#------------------------------------------------------------------------------
#$Date: 2020-07-21 04:41:47 +0300 (Tue, 21 Jul 2020) $
#$Revision: 254422 $
#$URL: file:///home/coder/svn-repositories/cod/cif/7/24/08/7240899.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_7240899
loop_
_publ_author_name
'Kim, Seulgi'
'Park, In-Hyeok'
'Lee, Shim Sung'
'Sim, Wonbo'
'Lee, Jai Young'
_publ_section_title
;
 Alkali metal complexes of bis-o-xylyl-(17-crown-5): from dinuclear
 monomer and dinuclear polymer to sandwich polymer
;
_journal_name_full               CrystEngComm
_journal_paper_doi               10.1039/D0CE00864H
_journal_year                    2020
_chemical_formula_moiety         'C26 H46 I2 Na2 O12'
_chemical_formula_sum            'C26 H46 I2 Na2 O12'
_chemical_formula_weight         850.41
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_atom_sites_solution_hydrogens   mixed
_audit_creation_method           SHELXL-2014/7
_audit_update_record
;
2020-05-22 deposited with the CCDC.	2020-07-20 downloaded from the CCDC.
;
_cell_angle_alpha                67.827(2)
_cell_angle_beta                 85.400(3)
_cell_angle_gamma                79.241(3)
_cell_formula_units_Z            1
_cell_length_a                   8.4111(9)
_cell_length_b                   10.3053(11)
_cell_length_c                   11.1643(12)
_cell_measurement_reflns_used    9773
_cell_measurement_temperature    203(2)
_cell_measurement_theta_max      28.30
_cell_measurement_theta_min      2.99
_cell_volume                     880.34(16)
_computing_cell_refinement       'Bruker SAINT'
_computing_data_collection       'Bruker APEX2'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_structure_solution    'Bruker SHELXTL'
_diffrn_ambient_temperature      203(2)
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       'φ and ω scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0348
_diffrn_reflns_av_unetI/netI     0.0318
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_limit_h_max       8
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_l_max       13
_diffrn_reflns_limit_l_min       -13
_diffrn_reflns_number            14747
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         25.996
_diffrn_reflns_theta_min         2.326
_exptl_absorpt_coefficient_mu    1.864
_exptl_absorpt_correction_T_max  0.963
_exptl_absorpt_correction_T_min  0.935
_exptl_absorpt_correction_type   multi-scan
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.604
_exptl_crystal_description       block
_exptl_crystal_F_000             426
_exptl_crystal_size_max          0.100
_exptl_crystal_size_mid          0.050
_exptl_crystal_size_min          0.040
_refine_diff_density_max         3.012
_refine_diff_density_min         -1.816
_refine_diff_density_rms         0.202
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.094
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     190
_refine_ls_number_reflns         3463
_refine_ls_number_restraints     2
_refine_ls_restrained_S_all      1.094
_refine_ls_R_factor_all          0.0671
_refine_ls_R_factor_gt           0.0654
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[σ²(Fo²)+(0.1302P)²+22.4856P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2656
_refine_ls_wR_factor_ref         0.2666
_reflns_Friedel_coverage         0.000
_reflns_number_gt                3278
_reflns_number_total             3463
_reflns_threshold_expression     'I > 2σ(I)'
_cod_data_source_file            d0ce00864h2.cif
_cod_data_source_block           1
_cod_database_code               7240899
_shelx_shelxl_version_number     2014/7
_shelx_space_group_comment
; 
The symmetry employed for this shelxl refinement is uniquely defined 
by the following loop, which should always be used as a source of 
symmetry information in preference to the above space-group names. 
They are only intended as comments. 
;
_shelx_estimated_absorpt_t_min   0.836
_shelx_estimated_absorpt_t_max   0.929
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-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_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
Na1 Na 0.1389(5) 0.7763(5) 0.2619(4) 0.0305(9) Uani 1 1 d . . . . .
I1 I 0.53435(9) 0.29980(8) 0.35151(7) 0.0360(3) Uani 1 1 d . . . . .
O1 O -0.0081(9) 0.5891(8) 0.2935(7) 0.0297(16) Uani 1 1 d . . . . .
O2 O -0.1441(10) 0.8460(9) 0.3038(8) 0.0326(17) Uani 1 1 d . . . . .
O3 O 0.0946(10) 0.9727(8) 0.3441(8) 0.0320(17) Uani 1 1 d . . . . .
O4 O 0.2760(11) 0.9706(8) 0.1253(8) 0.0337(18) Uani 1 1 d . . . . .
O5 O 0.2179(9) 0.7541(8) 0.0436(8) 0.0313(17) Uani 1 1 d . . . . .
C1 C -0.0999(14) 0.4330(11) 0.0967(11) 0.028(2) Uani 1 1 d . . . . .
H1 H -0.1690 0.3868 0.1632 0.033 Uiso 1 1 calc R U . . .
C2 C 0.0278(13) 0.4816(11) 0.1285(10) 0.027(2) Uani 1 1 d . . . . .
C3 C 0.1296(13) 0.5502(11) 0.0285(11) 0.027(2) Uani 1 1 d . . . . .
C7 C 0.0491(16) 0.4619(12) 0.2683(11) 0.033(2) Uani 1 1 d . . . . .
H7A H -0.0095 0.3869 0.3245 0.039 Uiso 1 1 calc R U . . .
H7B H 0.1642 0.4305 0.2899 0.039 Uiso 1 1 calc R U . . .
C8 C -0.1797(14) 0.6337(13) 0.2754(12) 0.035(3) Uani 1 1 d . . . . .
H8A H -0.2355 0.5514 0.3080 0.042 Uiso 1 1 calc R U . . .
