#------------------------------------------------------------------------------
#$Date: 2016-03-25 23:23:56 +0200 (Fri, 25 Mar 2016) $
#$Revision: 180037 $
#$URL: svn://www.crystallography.net/cod/cif/7/03/31/7033170.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_7033170
loop_
_publ_author_name
'Ewing, S. J.'
'Vaqueiro, P.'
_publ_section_title
;
 Structural complexity in indium selenides prepared using bicyclic amines
 as structure-directing agents.
;
_journal_issue                   4
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              1592
_journal_page_last               1600
_journal_paper_doi               10.1039/c4dt02819h
_journal_volume                  44
_journal_year                    2015
_chemical_absolute_configuration ad
_chemical_formula_moiety         'C2 H10 In7 N3 Se12'
_chemical_formula_sum            'C2 H10 In7 N3 Se12'
_chemical_formula_weight         1827.38
_space_group_IT_number           4
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  'P 2yb'
_symmetry_space_group_name_H-M   'P 1 21 1'
_atom_sites_solution_hydrogens   difmap
_atom_sites_solution_primary     direct
_cell_angle_alpha                90
_cell_angle_beta                 96.145(2)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   10.3062(3)
_cell_length_b                   13.4581(4)
_cell_length_c                   10.5966(3)
_cell_measurement_reflns_used    0
_cell_measurement_temperature    293
_cell_measurement_theta_max      0
_cell_measurement_theta_min      0
_cell_volume                     1461.32(7)
_computing_cell_refinement       'Apex2 (Bruker AXS, 2006)'
_computing_data_collection       'Apex2 (Bruker AXS, 2006)'
_computing_data_reduction        'Apex2 (Bruker AXS, 2006)'
_computing_molecular_graphics    'CAMERON (Watkin et al., 1996)'
_computing_publication_material  'CRYSTALS (Betteridge et al., 2003)'
_computing_structure_refinement  'CRYSTALS (Betteridge et al., 2003)'
_computing_structure_solution    'SHELXS 86 (Sheldrick, 1986)'
_diffrn_ambient_temperature      293
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measurement_device       Area
_diffrn_measurement_device_type  'Bruker Kappa Apex2'
_diffrn_measurement_method       ω/2θ
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.051
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       14
_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_number            26977
_diffrn_reflns_theta_full        29.133
_diffrn_reflns_theta_max         29.133
_diffrn_reflns_theta_min         1.987
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    20.368
_exptl_absorpt_correction_T_max  0.36
_exptl_absorpt_correction_T_min  0.23
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS (Siemens, 1996)'
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    4.153
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             1588
_exptl_crystal_size_max          0.080
_exptl_crystal_size_mid          0.050
_exptl_crystal_size_min          0.050
_refine_diff_density_max         1.53
_refine_diff_density_min         -1.37
_refine_ls_abs_structure_details 'Flack (1983), 2897 Friedel-pairs'
_refine_ls_abs_structure_Flack   0.079(12)
_refine_ls_extinction_method     None
_refine_ls_goodness_of_fit_ref   0.9972
_refine_ls_hydrogen_treatment    noref
_refine_ls_matrix_type           full
_refine_ls_number_parameters     193
_refine_ls_number_reflns         5410
_refine_ls_number_restraints     2
_refine_ls_R_factor_all          0.0492
_refine_ls_R_factor_gt           0.0358
_refine_ls_shift/su_max          0.0011085
_refine_ls_shift/su_mean         0.0000979
_refine_ls_structure_factor_coef F
_refine_ls_weighting_details
;
 Method, part 1, Chebychev polynomial, (Watkin, 1994, Prince, 1982) 
 [weight] = 1.0/[A₀*T₀(x)+A₁*T₁(x) ... +Aₙ₋₁]*Tₙ₋₁(x)] 
 where Ai are the Chebychev coefficients listed below and x= Fcalc/Fmax 
 Method = Robust Weighting (Prince, 1982) 
 W = [weight] * [1-(deltaF/6*sigmaF)²]² 
 Ai are: 
 0.240 0.202E-01 0.382E-01 
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.0547
_refine_ls_wR_factor_gt          0.0364
_refine_ls_wR_factor_ref         0.0344
_reflns_limit_h_max              14
_reflns_limit_h_min              -14
_reflns_limit_k_max              18
_reflns_limit_k_min              -15
_reflns_limit_l_max              14
_reflns_limit_l_min              0
_reflns_number_gt                5838
_reflns_number_total             6986
_reflns_threshold_expression     I>2.0σ(I)
_oxford_diffrn_Wilson_B_factor   0.00
_oxford_diffrn_Wilson_scale      0.00
_oxford_refine_ls_r_factor_ref   0.0327
_oxford_refine_ls_scale          0.06277(6)
_oxford_reflns_number_all        6967
_oxford_reflns_threshold_expression_ref I>3.0\s(I)
_cod_data_source_file            c4dt02819h2.cif
_cod_data_source_block           1
_cod_depositor_comments
'Adding full bibliography for 7033166--7033170.cif.'
