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#$Date: 2025-08-21 03:19:08 +0300 (Thu, 21 Aug 2025) $
#$Revision: 301842 $
#$URL: file:///home/coder/svn-repositories/cod/cif/4/50/61/4506129.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_4506129
loop_
_publ_author_name
'Walsh, Rosa D.'
'Smith, Jessica M.'
'Hanks, Timothy W.'
'Pennington, William T.'
_publ_section_title
;
 Computational and Crystallographic Studies of Pseudo-Polyhalides
;
_journal_issue                   6
_journal_name_full               'Crystal Growth & Design'
_journal_page_first              2759
_journal_paper_doi               10.1021/cg201231t
_journal_volume                  12
_journal_year                    2012
_chemical_formula_sum            'C21 H36 I7 N2 Na O6'
_chemical_formula_weight         1323.81
_space_group_IT_number           148
_symmetry_space_group_name_Hall  '-R 3'
_symmetry_space_group_name_H-M   'R -3 :H'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                120.00
_cell_formula_units_Z            6
_cell_length_a                   11.818(2)
_cell_length_b                   11.818(2)
_cell_length_c                   44.264(9)
_cell_measurement_temperature    293(2)
_cell_volume                     5353.9(17)
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 0.996
_diffrn_measured_fraction_theta_max 0.996
_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  0.0587
_diffrn_reflns_av_sigmaI/netI    0.0262
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       57
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_number            2978
_diffrn_reflns_theta_full        27.54
_diffrn_reflns_theta_max         27.54
_diffrn_reflns_theta_min         2.04
_exptl_absorpt_coefficient_mu    6.133
_exptl_crystal_density_diffrn    2.464
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             3636
_refine_diff_density_max         3.249
_refine_diff_density_min         -2.627
_refine_diff_density_rms         0.302
_refine_ls_extinction_coef       0.00037(5)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4^
_refine_ls_extinction_method     SHELXL
_refine_ls_goodness_of_fit_ref   1.187
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     113
_refine_ls_number_reflns         2749
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.187
_refine_ls_R_factor_all          0.0819
_refine_ls_R_factor_gt           0.0786
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[σ²(Fo²)+(0.0581P)²+290.1663P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1815
_refine_ls_wR_factor_ref         0.1836
_reflns_number_gt                2525
_reflns_number_total             2749
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            cg201231t_si_001.cif
_cod_data_source_block           bd1174
_cod_database_code               4506129
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-y, x-y, z'
'-x+y, -x, z'
'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+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, -z'
'y, -x+y, -z'
'x-y, x, -z'
'-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+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'
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
I1 I 0.0000 0.0000 0.05508(2) 0.0468(4) Uani 1 3 d S
I2 I -0.09405(8) -0.22983(8) 0.114380(13) 0.0474(3) Uani 1 1 d .
I3 I -0.08255(16) -0.48384(14) 0.15381(2) 0.0960(5) Uani 1 1 d .
Na1 Na 0.6667 0.3333 -0.02015(17) 0.0479(18) Uani 1 3 d S
O1 O 0.6270(10) 0.1220(9) -0.05198(16) 0.053(2) Uani 1 1 d .
O2 O 0.7488(9) 0.1961(8) 0.00393(16) 0.0463(18) Uani 1 1 d .
N1 N 0.6667 0.3333 -0.0932(3) 0.044(4) Uani 1 3 d S
N2 N 0.6667 0.3333 0.0420(3) 0.044(4) Uani 1 3 d S
C1 C -0.1386(12) -0.3410(11) 0.1546(2) 0.045(3) Uani 1 1 d .
C7 C 0.7511(14) 0.2842(14) 0.0522(2) 0.054(3) Uani 1 1 d .
H7A H 0.7358 0.2636 0.0736 0.065 Uiso 1 1 calc R
H7B H 0.8414 0.3525 0.0498 0.065 Uiso 1 1 calc R
C3 C 0.5895(14) 0.1000(12) -0.0832(3) 0.053(3) Uani 1 1 d .
H3A H 0.4990 0.0781 -0.0850 0.063 Uiso 1 1 calc R
H3B H 0.5960 0.0261 -0.0904 0.063 Uiso 1 1 calc R
C4 C 0.7463(14) 0.1235(15) -0.0461(3) 0.056(3) Uani 1 1 d .
H4A H 0.8203 0.2090 -0.0505 0.067 Uiso 1 1 calc R
H4B H 0.7525 0.0594 -0.0586 0.067 Uiso 1 1 calc R
C6 C 0.7298(14) 0.1639(13) 0.0353(2) 0.052(3) Uani 1 1 d .
H6A H 0.7914 0.1379 0.0421 0.062 Uiso 1 1 calc R
H6B H 0.6420 0.0921 0.0388 0.062 Uiso 1 1 calc R
C5 C 0.7454(14) 0.0910(13) -0.0132(3) 0.052(3) Uani 1 1 d .
