#------------------------------------------------------------------------------
#$Date: 2016-03-24 01:48:13 +0100 (jue 24 de mar de 2016) $
#$Revision: 179597 $
#$URL: svn://www.crystallography.net/cod/cif/4/50/61/4506133.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_4506133
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            'C27 H52 I7 K O14'
_chemical_formula_weight         1528.09
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           191
_symmetry_space_group_name_Hall  '-P 6 2'
_symmetry_space_group_name_H-M   'P 6/m m m'
_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            2
_cell_length_a                   14.643(5)
_cell_length_b                   14.643(5)
_cell_length_c                   8.933(3)
_cell_measurement_temperature    293(2)
_cell_volume                     1658.8(10)
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.997
_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  0.0368
_diffrn_reflns_av_sigmaI/netI    0.0112
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       10
_diffrn_reflns_limit_l_min       -11
_diffrn_reflns_number            15942
_diffrn_reflns_theta_full        26.38
_diffrn_reflns_theta_max         26.38
_diffrn_reflns_theta_min         2.78
_exptl_absorpt_coefficient_mu    6.747
_exptl_crystal_density_diffrn    3.059
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             1432
_refine_diff_density_max         1.924
_refine_diff_density_min         -1.514
_refine_diff_density_rms         0.388
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.049
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     18
_refine_ls_number_reflns         726
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.049
_refine_ls_R_factor_all          0.1175
_refine_ls_R_factor_gt           0.1175
_refine_ls_shift/su_max          0.006
_refine_ls_shift/su_mean         0.001
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[σ²(Fo²)+(0.0100P)²+240.0000P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2548
_refine_ls_wR_factor_ref         0.2548
_reflns_number_gt                726
_reflns_number_total             726
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            cg201231t_si_001.cif
_cod_data_source_block           cd0287a
_cod_database_code               4506133
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-y, x-y, z'
'-x+y, -x, z'
'-x, -y, z'
'y, -x+y, z'
'x-y, x, z'
'y, x, -z'
'x-y, -y, -z'
'-x, -x+y, -z'
'-y, -x, -z'
'-x+y, y, -z'
'x, x-y, -z'
'-x, -y, -z'
'y, -x+y, -z'
'x-y, x, -z'
'x, y, -z'
'-y, x-y, -z'
'-x+y, -x, -z'
'-y, -x, z'
'-x+y, y, z'
'x, x-y, z'
'y, x, z'
'x-y, -y, z'
'-x, -x+y, 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_adp_type
_atom_site_occupancy
_atom_site_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
I1 I 0.6667 0.3333 0.5000 0.0644(17) Uani 1 12 d S
I2 I 0.42956(10) 0.8591(2) 0.7988(3) 0.0746(10) Uani 1 2 d S
C1 C 0.470(4) 0.940(9) 1.0000 0.07(3) Uiso 0.50 4 d SP
C1A C 0.5000 0.5000 1.061(9) 0.042(19) Uiso 0.50 4 d SP
K1 K 1.0000 0.0000 1.0000 0.105(14) Uani 1 24 d S
K2 K 1.0000 0.0000 0.5000 0.22(14) Uiso 0.25 24 d SP
O1 O 1.227(8) 0.0000 1.0000 0.13(4) Uiso 0.50 4 d SP
loop_
_atom_site_aniso_label
_atom_site_aniso_U_11
_atom_site_aniso_U_22
_atom_site_aniso_U_33
_atom_site_aniso_U_23
_atom_site_aniso_U_13
_atom_site_aniso_U_12
I1 0.078(3) 0.078(3) 0.037(2) 0.000 0.000 0.0392(13)
I2 0.0736(14) 0.0544(14) 0.0895(18) -0.0167(15) -0.0084(7) 0.0272(7)
K1 0.092(18) 0.092(18) 0.13(4) 0.000 0.000 0.046(9)
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'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
K K 0.2009 0.2494 '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'
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 I2 C1A 25(3) . 14_567
C1A C1 C1A 71(10) 2_665 14_567
C1A C1 C1 36(7) 2_665 13_677
C1A C1 C1 36(7) 14_567 13_677
C1A C1 I2 155(9) 2_665 .
C1A C1 I2 84(5) 14_567 .
C1 C1 I2 120(3) 13_677 .
C1A C1 I2 84(5) 2_665 16_557
C1A C1 I2 155(9) 14_567 16_557
C1 C1 I2 120(3) 13_677 16_557
I2 C1 I2 121(5) . 16_557
C1 C1A C1 109(10) 15_657 3_565
C1 C1A C1A 54(7) 15_657 13_667
C1 C1A C1A 54(7) 3_565 13_667
C1 C1A I2 71(5) 15_657 15_657
C1 C1A I2 179(8) 3_565 15_657
C1A C1A I2 125.0(17) 13_667 15_657
C1 C1A I2 179(8) 15_657 18_567
C1 C1A I2 71(5) 3_565 18_567
C1A C1A I2 125.0(17) 13_667 18_567
I2 C1A I2 110(3) 15_657 18_567
O1 K1 O1 180(7) 15_547 3_765
O1 K1 O1 60.000(7) 15_547 .
O1 K1 O1 120.000(8) 3_765 .
O1 K1 O1 120.000(5) 15_547 14_667
O1 K1 O1 60.000(5) 3_765 14_667
O1 K1 O1 60.000(5) . 14_667
O1 K1 O1 120.000(8) 15_547 13_757
O1 K1 O1 60.000(8) 3_765 13_757
O1 K1 O1 180.000(7) . 13_757
O1 K1 O1 120.000(7) 14_667 13_757
O1 K1 O1 60.000(5) 15_547 2_645
O1 K1 O1 120.000(9) 3_765 2_645
O1 K1 O1 120.00(2) . 2_645
O1 K1 O1 180.00(2) 14_667 2_645
O1 K1 O1 60.000(8) 13_757 2_645
O1 K1 K2 90.000(6) 15_547 .
O1 K1 K2 90.000(6) 3_765 .
O1 K1 K2 90.000(1) . .
O1 K1 K2 90.000(1) 14_667 .
O1 K1 K2 90.000(1) 13_757 .
O1 K1 K2 90.000(1) 2_645 .
O1 K1 K2 90.000(6) 15_547 1_556
O1 K1 K2 90.000(6) 3_765 1_556
O1 K1 K2 90.000(1) . 1_556
O1 K1 K2 90.000(1) 14_667 1_556
O1 K1 K2 90.000(1) 13_757 1_556
O1 K1 K2 90.000(1) 2_645 1_556
K2 K1 K2 180.0 . 1_556
K1 K2 K1 180.0 1_554 .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
I2 C1 2.07(6) .
I2 C1A 2.18(5) 14_567
C1 C1A 0.94(9) 2_665
C1 C1A 0.94(9) 14_567
C1 C1 1.5(2) 13_677
C1 I2 2.07(6) 16_557
C1A C1 0.94(9) 15_657
C1A C1 0.94(9) 3_565
C1A C1A 1.09(16) 13_667
C1A I2 2.18(5) 15_657
C1A I2 2.18(5) 18_567
K1 O1 3.33(11) 15_547
K1 O1 3.33(11) 3_765
K1 O1 3.33(11) .
K1 O1 3.33(11) 14_667
K1 O1 3.33(11) 13_757
K1 O1 3.33(11) 2_645
K1 K2 4.4665(15) .
K1 K2 4.4665(15) 1_556
K2 K1 4.4665(15) 1_554