_cod_original_sg_symbol_H-M      'P 1 21 1 '
_cod_database_code               7033170
#BEGIN Tags that were not found in dictionaries:
_iucr_refine_instruction_details_constraints
;
BLOCK SCALE 
CONT N(1, X'S, U[ISO]) UNTIL N(5) 
CONT IN (1, X'S, U'S) UNTIL SE(19) 
CONT ENANTIO 
END                                                                             
;
_iucr_refine_instruction_details_restraints
;
NO 
REM   HREST   START (DO NOT REMOVE THIS LINE) 
REM   HREST   END (DO NOT REMOVE THIS LINE) 
DIST 1.54 0.01 = C(4) TO C(3) 
END                                                                             
;
#END Tags that were not found in dictionaries
loop_
_symmetry_equiv_pos_as_xyz
x,y,z
-x,y+1/2,-z
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_occupancy
_atom_site_adp_type
_atom_site_refinement_flags_posn
N1 N 0.6597(12) 0.7316(9) 0.3622(11) 0.038(3) 1.0000 Uiso .
N2 N 0.952(2) 0.8933(16) 0.0616(19) 0.086(6) 1.0000 Uiso .
C3 C 1.102(2) 0.9089(16) 0.085(2) 0.073(6) 1.0000 Uiso D
C4 C 1.140(3) 0.8150(17) 0.165(2) 0.090(8) 1.0000 Uiso D
N5 N 1.261(3) 0.8086(18) 0.195(2) 0.106(8) 1.0000 Uiso .
In1 In 0.47290(8) 0.49165(7) 1.00555(7) 0.0215 1.0000 Uani .
In2 In 0.63669(8) 0.73038(7) 0.85069(8) 0.0213 1.0000 Uani .
In3 In 0.28153(7) 0.50307(7) 0.29235(7) 0.0193 1.0000 Uani .
In4 In 0.01020(8) 0.26747(7) 0.30373(9) 0.0263 1.0000 Uani .
In5 In 0.31133(8) 0.60350(7) 0.65582(8) 0.0210 1.0000 Uani .
In6 In 0.97389(8) 0.51885(7) 0.50800(8) 0.0214 1.0000 Uani .
In7 In 0.66350(8) 0.40600(7) 0.32037(8) 0.0200 1.0000 Uani .
Se8 Se 0.44287(16) 0.30598(10) 0.95126(12) 0.0328 1.0000 Uani .
Se9 Se 0.26364(13) 0.56932(11) 0.06485(12) 0.0305 1.0000 Uani .
Se10 Se 0.67646(13) 0.53935(10) 0.15260(12) 0.0266 1.0000 Uani .
Se11 Se 0.53505(11) 0.55652(9) 0.78495(10) 0.0173 1.0000 Uani .
Se12 Se 0.88103(14) 0.68843(13) 0.87597(19) 0.0492 1.0000 Uani .
Se13 Se 0.42201(11) 0.34395(9) 0.34987(10) 0.0190 1.0000 Uani .
Se14 Se 0.36534(14) 0.64735(10) 0.43347(12) 0.0277 1.0000 Uani .
Se15 Se 0.16221(13) 0.45503(10) 0.66476(13) 0.0296 1.0000 Uani .
Se16 Se 0.03198(11) 0.46023(9) 0.28388(11) 0.0202 1.0000 Uani .
Se17 Se 0.97407(15) 0.70722(10) 0.47031(14) 0.0349 1.0000 Uani .
Se18 Se 0.76163(11) 0.25223(9) 0.21211(10) 0.0189 1.0000 Uani .
Se19 Se 0.74697(13) 0.45898(12) 0.54406(12) 0.0327 1.0000 Uani .
H31 H 1.1225 0.9724 0.1300 0.0864 1.0000 Uiso .
H32 H 1.1413 0.9151 0.0063 0.0864 1.0000 Uiso .
H41 H 1.1009 0.8095 0.2458 0.1047 1.0000 Uiso .
H42 H 1.1161 0.7514 0.1217 0.1047 1.0000 Uiso .
