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#$Date: 2016-03-24 02:38:42 +0200 (Thu, 24 Mar 2016) $
#$Revision: 179590 $
#$URL: svn://www.crystallography.net/cod/cif/4/50/55/4505572.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_4505572
loop_
_publ_author_name
'Cepeda, Javier'
'Beobide, Garikoitz'
'Castillo, Oscar'
'Luque, Antonio'
'Pérez-Yáñez, Sonia'
'Román, Pascual'
_publ_contact_author
;
 Oscar Castillo. Departamento de Quimica Inorganica. 
Facultad de Ciencia y Tecnologia
Universidad del Pais Vasco,  Apdo. 644, 
E-48080 Bilbao, Spain
;
_publ_section_title
;
 Structure-Directing Effect of Organic Cations in the Assembly of Anionic
 In(III)/Diazinedicarboxylate Architectures
;
_journal_issue                   3
_journal_name_full               'Crystal Growth & Design'
_journal_page_first              1501
_journal_paper_doi               10.1021/cg201572y
_journal_volume                  12
_journal_year                    2012
_chemical_compound_source        'synthesis as described'
_chemical_formula_moiety         'C12 H4 In N4 O8, C2 H8 N'
_chemical_formula_structural     'C12 H4 In N4 O8, C2 H8 N'
_chemical_formula_sum            'C14 H12 In N5 O8'
_chemical_formula_weight         493.09
_chemical_name_systematic
;
poly-[dimethylammonium (mu-pyridazine-3,6-dicarboxylato)-k2N,O:kO')
indate(III)] 
;
_space_group_IT_number           167
_symmetry_cell_setting           trigonal
_symmetry_Int_Tables_number      167
_symmetry_space_group_name_Hall  '-R 3 2"c'
_symmetry_space_group_name_H-M   'R -3 c :H'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL97
_cell_angle_alpha                90.000
_cell_angle_beta                 90.000
_cell_angle_gamma                120.000
_cell_formula_units_Z            18
_cell_length_a                   15.380(1)
_cell_length_b                   15.380(1)
_cell_length_c                   52.911(1)
_cell_measurement_reflns_used    3523
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      30.00
_cell_measurement_theta_min      2.89
_cell_volume                     10839.0(10)
_computing_cell_refinement       'CrysAlis CCD (Oxford Diffraction, 2003)'
_computing_data_collection       'CrysAlis CCD (Oxford Diffraction, 2003)'
_computing_data_reduction        'CrysAlis RED (Oxford Diffraction, 2003)'
_computing_molecular_graphics    'Ortep-3 (Farrugia, 1997)'
_computing_publication_material  'WinGX (Farrugia, 1999)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'Sir92 (Altomare et al., 1993)'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measurement_device_type  Xcalibur
_diffrn_measurement_method       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  0.0215
_diffrn_reflns_av_sigmaI/netI    0.0175
_diffrn_reflns_limit_h_max       0
_diffrn_reflns_limit_h_min       -18
_diffrn_reflns_limit_k_max       21
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       74
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_number            3523
_diffrn_reflns_theta_full        30.00
_diffrn_reflns_theta_max         30.00
_diffrn_reflns_theta_min         2.89
_diffrn_standards_decay_%        0
_diffrn_standards_interval_count 0
_diffrn_standards_interval_time  0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    1.022
_exptl_absorpt_correction_T_max  0.945
_exptl_absorpt_correction_T_min  0.853
_exptl_absorpt_correction_type   numerical
_exptl_absorpt_process_details
;
CrysAlis RED, Oxford Diffraction Ltd.,
Version 1.170.32 (release 06.06.2003 CrysAlis170 VC++)
(compiled Jun  6 2003,13:53:32)
Analytical numeric absorption correction using a multifaceted crystal
model based on expressions derived by R.C. Clark & J.S. Reid.
;
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.360
_exptl_crystal_description       'trigonal prism'
_exptl_crystal_F_000             4392
_exptl_crystal_size_max          0.45
_exptl_crystal_size_mid          0.34
_exptl_crystal_size_min          0.29
_platon_squeeze_details
;
 The SQUEEZE procedure removes the electron density placed within the 
 channels corresponding to disordered solvent molecules and 0.166667 
 dimethylammonium cations per In atom.
