#------------------------------------------------------------------------------
#$Date: 2019-12-26 19:55:02 +0200 (Thu, 26 Dec 2019) $
#$Revision: 246019 $
#$URL: file:///home/coder/svn-repositories/cod/cif/2/31/16/2311604.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_2311604
loop_
_publ_author_name
'Talley, Allison'
'Kelley, Annette F.'
'Bond, Marcus R.'
_publ_section_title
;
 Poly[tetrakis(n-propylammonium)
 [octa-μ-chlorido-dichloridotrinickelate(II)]]: a hybrid
 organic-inorganic layer compound in the Cs4Mg3F10 structure type.
;
_journal_coeditor_code           FG3235
_journal_issue                   'Pt 12'
_journal_name_full
'Acta crystallographica. Section C, Crystal structure communications'
_journal_page_first              m395
_journal_page_last               9
_journal_paper_doi               10.1107/S0108270111050116
_journal_volume                  67
_journal_year                    2011
_chemical_formula_iupac          '(C3 H10 N)4 [Ni3 Cl10]'
_chemical_formula_moiety         '4(C3 H10 N +), Cl10 Ni3 4-'
_chemical_formula_sum            'C12 H40 Cl10 N4 Ni3'
_chemical_formula_weight         771.09
_chemical_name_systematic
;
Poly[tetrakis(n-propylammonium)
[octa-μ-chlorido-dichloridotrinickelate(II)]]
;
_space_group_crystal_system      orthorhombic
_space_group_IT_number           64
_space_group_name_Hall           '-C 2ac 2'
_space_group_name_H-M_alt        'C m c e'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_conform_dict_name         cif_core.dic
_audit_conform_dict_version      2.4
_audit_creation_method           'WinGX routine CIF_UPDATE'
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   6.91320(10)
_cell_length_b                   23.9825(2)
_cell_length_c                   17.3695(2)
_cell_measurement_reflns_used    4076
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      37.036
_cell_measurement_theta_min      0.998
_cell_volume                     2879.79(6)
_computing_cell_refinement       'SCALEPACK (Otwinowski & Minor, 1997)'
_computing_data_collection       'COLLECT (Nonius, 1998)'
_computing_data_reduction
'DENZO and SCALEPACK (Otwinowski & Minor, 1997)'
_computing_molecular_graphics    'ORTEP-3 for Windows (Farrugia, 1997)'
_computing_publication_material  'WinGX (Farrugia, 1999)'
_computing_structure_refinement  'SHELXL97 (Sheldrick, 2008)'
_computing_structure_solution    'SIR92 (Altomare et al., 1993)'
_diffrn_ambient_temperature      100(2)
_diffrn_detector_area_resol_mean 9
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device       '95mm CCD camera on κ-goniostat'
_diffrn_measurement_device_type  'Nonius KappaCCD area-detector'
_diffrn_measurement_method       CCD
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.043
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       0
_diffrn_reflns_limit_k_max       40
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       29
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_number            3904
_diffrn_reflns_theta_full        36.98
_diffrn_reflns_theta_max         36.98
_diffrn_reflns_theta_min         3.4
_exptl_absorpt_coefficient_mu    2.88
_exptl_absorpt_correction_T_max  0.638
_exptl_absorpt_correction_T_min  0.527
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
'(DENZO and SCALEPACK; Otwinowski & Minor, 1997)'
_exptl_crystal_colour            orange
_exptl_crystal_density_diffrn    1.778
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             1576
_exptl_crystal_size_max          0.25
_exptl_crystal_size_mid          0.19
_exptl_crystal_size_min          0.16
_refine_diff_density_max         0.703
_refine_diff_density_min         -1.100
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.034
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     85
_refine_ls_number_reflns         3904
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.034
_refine_ls_R_factor_all          0.0292
_refine_ls_R_factor_gt           0.0231
_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)+(0.0190P)²+4.7563P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0531