H21 H 0.9078 0.9450 0.0125 0.1019 1.0000 Uiso .
H22 H 0.9153 0.8888 0.1409 0.1019 1.0000 Uiso .
H23 H 0.9341 0.8315 0.0171 0.1019 1.0000 Uiso .
H51 H 1.2901 0.7515 0.2448 0.1226 1.0000 Uiso .
H52 H 1.2900 0.8667 0.2441 0.1226 1.0000 Uiso .
H53 H 1.3052 0.8087 0.1201 0.1226 1.0000 Uiso .
loop_
_atom_type_symbol
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_Cromer_Mann_a1
_atom_type_scat_Cromer_Mann_b1
_atom_type_scat_Cromer_Mann_a2
_atom_type_scat_Cromer_Mann_b2
_atom_type_scat_Cromer_Mann_a3
_atom_type_scat_Cromer_Mann_b3
_atom_type_scat_Cromer_Mann_a4
_atom_type_scat_Cromer_Mann_b4
_atom_type_scat_Cromer_Mann_c
_atom_type_scat_source
C 0.0033 0.0016 2.3100 20.8439 1.0200 10.2075 1.5886 0.5687 0.8650 51.6512
0.2156 'International Tables Vol C 4.2.6.8 and 6.1.1.4'
H 0.0000 0.0000 0.4930 10.5109 0.3229 26.1257 0.1402 3.1424 0.0408 57.7998
0.0030 'International Tables Vol C 4.2.6.8 and 6.1.1.4'
N 0.0061 0.0033 12.2126 0.0057 3.1322 9.8933 2.0125 28.9975 1.1663 0.5826
-11.5290 'International Tables Vol C 4.2.6.8 and 6.1.1.4'
Se -0.0929 2.2259 17.0006 2.4098 5.8196 0.2726 3.9731 15.2372 4.3543 43.8163
2.8409 'International Tables Vol C 4.2.6.8 and 6.1.1.4'
In -0.7276 1.3100 19.1624 0.5476 18.5596 6.3776 4.2948 25.8499 2.0396 92.8029
4.9391 'International Tables Vol C 4.2.6.8 and 6.1.1.4'
loop_
_geom_angle_atom_site_label_1
_geom_angle_site_symmetry_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle_site_symmetry_3
_geom_angle
_geom_angle_publ_flag
C3 . N2 H21 . 113.7 no
C3 . N2 H22 . 110.5 no
H21 . N2 H22 . 108.0 no
C3 . N2 H23 . 109.4 no
H21 . N2 H23 . 107.7 no
H22 . N2 H23 . 107.3 no
N2 . C3 C4 . 99.5(18) yes
N2 . C3 H31 . 110.3 no
C4 . C3 H31 . 114.5 no
N2 . C3 H32 . 111.7 no
C4 . C3 H32 . 116.1 no
H31 . C3 H32 . 104.9 no
C3 . C4 N5 . 112(2) yes
C3 . C4 H41 . 115.7 no
N5 . C4 H41 . 105.4 no
C3 . C4 H42 . 114.5 no
N5 . C4 H42 . 104.5 no
H41 . C4 H42 . 103.4 no
C4 . N5 H51 . 115.9 no
C4 . N5 H52 . 108.7 no
H51 . N5 H52 . 106.8 no
C4 . N5 H53 . 109.9 no
H51 . N5 H53 . 107.9 no
H52 . N5 H53 . 107.2 no
Se10 1_556 In1 Se9 1_556 114.17(5) yes
Se10 1_556 In1 Se8 . 116.79(6) yes
Se9 1_556 In1 Se8 . 111.73(6) yes
Se10 1_556 In1 Se11 . 101.29(5) yes
Se9 1_556 In1 Se11 . 112.14(5) yes
Se8 . In1 Se11 . 99.09(5) yes
Se13 2_656 In2 Se8 2_657 111.51(5) yes
Se13 2_656 In2 Se11 . 104.61(5) yes
Se8 2_657 In2 Se11 . 114.84(5) yes
Se13 2_656 In2 Se12 . 110.47(5) yes
Se8 2_657 In2 Se12 . 113.63(7) yes
Se11 . In2 Se12 . 101.00(6) yes
Se9 . In3 Se13 . 119.10(5) yes
Se9 . In3 Se14 . 105.87(5) yes
Se13 . In3 Se14 . 110.04(5) yes
Se9 . In3 Se16 . 94.17(5) yes
Se13 . In3 Se16 . 110.06(5) yes
