ni Ni 0.3393 1.1124 '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'
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
_geom_angle_publ_flag
O3 Ni1 O3 2_666 . 180.0000(10) ?
O3 Ni1 O1 2_666 . 92.61(9) ?
O3 Ni1 O1 . . 87.39(9) y
O3 Ni1 O1 2_666 2_666 87.39(9) ?
O3 Ni1 O1 . 2_666 92.61(9) y
O1 Ni1 O1 . 2_666 180.0000(10) ?
O3 Ni1 O2 2_666 . 89.24(9) ?
O3 Ni1 O2 . . 90.76(9) y
O1 Ni1 O2 . . 86.66(8) y
O1 Ni1 O2 2_666 . 93.34(8) ?
O3 Ni1 O2 2_666 2_666 90.76(9) ?
O3 Ni1 O2 . 2_666 89.24(9) y
O1 Ni1 O2 . 2_666 93.34(8) y
O1 Ni1 O2 2_666 2_666 86.66(8) ?
O2 Ni1 O2 . 2_666 180.0000(10) ?
Ni1 O1 H1 . . 121(2) ?
Ni1 O1 H2 . . 127.3(18) ?
H1 O1 H2 . . 106(3) ?
Ni1 O2 H3 . . 121(3) ?
Ni1 O2 H4 . . 127(2) ?
H3 O2 H4 . . 104(3) ?
Ni1 O3 H5 . . 121(2) ?
Ni1 O3 H6 . . 127(2) ?
H5 O3 H6 . . 112(3) ?
C2 N1 C1 . . 108.67(15) ?
C2 N1 C3 . . 108.16(17) ?
C1 N1 C3 . . 107.79(16) ?
C4 N2 C6 . . 108.33(16) ?
C4 N2 C1 . . 108.53(17) ?
C6 N2 C1 . . 108.04(16) ?
C5 N3 C2 . . 107.84(17) ?
C5 N3 C4 . . 108.05(16) ?
C2 N3 C4 . . 108.34(17) ?
C5 N4 C3 . . 108.55(16) ?
C5 N4 C6 . . 108.52(16) ?
C3 N4 C6 . . 108.11(17) ?
N1 C1 N2 . . 111.89(16) ?
N1 C1 H11 . . 109.2 ?
N2 C1 H11 . . 109.2 ?
N1 C1 H12 . . 109.2 ?
N2 C1 H12 . . 109.2 ?
H11 C1 H12 . . 107.9 ?
N1 C2 N3 . . 111.96(16) ?
N1 C2 H13 . . 109.2 ?
N3 C2 H13 . . 109.2 ?
N1 C2 H14 . . 109.2 ?
N3 C2 H14 . . 109.2 ?
H13 C2 H14 . . 107.9 ?
N4 C3 N1 . . 111.71(16) ?
N4 C3 H15 . . 109.3 ?
N1 C3 H15 . . 109.3 ?
N4 C3 H16 . . 109.3 ?
N1 C3 H16 . . 109.3 ?
H15 C3 H16 . . 107.9 ?
N2 C4 N3 . . 112.02(16) ?
N2 C4 H17 . . 109.2 ?
N3 C4 H17 . . 109.2 ?
N2 C4 H18 . . 109.2 ?
N3 C4 H18 . . 109.2 ?
H17 C4 H18 . . 107.9 ?
N4 C5 N3 . . 112.04(16) ?
N4 C5 H19 . . 109.2 ?
N3 C5 H19 . . 109.2 ?
N4 C5 H20 . . 109.2 ?
N3 C5 H20 . . 109.2 ?
H19 C5 H20 . . 107.9 ?
N2 C6 N4 . . 111.60(16) ?
N2 C6 H21 . . 109.3 ?
N4 C6 H21 . . 109.3 ?
N2 C6 H22 . . 109.3 ?
N4 C6 H22 . . 109.3 ?
H21 C6 H22 . . 108.0 ?
H7 O4 H8 . . 109(4) ?
H9 O5 H10 . . 102(3) ?
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
Ni1 O3 2_666 2.0227(18) ?
Ni1 O3 . 2.0227(18) y
Ni1 O1 . 2.0460(17) y
Ni1 O1 2_666 2.0460(17) ?
Ni1 O2 . 2.0554(18) y
Ni1 O2 2_666 2.0554(18) ?
O1 H1 . 0.77(3) ?
O1 H2 . 0.85(3) ?
O2 H3 . 0.76(4) ?
O2 H4 . 0.84(4) ?
O3 H5 . 0.85(3) ?
O3 H6 . 0.71(3) ?
N1 C2 . 1.474(3) ?
N1 C1 . 1.474(3) ?
N1 C3 . 1.479(3) ?
N2 C4 . 1.472(3) ?
N2 C6 . 1.472(3) ?
N2 C1 . 1.475(3) ?
N3 C5 . 1.476(3) ?
N3 C2 . 1.476(3) ?
N3 C4 . 1.476(3) ?
N4 C5 . 1.467(3) ?
N4 C3 . 1.471(3) ?
N4 C6 . 1.478(3) ?
C1 H11 . 0.9700 ?
C1 H12 . 0.9700 ?
C2 H13 . 0.9700 ?
C2 H14 . 0.9700 ?
C3 H15 . 0.9700 ?
C3 H16 . 0.9700 ?
C4 H17 . 0.9700 ?
C4 H18 . 0.9700 ?
C5 H19 . 0.9700 ?
C5 H20 . 0.9700 ?
C6 H21 . 0.9700 ?
C6 H22 . 0.9700 ?
O4 H7 . 0.88(5) ?
O4 H8 . 0.77(5) ?
O5 H9 . 0.79(3) ?
O5 H10 . 0.82(4) ?
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
O1 H1 N1 2_676 0.77(3) 2.06(3) 2.823(3) 172(3)
O1 H2 O4 . 0.85(3) 1.90(3) 2.739(3) 166(3)
O2 H3 N2 . 0.76(4) 2.08(4) 2.814(3) 164(3)
O2 H4 Cl1 . 0.84(4) 2.39(4) 3.191(2) 158(3)
O3 H5 N4 1_556 0.85(3) 1.98(3) 2.799(3) 161(3)
O3 H6 O5 . 0.71(3) 2.00(3) 2.714(3) 172(3)
O4 H7 Cl1 2_665 0.88(5) 2.37(5) 3.253(3) 176(4)
O4 H8 Cl1 1_455 0.77(5) 2.44(5) 3.210(3) 173(4)
O5 H9 N3 2_776 0.79(3) 2.05(3) 2.838(3) 170(3)
O5 H10 Cl1 1_566 0.82(4) 2.35(4) 3.168(3) 174(3)