_refine_ls_wR_factor_ref         0.0558
_reflns_number_gt                3435
_reflns_number_total             3904
_reflns_threshold_expression     I>2σ(I)
_cod_data_source_file            fg3235sup1.cif
_cod_data_source_block           I_100K
_cod_original_sg_symbol_Hall     '-C 2bc 2'
_cod_database_code               2311604
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x+1/2, -y, z+1/2'
'x, -y, -z'
'-x+1/2, y, -z+1/2'
'x+1/2, y+1/2, z'
'-x+1, -y+1/2, z+1/2'
'x+1/2, -y+1/2, -z'
'-x+1, y+1/2, -z+1/2'
'-x, -y, -z'
'x-1/2, y, -z-1/2'
'-x, y, z'
'x-1/2, -y, z-1/2'
'-x+1/2, -y+1/2, -z'
'x, y+1/2, -z-1/2'
'-x+1/2, y+1/2, z'
'x, -y+1/2, z-1/2'
loop_
_atom_site_type_symbol
_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_symmetry_multiplicity
Ni Ni1 0.0000 0.437029(7) 0.150913(10) 0.01063(4) Uani d S 1 2
Ni Ni2 0.0000 0.5000 0.0000 0.00910(5) Uani d S 1 4
Cl Cl1 0.0000 0.340258(14) 0.16434(2) 0.01974(7) Uani d S 1 2
Cl Cl2 0.2500 0.450502(14) 0.2500 0.01337(6) Uani d S 1 2
Cl Cl3 0.0000 0.536300(13) 0.127854(18) 0.01294(6) Uani d S 1 2
Cl Cl4 0.23670(3) 0.434124(9) 0.046224(13) 0.01319(4) Uani d . 1 1
N N11 0.0000 0.34717(5) 0.34565(7) 0.0158(2) Uani d S 1 2
H H11A 0.0000 0.3555 0.2957 0.024 Uiso calc SR 1 2
H H11B 0.1051 0.3614 0.3677 0.024 Uiso calc PR 0.50 1
H H11C -0.1051 0.3614 0.3677 0.024 Uiso calc PR 0.50 1
C C12 0.0000 0.28585(7) 0.35532(10) 0.0303(4) Uani d S 1 2
H H12A 0.1134 0.2705 0.3301 0.045 Uiso calc PR 0.50 1
H H12B -0.1134 0.2705 0.3301 0.045 Uiso calc PR 0.50 1
C C13 0.0000 0.26829(9) 0.43810(11) 0.0302(4) Uani d S 1 2
H H13A -0.1135 0.2835 0.4634 0.045 Uiso calc PR 0.50 1
H H13B 0.1135 0.2835 0.4634 0.045 Uiso calc PR 0.50 1
C C14 0.0000 0.20519(10) 0.44665(16) 0.0471(7) Uani d S 1 2
H H14A 0.0000 0.1956 0.5003 0.071 Uiso calc SPR 0.50 2
H H14B 0.1134 0.1901 0.4225 0.071 Uiso calc PR 0.25 1
H H14C -0.1134 0.1901 0.4225 0.071 Uiso calc PR 0.25 1
H H14D 0.0000 0.1882 0.3966 0.071 Uiso calc SPR 0.50 2
H H14E -0.1134 0.1938 0.4744 0.071 Uiso calc PR 0.25 1
H H14F 0.1134 0.1938 0.4744 0.071 Uiso calc PR 0.25 1
N N21 0.5000 0.53121(5) 0.12649(8) 0.0192(2) Uani d S 1 2
H H21A 0.5000 0.5019 0.1579 0.029 Uiso calc SPR 0.50 2
H H21B 0.6051 0.5303 0.0969 0.029 Uiso calc PR 0.25 1
H H21C 0.3949 0.5303 0.0969 0.029 Uiso calc PR 0.25 1
H H21D 0.5000 0.5397 0.0766 0.029 Uiso calc SPR 0.50 2
H H21E 0.3949 0.5113 0.1376 0.029 Uiso calc PR 0.25 1
H H21F 0.6051 0.5113 0.1376 0.029 Uiso calc PR 0.25 1
C C22 0.5000 0.58316(8) 0.17255(10) 0.0272(4) Uani d S 1 2
H H22A 0.3866 0.5837 0.2054 0.041 Uiso calc PR 0.50 1
H H22B 0.6134 0.5837 0.2054 0.041 Uiso calc PR 0.50 1
C C23 0.5000 0.63269(9) 0.12407(15) 0.0597(10) Uani d S 1 2
H H23A 0.3865 0.6322 0.0912 0.090 Uiso calc PR 0.50 1
H H23B 0.6135 0.6322 0.0912 0.090 Uiso calc PR 0.50 1
C C24 0.5000 0.68647(10) 0.1726(2) 0.0647(10) Uani d S 1 2
H H24A 0.5000 0.7183 0.1391 0.097 Uiso calc SPR 0.50 2
H H24B 0.6134 0.6873 0.2045 0.097 Uiso calc PR 0.25 1
H H24C 0.3866 0.6873 0.2045 0.097 Uiso calc PR 0.25 1
H H24D 0.5000 0.6770 0.2263 0.097 Uiso calc SPR 0.50 2
H H24E 0.3866 0.7080 0.1609 0.097 Uiso calc PR 0.25 1
H H24F 0.6134 0.7080 0.1609 0.097 Uiso calc PR 0.25 1
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.003 0.002 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0 0 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Cl Cl 0.148 0.159 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.006 0.003 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Ni Ni 0.339 1.112 '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_3
_geom_angle
_geom_angle_publ_flag
Cl1 Ni1 Cl2 . 93.482(11) y
Cl1 Ni1 Cl3 . 176.187(14) y
Cl1 Ni1 Cl4 . 92.633(10) y
Cl2 Ni1 Cl2 11 89.247(6) y
Cl2 Ni1 Cl3 . 89.230(10) y
Cl2 Ni1 Cl4 . 93.084(6) y
Cl2 Ni1 Cl4 11 173.311(11) y
Cl3 Ni1 Cl4 . 84.537(9) y
Cl4 Ni1 Cl4 11 83.927(12) y
Cl3 Ni2 Cl4 . 85.937(8) y
Cl4 Ni2 Cl4 3_565 94.563(12) y
Ni1 Cl2 Ni1 10_656 164.908(17) y
Ni2 Cl3 Ni1 . 78.144(10) y
Ni2 Cl4 Ni1 . 77.001(8) y
C12 N11 H11A . 109.5 ?
