#------------------------------------------------------------------------------
#$Date: 2017-11-08 06:59:47 +0200 (Wed, 08 Nov 2017) $
#$Revision: 202939 $
#$URL: file:///home/coder/svn-repositories/cod/cif/7/04/46/7044698.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_7044698
loop_
_publ_author_name
'Katam, Srinivas'
'Ganesan, Prabusankar'
_publ_section_title
;
 Large CuI8 Chalcogenone Cubic Cages with Non-interacting Counter Ion
;
_journal_name_full               'Dalton Transactions'
_journal_paper_doi               10.1039/C7DT03796A
_journal_year                    2017
_chemical_formula_moiety         'C204 H252 Cu8 N60 Se24, 6(F6 P)'
_chemical_formula_sum            'C204 H252 Cu8 F36 N60 P6 Se24'
_chemical_formula_weight         6817.85
_chemical_name_systematic
;
 ? 
;
_space_group_crystal_system      cubic
_space_group_IT_number           222
_space_group_name_Hall           '-P 4a 2bc 3'
_space_group_name_H-M_alt        'P n -3 n'
_symmetry_Int_Tables_number      222
_symmetry_space_group_name_Hall  '-P 4a 2bc 3'
_symmetry_space_group_name_H-M   'P n -3 n :2'
_atom_sites_solution_primary     direct
_audit_creation_date             2017-07-07
_audit_creation_method
;
Olex2 1.2
(compiled 2016.02.19 svn.r3266 for OlexSys, GUI svn.r5155)
;
_audit_update_record
;
2017-09-09 deposited with the CCDC.
2017-11-06 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   24.82051(14)
_cell_length_b                   24.82051(14)
_cell_length_c                   24.82051(14)
_cell_measurement_reflns_used    3704
_cell_measurement_temperature    298
_cell_measurement_theta_max      71.5218
_cell_measurement_theta_min      3.9792
_cell_volume                     15290.87(15)
_computing_cell_refinement
;
CrysAlisPro, Agilent Technologies,
Version 1.171.35.19 (release 27-10-2011 CrysAlis171 .NET)
(compiled Oct 27 2011,15:02:11)
;
_computing_data_collection
;
CrysAlisPro, Agilent Technologies,
Version 1.171.35.19 (release 27-10-2011 CrysAlis171 .NET)
(compiled Oct 27 2011,15:02:11)
;
_computing_data_reduction
;
CrysAlisPro, Agilent Technologies,
Version 1.171.35.19 (release 27-10-2011 CrysAlis171 .NET)
(compiled Oct 27 2011,15:02:11)
;
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'olex2.refine (Bourhis et al., 2015)'
_computing_structure_solution    'SIR2004 (Burla et al., 2007)'
_diffrn_ambient_temperature      298
_diffrn_detector_area_resol_mean 16.1293
_diffrn_measured_fraction_theta_full 0.9833
_diffrn_measured_fraction_theta_max 0.9833
_diffrn_measurement_details
;
#__ type_ start__ end____ width___ exp.time_
  1 omega  -50.00  -12.00   1.0000    8.4300
omega____ theta____ kappa____ phi______ frames
    -        0.0000  130.0000  -15.0000 38

#__ type_ start__ end____ width___ exp.time_
  2 omega  -50.00   22.00   1.0000   25.7000
omega____ theta____ kappa____ phi______ frames
    -      -42.5000   38.0000   90.0000 72

#__ type_ start__ end____ width___ exp.time_
  3 omega   54.00   87.00   1.0000   25.7000
omega____ theta____ kappa____ phi______ frames
    -      110.2786  -38.0000 -120.0000 33

#__ type_ start__ end____ width___ exp.time_
  4 omega   39.00  101.00   1.0000   25.7000
omega____ theta____ kappa____ phi______ frames
    -      110.2786  -91.0000  -60.0000 62
;
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at zero, Eos'
_diffrn_measurement_method       'ω scans'
_diffrn_radiation_type           'Cu K\a'
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0288
_diffrn_reflns_av_unetI/netI     0.0238
_diffrn_reflns_limit_h_max       26