H5A H 0.6671 0.0092 -0.0084 0.063 Uiso 1 1 calc R
H5B H 0.8209 0.0824 -0.0084 0.063 Uiso 1 1 calc R
C2 C 0.6743(14) 0.2189(13) -0.1029(2) 0.051(3) Uani 1 1 d .
H2A H 0.7644 0.2386 -0.1020 0.061 Uiso 1 1 calc R
H2B H 0.6456 0.1988 -0.1238 0.061 Uiso 1 1 calc R
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'
Na Na 0.0362 0.0249 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
I I -0.4742 1.8119 '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
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
I2 I1 I2 70.86(3) 2 3
I2 I1 I2 70.86(3) 2 .
I2 I1 I2 70.86(3) 3 .
C1 I2 I3 32.9(3) . .
C1 I2 I1 170.7(3) . .
I3 I2 I1 152.76(3) . .
C1 I2 I3 55.8(3) . 13_445
I3 I2 I3 88.68(3) . 13_445
I1 I2 I3 117.56(3) . 13_445
C1 I3 I2 33.2(3) . .
C1 I3 I2 58.1(3) . 13_445
I2 I3 I2 91.32(3) . 13_445
O2 Na1 O2 103.2(3) . 2_655
O2 Na1 O2 103.2(3) . 3_665
O2 Na1 O2 103.2(3) 2_655 3_665
O2 Na1 O1 64.4(2) . .
O2 Na1 O1 154.6(3) 2_655 .
O2 Na1 O1 101.3(3) 3_665 .
O2 Na1 O1 101.3(3) . 2_655
O2 Na1 O1 64.4(2) 2_655 2_655
O2 Na1 O1 154.6(3) 3_665 2_655
O1 Na1 O1 95.2(3) . 2_655
O2 Na1 O1 154.6(3) . 3_665
O2 Na1 O1 101.3(3) 2_655 3_665
O2 Na1 O1 64.4(2) 3_665 3_665
O1 Na1 O1 95.2(3) . 3_665
O1 Na1 O1 95.2(3) 2_655 3_665
O2 Na1 N2 64.8(2) . .
O2 Na1 N2 64.8(2) 2_655 .
O2 Na1 N2 64.8(2) 3_665 .
O1 Na1 N2 121.5(2) . .
O1 Na1 N2 121.5(2) 2_655 .
O1 Na1 N2 121.5(2) 3_665 .
C4 O1 C3 113.0(9) . .
C4 O1 Na1 100.4(7) . .
C3 O1 Na1 124.5(7) . .
C6 O2 C5 110.5(9) . .
C6 O2 Na1 121.7(7) . .
C5 O2 Na1 118.8(6) . .
C2 N1 C2 111.7(7) . 2_655
C2 N1 C2 111.7(7) . 3_665
C2 N1 C2 111.7(7) 2_655 3_665
C7 N2 C7 110.8(7) . 3_665
C7 N2 C7 110.8(7) . 2_655
C7 N2 C7 110.8(7) 3_665 2_655
C7 N2 Na1 108.1(7) . .
C7 N2 Na1 108.1(7) 3_665 .
C7 N2 Na1 108.1(7) 2_655 .
C1 C1 I3 120.3(11) 13_445 .
C1 C1 I2 125.8(12) 13_445 .
I3 C1 I2 113.9(5) . .
N2 C7 C6 113.3(10) . .
O1 C3 C2 112.6(10) . .
O1 C4 C5 107.0(10) . .
O2 C6 C7 107.5(10) . .
O2 C5 C4 107.2(10) . .
N1 C2 C3 111.4(10) . .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
I1 I2 3.5332(11) 2
I1 I2 3.5332(11) 3
I1 I2 3.5332(11) .
I2 C1 2.115(10) .
I2 I3 3.5332(14) .
I2 I3 3.6173(13) 13_445
I3 C1 2.100(12) .
I3 I2 3.6173(13) 13_445
Na1 O2 2.507(8) .
Na1 O2 2.507(8) 2_655
Na1 O2 2.507(8) 3_665
Na1 O1 2.696(9) .
Na1 O1 2.696(9) 2_655
Na1 O1 2.696(9) 3_665
Na1 N2 2.751(16) .
O1 C4 1.426(16) .
O1 C3 1.433(13) .
O2 C6 1.428(12) .
O2 C5 1.438(14) .
N1 C2 1.465(13) .
N1 C2 1.465(13) 2_655
N1 C2 1.465(13) 3_665
N2 C7 1.454(13) .
N2 C7 1.454(13) 3_665
N2 C7 1.454(13) 2_655
C1 C1 1.32(2) 13_445
C7 C6 1.513(18) .
C3 C2 1.529(18) .
C4 C5 1.506(16) .
loop_
_cod_related_entry_id
_cod_related_entry_database
_cod_related_entry_code
1 PubChem 168345111