;
_refine_diff_density_max         2.515
_refine_diff_density_min         -0.746
_refine_diff_density_rms         0.147
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.114
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     124
_refine_ls_number_reflns         3523
_refine_ls_number_restraints     3
_refine_ls_restrained_S_all      1.115
_refine_ls_R_factor_all          0.0496
_refine_ls_R_factor_gt           0.0416
_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)+(0.0847P)²+29.5052P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1296
_refine_ls_wR_factor_ref         0.1339
_reflns_number_gt                2963
_reflns_number_total             3523
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            cg201572y_si_002.cif
_cod_data_source_block           Compound5
_cod_original_sg_symbol_H-M      'R -3c'
_cod_database_code               4505572
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-y, x-y, z'
'-x+y, -x, z'
'x-y, -y, -z+1/2'
'-x, -x+y, -z+1/2'
'y, x, -z+1/2'
'x+2/3, y+1/3, z+1/3'
'-y+2/3, x-y+1/3, z+1/3'
'-x+y+2/3, -x+1/3, z+1/3'
'x-y+2/3, -y+1/3, -z+5/6'
'-x+2/3, -x+y+1/3, -z+5/6'
'y+2/3, x+1/3, -z+5/6'
'x+1/3, y+2/3, z+2/3'
'-y+1/3, x-y+2/3, z+2/3'
'-x+y+1/3, -x+2/3, z+2/3'
'x-y+1/3, -y+2/3, -z+7/6'
'-x+1/3, -x+y+2/3, -z+7/6'
'y+1/3, x+2/3, -z+7/6'
'-x, -y, -z'
'y, -x+y, -z'
'x-y, x, -z'
'-x+y, y, z-1/2'
'x, x-y, z-1/2'
'-y, -x, z-1/2'
'-x+2/3, -y+1/3, -z+1/3'
'y+2/3, -x+y+1/3, -z+1/3'
'x-y+2/3, x+1/3, -z+1/3'
'-x+y+2/3, y+1/3, z-1/6'
'x+2/3, x-y+1/3, z-1/6'
'-y+2/3, -x+1/3, z-1/6'
'-x+1/3, -y+2/3, -z+2/3'
'y+1/3, -x+y+2/3, -z+2/3'
'x-y+1/3, x+2/3, -z+2/3'
'-x+y+1/3, y+2/3, z+1/6'
'x+1/3, x-y+2/3, z+1/6'
'-y+1/3, -x+2/3, z+1/6'
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
_atom_site_disorder_assembly
_atom_site_disorder_group
In1 In 0.548878(18) 0.0000 0.2500 0.02232(12) Uani 1 2 d S . .
N11 N 0.57885(18) -0.10694(18) 0.22648(5) 0.0248(5) Uani 1 1 d . . .
N12 N 0.54620(19) -0.20292(18) 0.23292(5) 0.0256(5) Uani 1 1 d . . .
C13 C 0.5631(2) -0.2593(2) 0.21689(6) 0.0289(6) Uani 1 1 d . . .
C14 C 0.6127(3) -0.2233(3) 0.19381(7) 0.0381(8) Uani 1 1 d . . .
H14 H 0.6234 -0.2648 0.1830 0.046 Uiso 1 1 calc R . .
C15 C 0.6453(3) -0.1250(3) 0.18740(7) 0.0377(7) Uani 1 1 d . . .
H15 H 0.6787 -0.0976 0.1723 0.045 Uiso 1 1 calc R . .
C16 C 0.6258(2) -0.0684(2) 0.20466(6) 0.0288(6) Uani 1 1 d . . .
C18 C 0.5250(2) -0.3672(2) 0.22443(6) 0.0290(6) Uani 1 1 d . . .
O181 O 0.49646(17) -0.39160(16) 0.24717(4) 0.0294(4) Uani 1 1 d . . .
O182 O 0.5236(2) -0.42572(18) 0.20841(5) 0.0396(6) Uani 1 1 d . . .
C17 C 0.6559(2) 0.0403(2) 0.20032(6) 0.0311(6) Uani 1 1 d . . .
O171 O 0.64317(17) 0.08635(15) 0.21867(4) 0.0292(5) Uani 1 1 d . . .