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       30
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_number            12189
_diffrn_reflns_theta_full        71.6646
_diffrn_reflns_theta_max         71.66
_diffrn_reflns_theta_min         4.36
_exptl_absorpt_coefficient_mu    4.785
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.78756
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro, Agilent Technologies,
Version 1.171.35.19 (release 27-10-2011 CrysAlis171 .NET)
(compiled Oct 27 2011,15:02:11)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            colourless
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.4807
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             6665.9592
_exptl_crystal_size_max          0.24
_exptl_crystal_size_mid          0.16
_exptl_crystal_size_min          0.12
_refine_diff_density_max         0.3893
_refine_diff_density_min         -0.6408
_refine_diff_density_rms         0.0721
_refine_ls_d_res_high            0.8122
_refine_ls_d_res_low             10.1329
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4^
_refine_ls_goodness_of_fit_ref   1.0110
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_constraints    18
_refine_ls_number_parameters     131
_refine_ls_number_reflns         2478
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.0110
_refine_ls_R_factor_all          0.0478
_refine_ls_R_factor_gt           0.0359
_refine_ls_shift/su_max          0.0002
_refine_ls_shift/su_mean         0.0000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[σ²(Fo²)+(0.0462P)²+9.9173P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0893
_refine_ls_wR_factor_ref         0.0979
_reflns_Friedel_coverage         0.0
_reflns_limit_h_max              16
_reflns_limit_h_min              0
_reflns_limit_k_max              30
_reflns_limit_k_min              2
_reflns_limit_l_max              21
_reflns_limit_l_min              0
_reflns_number_gt                1920
_reflns_number_total             2478
_reflns_threshold_expression     I>=2u(I)
_cod_data_source_file            c7dt03796a2.cif
_cod_data_source_block           2
_cod_database_code               7044698
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2.a Ternary CH refined with riding coordinates:
 C4(H4)
2.b Aromatic/amide H refined with riding coordinates:
 C2(H2), C3(H3), C8(H8), C9(H9)
2.c Idealised Me refined as rotating group:
 C5(H5a,H5b,H5c), C6(H6a,H6b,H6c)
;
_olex2_submission_special_instructions 'No special instructions were received'
loop_
_space_group_symop_id
_space_group_symop_operation_xyz
1 x,y,z
2 x,-z+1/2,y
3 x,z,-y+1/2
4 z,y,-x+1/2
5 -z+1/2,y,x
6 -y+1/2,x,z
7 y,-x+1/2,z
8 z,x,y
9 y,z,x
10 -y+1/2,-z+1/2,x
11 z,-x+1/2,-y+1/2
12 -y+1/2,z,-x+1/2
13 -z+1/2,-x+1/2,y
14 -z+1/2,x,-y+1/2
15 y,-z+1/2,-x+1/2
16 x,-y+1/2,-z+1/2
17 -x+1/2,y,-z+1/2
18 -x+1/2,-y+1/2,z
19 y,x,-z+1/2
20 -y+1/2,-x+1/2,-z+1/2
21 z,-y+1/2,x
22 -z+1/2,-y+1/2,-x+1/2
23 -x+1/2,z,y
24 -x+1/2,-z+1/2,-y+1/2
25 -x,-y,-z
26 -x,z-1/2,-y
27 -x,-z,y-1/2
28 -z,-y,x-1/2
29 z-1/2,-y,-x
30 y-1/2,-x,-z
31 -y,x-1/2,-z
32 -z,-x,-y
33 -y,-z,-x
34 y-1/2,z-1/2,-x
35 -z,x-1/2,y-1/2
36 y-1/2,-z,x-1/2
37 z-1/2,x-1/2,-y
38 z-1/2,-x,y-1/2
39 -y,z-1/2,x-1/2
40 -x,y-1/2,z-1/2
41 x-1/2,-y,z-1/2
42 x-1/2,y-1/2,-z
43 -y,-x,z-1/2
44 y-1/2,x-1/2,z-1/2
45 -z,y-1/2,-x
46 z-1/2,y-1/2,x-1/2
47 x-1/2,-z,-y
48 x-1/2,z-1/2,y-1/2
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_site_symmetry_order
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
Se1 Se 0.404428(17) 0.367774(16) 0.497099(16) 0.06516(17) Uani 1.000000 1 . . .