C12 N11 H11B . 109.5 ?
H11A N11 H11B . 109.5 ?
C12 N11 H11C . 109.5 ?
H11A N11 H11C . 109.5 ?
H11B N11 H11C . 109.5 ?
N11 C12 C13 . 112.85(15) ?
N11 C12 H12A . 109.0 ?
C13 C12 H12A . 109.0 ?
N11 C12 H12B . 109.0 ?
C13 C12 H12B . 109.0 ?
H12A C12 H12B . 107.8 ?
C12 C13 C14 . 111.94(18) ?
C12 C13 H13A . 109.2 ?
C14 C13 H13A . 109.2 ?
C12 C13 H13B . 109.2 ?
C14 C13 H13B . 109.2 ?
H13A C13 H13B . 107.9 ?
C13 C14 H14A . 109.5 ?
C13 C14 H14B . 109.5 ?
H14A C14 H14B . 109.5 ?
C13 C14 H14C . 109.5 ?
H14A C14 H14C . 109.5 ?
H14B C14 H14C . 109.5 ?
C13 C14 H14D . 109.5 ?
C13 C14 H14E . 109.5 ?
H14D C14 H14E . 109.5 ?
C13 C14 H14F . 109.5 ?
H14D C14 H14F . 109.5 ?
H14E C14 H14F . 109.5 ?
C22 N21 H21A . 109.5 ?
C22 N21 H21B . 109.5 ?
H21A N21 H21B . 109.5 ?
C22 N21 H21C . 109.5 ?
H21A N21 H21C . 109.5 ?
H21B N21 H21C . 109.5 ?
C22 N21 H21D . 109.5 ?
C22 N21 H21E . 109.5 ?
H21D N21 H21E . 109.5 ?
C22 N21 H21F . 109.5 ?
H21D N21 H21F . 109.5 ?
H21E N21 H21F . 109.5 ?
C23 C22 N21 . 111.96(16) ?
C23 C22 H22A . 109.2 ?
N21 C22 H22A . 109.2 ?
C23 C22 H22B . 109.2 ?
N21 C22 H22B . 109.2 ?
H22A C22 H22B . 107.9 ?
C22 C23 C24 . 111.5(2) ?
C22 C23 H23A . 109.3 ?
C24 C23 H23A . 109.3 ?
C22 C23 H23B . 109.3 ?
C24 C23 H23B . 109.3 ?
H23A C23 H23B . 108.0 ?
C23 C24 H24A . 109.5 ?
C23 C24 H24B . 109.5 ?
H24A C24 H24B . 109.5 ?
C23 C24 H24C . 109.5 ?
H24A C24 H24C . 109.5 ?
H24B C24 H24C . 109.5 ?
C23 C24 H24D . 109.5 ?
C23 C24 H24E . 109.5 ?
H24D C24 H24E . 109.5 ?
C23 C24 H24F . 109.5 ?
H24D C24 H24F . 109.5 ?
H24E C24 H24F . 109.5 ?
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_publ_flag
Ni1 Cl1 2.3325(4) y
Ni1 Cl2 2.46040(13) y
Ni1 Cl3 2.4142(4) y
Ni1 Cl4 2.4473(3) y
Ni2 Cl3 2.3853(3) y
Ni2 Cl4 2.4121(2) y
N11 C12 1.480(2) ?
N11 H11A 0.8900 ?
N11 H11B 0.8900 ?
N11 H11C 0.8900 ?
C12 C13 1.498(2) ?
C12 H12A 0.9700 ?
C12 H12B 0.9700 ?
C13 C14 1.520(3) ?
C13 H13A 0.9700 ?
C13 H13B 0.9700 ?
C14 H14A 0.9600 ?
C14 H14B 0.9600 ?
C14 H14C 0.9600 ?
C14 H14D 0.9600 ?
C14 H14E 0.9600 ?
C14 H14F 0.9600 ?
N21 C22 1.481(2) ?
N21 H21A 0.8900 ?
N21 H21B 0.8900 ?
N21 H21C 0.8900 ?
N21 H21D 0.8900 ?
N21 H21E 0.8900 ?
N21 H21F 0.8900 ?
C22 C23 1.456(3) ?
C22 H22A 0.9700 ?
C22 H22B 0.9700 ?
C23 C24 1.541(3) ?
C23 H23A 0.9700 ?
C23 H23B 0.9700 ?
C24 H24A 0.9600 ?
C24 H24B 0.9600 ?
C24 H24C 0.9600 ?
C24 H24D 0.9600 ?
C24 H24E 0.9600 ?
C24 H24F 0.9600 ?
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
N11 H11A Cl1 1_555 0.890 2.311 3.1536(13) 157.96 yes
N11 H11B Cl4 4_555 0.890 2.543 3.3451(10) 150.19 yes