O172 O 0.6905(2) 0.07605(19) 0.17945(5) 0.0475(7) Uani 1 1 d . . .
C21 C 0.6667 0.3333 0.22757(18) 0.075(3) Uiso 1 3 d SD . .
N22 N 0.6678(12) 0.309(4) 0.2009(3) 0.206(17) Uiso 0.33 1 d PD A -1
C23 C 0.7670(7) 0.3318(8) 0.19168(17) 0.0334(19) Uiso 0.33 1 d PD A -1
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 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'
In In -0.7276 1.3100 '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
O181 In1 O181 87.77(12) 2_545 5_665
O181 In1 O171 125.10(9) 2_545 .
O181 In1 O171 87.04(9) 5_665 .
O181 In1 O171 87.04(9) 2_545 4
O181 In1 O171 125.10(9) 5_665 4
O171 In1 O171 137.42(13) . 4
O181 In1 N11 86.39(9) 2_545 .
O181 In1 N11 150.72(9) 5_665 .
O171 In1 N11 73.17(8) . .
O171 In1 N11 83.21(9) 4 .
O181 In1 N11 150.72(9) 2_545 4
O181 In1 N11 86.39(9) 5_665 4
O171 In1 N11 83.22(9) . 4
O171 In1 N11 73.17(8) 4 4
N11 In1 N11 111.68(12) . 4
C16 N11 N12 122.0(2) . .
C16 N11 In1 114.23(19) . .
N12 N11 In1 123.60(18) . .
C13 N12 N11 117.9(3) . .
N12 C13 C14 123.0(3) . .
N12 C13 C18 117.0(3) . .
C14 C13 C18 120.0(3) . .
C15 C14 C13 118.5(3) . .
C14 C15 C16 116.8(3) . .
N11 C16 C15 121.8(3) . .
N11 C16 C17 114.9(3) . .
C15 C16 C17 123.3(3) . .
O182 C18 O181 124.0(3) . .
O182 C18 C13 118.5(3) . .
O181 C18 C13 117.4(3) . .
C18 O181 In1 105.45(18) . 3_655
O172 C17 O171 126.1(3) . .
O172 C17 C16 117.1(3) . .
O171 C17 C16 116.9(3) . .
C17 O171 In1 118.99(19) . .
N22 C21 N22 26(4) 2_655 .
N22 C21 N22 26(4) 2_655 3_665
N22 C21 N22 26(4) . 3_665
C21 N22 C23 113.8(7) . .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
In1 O181 2.162(2) 2_545
In1 O181 2.162(2) 5_665
In1 O171 2.165(2) .
In1 O171 2.165(2) 4
In1 N11 2.286(2) .
In1 N11 2.286(2) 4
N11 C16 1.334(4) .
N11 N12 1.344(3) .
N12 C13 1.328(4) .
C13 C14 1.399(5) .
C13 C18 1.511(4) .
C14 C15 1.376(5) .
C15 C16 1.394(5) .
C16 C17 1.512(4) .
C18 O182 1.229(4) .
C18 O181 1.271(4) .
O181 In1 2.162(2) 3_655
C17 O172 1.230(4) .
C17 O171 1.273(4) .
C21 N22 1.462(5) 2_655
C21 N22 1.462(5) .
C21 N22 1.462(5) 3_665
N22 C23 1.470(5) .
loop_
_platon_squeeze_void_nr
_platon_squeeze_void_average_x
_platon_squeeze_void_average_y
_platon_squeeze_void_average_z
_platon_squeeze_void_volume
_platon_squeeze_void_count_electrons
_platon_squeeze_void_content
1 0.000 0.000 0.000 101 17 ' '
2 -0.333 0.333 0.083 549 104 ' '
3 0.000 0.000 0.250 540 103 ' '
4 0.333 0.667 0.417 549 104 ' '
5 0.000 0.000 0.500 101 17 ' '
6 -0.334 0.333 0.583 549 104 ' '
7 0.000 0.000 0.750 540 103 ' '
8 0.333 0.667 0.917 549 104 ' '
9 0.333 0.667 0.167 102 17 ' '
10 0.333 0.667 0.667 102 17 ' '
11 0.666 0.333 0.333 102 17 ' '
12 0.666 0.333 0.833 102 17 ' '