Cu1 Cu 0.42319(2) 0.42319(2) 0.42319(2) 0.0584(3) Uani 1.000000 3 S T P
N1 N 0.35538(12) 0.40689(12) 0.59298(11) 0.0574(7) Uani 1.000000 1 . . .
N2 N 0.30175(10) 0.41814(10) 0.52565(10) 0.0478(6) Uani 1.000000 1 . . .
N3 N 0.25 0.46753(10) 0.46753(10) 0.0434(8) Uani 1.000000 2 S T P
C1 C 0.35144(14) 0.39965(12) 0.53928(13) 0.0496(8) Uani 1.000000 1 . . .
C2 C 0.30899(16) 0.43020(15) 0.61245(14) 0.0639(10) Uani 1.000000 1 . . .
H2 H 0.30211(16) 0.43911(15) 0.64819(14) 0.0767(12) Uiso 1.000000 1 R . .
C3 C 0.27577(15) 0.43770(15) 0.57116(13) 0.0584(9) Uani 1.000000 1 . . .
H3 H 0.24164(15) 0.45310(15) 0.57248(13) 0.0701(10) Uiso 1.000000 1 R . .
C4 C 0.40361(18) 0.39593(19) 0.62654(16) 0.0782(12) Uani 1.000000 1 . . .
H4 H 0.42935(18) 0.37589(19) 0.60429(16) 0.0938(15) Uiso 1.000000 1 R . .
C5 C 0.4299(3) 0.4480(3) 0.6425(3) 0.164(3) Uani 1.000000 1 . . .
H5a H 0.431(2) 0.4716(10) 0.6119(7) 0.245(5) Uiso 1.000000 1 GR . .
H5b H 0.4094(15) 0.4647(13) 0.6707(17) 0.245(5) Uiso 1.000000 1 GR . .
H5c H 0.4658(10) 0.4410(4) 0.655(2) 0.245(5) Uiso 1.000000 1 GR . .
C6 C 0.3887(3) 0.3609(3) 0.6732(2) 0.162(3) Uani 1.000000 1 . . .
H6a H 0.368(2) 0.3813(8) 0.6985(12) 0.243(5) Uiso 1.000000 1 GR . .
H6b H 0.368(2) 0.3307(14) 0.6607(4) 0.243(5) Uiso 1.000000 1 GR . .
H6c H 0.4209(3) 0.348(2) 0.6905(15) 0.243(5) Uiso 1.000000 1 GR . .
C7 C 0.27701(13) 0.42190(12) 0.47350(13) 0.0482(7) Uani 1.000000 1 . . .
C8 C 0.27856(15) 0.38148(14) 0.43628(15) 0.0615(9) Uani 1.000000 1 . . .
H8 H 0.29805(15) 0.35007(14) 0.44240(15) 0.0738(11) Uiso 1.000000 1 R . .
C9 C 0.25 0.38912(15) 0.38912(15) 0.0688(14) Uani 1.000000 2 S T P
H9 H 0.25 0.36263(15) 0.36263(15) 0.0825(17) Uiso 1.000000 2 RS T P
P1 P 0.5 0.25 0.75 0.0594(5) Uani 1.000000 4 S T P
F1 F 0.50035(12) 0.26888(9) 0.68889(9) 0.0906(8) Uani 1.000000 1 . . .