Se14 . In3 Se16 . 117.18(5) yes
Se18 1_455 In4 Se12 2_646 100.35(5) yes
Se18 1_455 In4 Se17 2_646 106.56(5) yes
Se12 2_646 In4 Se17 2_646 126.07(7) yes
Se18 1_455 In4 Se16 . 97.78(5) yes
Se12 2_646 In4 Se16 . 107.83(6) yes
Se17 2_646 In4 Se16 . 113.51(5) yes
Se18 2_656 In5 Se11 . 101.13(4) yes
Se18 2_656 In5 Se14 . 115.09(5) yes
Se11 . In5 Se14 . 105.71(5) yes
Se18 2_656 In5 Se15 . 112.11(5) yes
Se11 . In5 Se15 . 107.05(5) yes
Se14 . In5 Se15 . 114.30(5) yes
Se16 1_655 In6 Se15 1_655 104.76(5) yes
Se16 1_655 In6 Se17 . 98.72(5) yes
Se15 1_655 In6 Se17 . 114.75(5) yes
Se16 1_655 In6 Se19 . 110.04(5) yes
Se15 1_655 In6 Se19 . 116.19(6) yes
Se17 . In6 Se19 . 110.65(6) yes
Se10 . In7 Se13 . 114.94(5) yes
Se10 . In7 Se18 . 101.53(5) yes
Se13 . In7 Se18 . 102.24(4) yes
Se10 . In7 Se19 . 114.69(5) yes
Se13 . In7 Se19 . 101.85(5) yes
Se18 . In7 Se19 . 121.53(5) yes
In1 . Se8 In2 2_647 104.20(5) yes
In3 . Se9 In1 1_554 96.45(5) yes
In1 1_554 Se10 In7 . 98.51(5) yes
In1 . Se11 In5 . 104.96(5) yes
In1 . Se11 In2 . 100.81(5) yes
In5 . Se11 In2 . 103.09(5) yes
In2 . Se12 In4 2_656 109.63(6) yes
In7 . Se13 In2 2_646 102.89(4) yes
In7 . Se13 In3 . 102.44(4) yes
In2 2_646 Se13 In3 . 102.30(5) yes
In5 . Se14 In3 . 105.82(5) yes
In6 1_455 Se15 In5 . 97.58(5) yes
In6 1_455 Se16 In3 . 102.69(5) yes
In6 1_455 Se16 In4 . 101.25(5) yes
In3 . Se16 In4 . 107.88(5) yes
In6 . Se17 In4 2_656 99.86(6) yes
In4 1_655 Se18 In7 . 100.48(5) yes
In4 1_655 Se18 In5 2_646 100.75(5) yes
In7 . Se18 In5 2_646 103.00(4) yes
In6 . Se19 In7 . 100.03(5) yes
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
N2 C3 . 1.55(3) yes
N2 H21 . 0.956 no
N2 H22 . 0.961 no
N2 H23 . 0.965 no
C3 C4 . 1.549(10) yes
C3 H31 . 0.989 no
C3 H32 . 0.968 no
C4 N5 . 1.25(3) yes
C4 H41 . 0.986 no
C4 H42 . 0.991 no
N5 H51 . 0.962 no
N5 H52 . 0.970 no
N5 H53 . 0.957 no
In1 Se10 1_556 2.5577(15) yes
In1 Se9 1_556 2.5356(16) yes
In1 Se8 . 2.5754(16) yes
In1 Se11 . 2.6376(14) yes
In2 Se13 2_656 2.6350(14) yes
In2 Se8 2_657 2.5457(16) yes
In2 Se11 . 2.6270(14) yes
In2 Se12 . 2.5666(16) yes
In3 Se9 . 2.5585(14) yes
In3 Se13 . 2.6200(14) yes
In3 Se14 . 2.5447(15) yes
In3 Se16 . 2.6280(14) yes
In4 Se18 1_455 2.6486(14) yes
In4 Se12 2_646 2.5439(18) yes
In4 Se17 2_646 2.5167(18) yes
In4 Se16 . 2.6143(15) yes
In5 Se18 2_656 2.5992(14) yes
In5 Se11 . 2.6292(13) yes
In5 Se14 . 2.5477(15) yes
In5 Se15 . 2.5287(15) yes
In6 Se16 1_655 2.6315(14) yes
In6 Se15 1_655 2.5639(15) yes
In6 Se17 . 2.5664(16) yes
In6 Se19 . 2.5409(15) yes
In7 Se10 . 2.5396(15) yes
In7 Se13 . 2.6751(14) yes
In7 Se18 . 2.6210(14) yes
In7 Se19 . 2.5359(15) yes