F2 F 0.56321(14) 0.25 0.75 0.1122(14) Uani 1.000000 2 S T P
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_a2
_atom_type_scat_Cromer_Mann_a3
_atom_type_scat_Cromer_Mann_a4
_atom_type_scat_Cromer_Mann_b1
_atom_type_scat_Cromer_Mann_b2
_atom_type_scat_Cromer_Mann_b3
_atom_type_scat_Cromer_Mann_b4
_atom_type_scat_Cromer_Mann_c
_atom_type_scat_source
_atom_type_scat_dispersion_source
C 0.01920 0.00962 2.31000 1.02000 1.58860 0.86500 20.84390 10.20750 0.56870
51.65120 0.215599998832
'International Tables Volume C Table 6.1.1.4 (pp. 500-502)'
'Henke, Gullikson and Davis, At. Data and Nucl. Data Tables, 1993, 54, 2'
F 0.07537 0.05506 3.53920 2.64120 1.51700 1.02430 10.28250 4.29440 0.26150
26.14760 0.277599990368
'International Tables Volume C Table 6.1.1.4 (pp. 500-502)'
'Henke, Gullikson and Davis, At. Data and Nucl. Data Tables, 1993, 54, 2'
H 0.00000 0.00000 0.49300 0.32291 0.14019 0.04081 10.51090 26.12570 3.14236
57.79970 0.0030380000826
'International Tables Volume C Table 6.1.1.4 (pp. 500-502)'
'Henke, Gullikson and Davis, At. Data and Nucl. Data Tables, 1993, 54, 2'
N 0.03256 0.01839 12.21260 3.13220 2.01250 1.16630 0.00570 9.89330 28.99750
0.58260 -11.5290002823
'International Tables Volume C Table 6.1.1.4 (pp. 500-502)'
'Henke, Gullikson and Davis, At. Data and Nucl. Data Tables, 1993, 54, 2'
P 0.30360 0.43703 6.43450 4.17910 1.78000 1.49080 1.90670 27.15700 0.52600
68.16450 1.11489999294
'International Tables Volume C Table 6.1.1.4 (pp. 500-502)'
'Henke, Gullikson and Davis, At. Data and Nucl. Data Tables, 1993, 54, 2'
Cu -1.96878 0.60861 13.33800 7.16760 5.61580 1.67350 3.58280 0.24700 11.39660
64.81260 1.19099998474
'International Tables Volume C Table 6.1.1.4 (pp. 500-502)'
'Henke, Gullikson and Davis, At. Data and Nucl. Data Tables, 1993, 54, 2'
Se -0.79210 1.18296 17.00060 5.81960 3.97310 4.35430 2.40980 0.27260 15.23720
43.81630 2.84089994431
'International Tables Volume C Table 6.1.1.4 (pp. 500-502)'
'Henke, Gullikson and Davis, At. Data and Nucl. Data Tables, 1993, 54, 2'
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
C1 Se1 Cu1 109.41(9) . 9
Se1 Cu1 Se1 120.0 9 8
Se1 Cu1 Se1 120.0 9 .
Se1 Cu1 Se1 120.0 . 8
C2 N1 C1 110.0(3) . .
C4 N1 C1 126.1(3) . .
C4 N1 C2 123.7(3) . .
C3 N2 C1 109.7(3) . .
C7 N2 C1 129.4(3) . .
C7 N2 C3 120.8(3) . .
C7 N3 C7 116.6(4) 23 .
N1 C1 Se1 124.2(2) . .
N2 C1 Se1 130.3(2) . .
N2 C1 N1 105.5(3) . .
H2 C2 N1 126.06(19) . .
C3 C2 N1 107.9(3) . .
C3 C2 H2 126.1(2) . .
C2 C3 N2 106.9(3) . .
H3 C3 N2 126.56(19) . .
H3 C3 C2 126.6(2) . .
H4 C4 N1 107.6(2) . .
C5 C4 N1 109.9(4) . .
C5 C4 H4 107.6(3) . .
C6 C4 N1 110.0(4) . .
C6 C4 H4 107.6(3) . .
C6 C4 C5 113.8(5) . .
H5a C5 C4 109.5 . .
H5b C5 C4 109.5 . .
H5b C5 H5a 109.5 . .
H5c C5 C4 109.5 . .
H5c C5 H5a 109.5 . .
H5c C5 H5b 109.5 . .
H6a C6 C4 109.5 . .
H6b C6 C4 109.5 . .
H6b C6 H6a 109.5 . .
H6c C6 C4 109.5 . .
H6c C6 H6a 109.5 . .
H6c C6 H6b 109.5 . .
N3 C7 N2 111.9(3) . .
C8 C7 N2 123.4(3) . .
C8 C7 N3 124.6(3) . .
H8 C8 C7 121.4(2) . .
C9 C8 C7 117.3(4) . .
C9 C8 H8 121.4(2) . .
C8 C9 C8 119.7(5) 23 .
H9 C9 C8 120.1(2) . .
H9 C9 C8 120.1(2) . 23
F1 P1 F1 179.4(2) 16_556 .
F1 P1 F1 90.002(14) 27_666 16_556
F1 P1 F1 90.002(15) 27_666 .
F1 P1 F1 90.002(15) 26_656 16_556
F1 P1 F1 90.002(14) 26_656 .
F1 P1 F1 179.4(2) 26_656 27_666
F2 P1 F1 89.68(10) . 16_556
F2 P1 F1 90.32(10) . 26_656
F2 P1 F1 89.68(10) 27_666 27_666
F2 P1 F1 90.32(10) 27_666 .
F2 P1 F1 89.68(10) . .
F2 P1 F1 90.32(10) . 27_666
F2 P1 F1 89.68(10) 27_666 26_656
F2 P1 F1 90.32(10) 27_666 16_556
F2 P1 F2 180.0 27_666 .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
Se1 Cu1 2.3397(4) 9
Se1 C1 1.858(3) .
N1 C1 1.349(4) .
N1 C2 1.376(4) .
N1 C4 1.484(5) .
N2 C1 1.359(4) .
N2 C3 1.388(4) .
N2 C7 1.436(4) .
N3 C7 1.325(4) 23
N3 C7 1.325(4) .
C2 H2 0.9300 .
C2 C3 1.329(5) .
C3 H3 0.9300 .
C4 H4 0.9800 .
C4 C5 1.501(7) .
C4 C6 1.496(7) .
C5 H5a 0.9600 .
C5 H5b 0.9600 .
C5 H5c 0.9600 .
C6 H6a 0.9600 .
C6 H6b 0.9600 .
C6 H6c 0.9600 .
C7 C8 1.364(4) .
C8 H8 0.9300 .
C8 C9 1.381(4) .
C9 H9 0.9300 .
P1 F1 1.588(2) 26_656
P1 F1 1.588(2) 27_666
P1 F1 1.588(2) 16_556
P1 F1 1.588(2) .
P1 F2 1.569(4) .
P1 F2 1.569(4) 27_666
loop_
_smtbx_masks_void_nr
_smtbx_masks_void_average_x
_smtbx_masks_void_average_y
_smtbx_masks_void_average_z
_smtbx_masks_void_volume
_smtbx_masks_void_count_electrons
1 0.000 0.000 0.000 56.7 6.6
2 0.000 0.000 0.500 56.7 6.6
3 0.123 0.403 -0.439 1558.8 684.4
4 0.000 0.500 0.000 56.7 6.6
5 0.000 0.500 0.500 56.7 6.6
6 0.243 0.590 -0.181 1558.8 677.6
7 0.500 0.000 0.000 56.7 6.6
8 0.500 0.000 0.500 56.7 6.6
9 0.500 0.500 0.500 56.7 6.6
10 0.500 0.500 0.000 56.7 6.6