H8B H -0.2046 0.6856 0.1836 0.042 Uiso 1 1 calc R U . . .
C9 C -0.2317(16) 0.7299(14) 0.3519(13) 0.039(3) Uani 1 1 d . . . . .
H9A H -0.3482 0.7658 0.3425 0.047 Uiso 1 1 calc R U . . .
H9B H -0.2090 0.6763 0.4439 0.047 Uiso 1 1 calc R U . . .
C10 C -0.1738(16) 0.9315(14) 0.3796(13) 0.039(3) Uani 1 1 d . . . . .
H10A H -0.1475 0.8733 0.4702 0.047 Uiso 1 1 calc R U . . .
H10B H -0.2883 0.9750 0.3750 0.047 Uiso 1 1 calc R U . . .
C11 C -0.0710(15) 1.0440(13) 0.3284(13) 0.037(3) Uani 1 1 d . . . . .
H11A H -0.0938 1.1001 0.2368 0.044 Uiso 1 1 calc R U . . .
H11B H -0.0923 1.1079 0.3764 0.044 Uiso 1 1 calc R U . . .
C12 C 0.2099(16) 1.0673(14) 0.2847(13) 0.040(3) Uani 1 1 d . . . . .
H12A H 0.3160 1.0225 0.3243 0.048 Uiso 1 1 calc R U . . .
H12B H 0.1758 1.1553 0.3012 0.048 Uiso 1 1 calc R U . . .
C13 C 0.2244(17) 1.1020(14) 0.1426(14) 0.042(3) Uani 1 1 d . . . . .
H13A H 0.1198 1.1490 0.1010 0.051 Uiso 1 1 calc R U . . .
H13B H 0.3037 1.1655 0.1047 0.051 Uiso 1 1 calc R U . . .
C14 C 0.2833(16) 0.9824(13) -0.0057(11) 0.037(3) Uani 1 1 d . . . . .
H14A H 0.3572 1.0475 -0.0549 0.045 Uiso 1 1 calc R U . . .
H14B H 0.1757 1.0206 -0.0443 0.045 Uiso 1 1 calc R U . . .
C15 C 0.3410(15) 0.8406(13) -0.0106(11) 0.035(3) Uani 1 1 d . . . . .
H15A H 0.3641 0.8488 -0.1003 0.042 Uiso 1 1 calc R U . . .
H15B H 0.4410 0.7968 0.0389 0.042 Uiso 1 1 calc R U . . .
C16 C 0.2718(14) 0.6094(13) 0.0510(12) 0.033(2) Uani 1 1 d . . . . .
H16A H 0.3179 0.5506 0.1363 0.039 Uiso 1 1 calc R U . . .
H16B H 0.3561 0.6075 -0.0146 0.039 Uiso 1 1 calc R U . . .
O1S O 0.3538(16) 0.6347(12) 0.3777(13) 0.071(4) Uani 1 1 d D . . . .
H1SA H 0.4390 0.6660 0.3580 0.085 Uiso 1 1 d DR U . . .
H1SB H 0.3829 0.5646 0.3581 0.085 Uiso 1 1 d DR U . . .
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'
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'
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
_geom_angle_publ_flag
O1S Na1 O1 95.3(4) . . ?
O1S Na1 O2 136.6(5) . . ?
O1 Na1 O2 69.1(3) . . ?
O1S Na1 O4 97.7(5) . . ?
O1 Na1 O4 152.3(3) . . ?
O2 Na1 O4 114.9(3) . . ?
O1S Na1 O3 101.2(4) . . ?
O1 Na1 O3 132.0(3) . . ?
O2 Na1 O3 68.1(3) . . ?
O4 Na1 O3 68.9(3) . . ?
O1S Na1 O5 99.3(4) . . ?
O1 Na1 O5 84.5(3) . . ?
O2 Na1 O5 118.1(3) . . ?
O4 Na1 O5 69.3(3) . . ?
O3 Na1 O5 135.2(3) . . ?
C7 O1 C8 112.0(8) . . ?
C7 O1 Na1 126.6(7) . . ?
C8 O1 Na1 114.6(6) . . ?
C10 O2 C9 111.6(9) . . ?
C10 O2 Na1 114.4(7) . . ?
C9 O2 Na1 113.6(7) . . ?
C11 O3 C12 113.4(9) . . ?
C11 O3 Na1 111.2(6) . . ?
C12 O3 Na1 109.9(7) . . ?
C14 O4 C13 114.1(9) . . ?
C14 O4 Na1 111.7(7) . . ?
C13 O4 Na1 115.3(7) . . ?
C15 O5 C16 111.7(9) . . ?
C15 O5 Na1 106.1(6) . . ?
C16 O5 Na1 114.2(6) . . ?
C3 C1 C2 122.8(10) 2_565 . ?
C1 C2 C3 118.0(10) . . ?
C1 C2 C7 119.3(10) . . ?
C3 C2 C7 122.7(10) . . ?
C1 C3 C2 119.2(10) 2_565 . ?
C1 C3 C16 117.9(10) 2_565 . ?
C2 C3 C16 122.9(10) . . ?
O1 C7 C2 112.8(9) . . ?
O1 C8 C9 105.6(9) . . ?
O2 C9 C8 108.7(9) . . ?
O2 C10 C11 108.3(10) . . ?
O3 C11 C10 106.8(10) . . ?
O3 C12 C13 111.9(10) . . ?
O4 C13 C12 106.5(11) . . ?
O4 C14 C15 108.8(10) . . ?
O5 C15 C14 108.8(10) . . ?
O5 C16 C3 109.5(9) . . ?
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Na1 O1S 2.244(12) . ?
Na1 O1 2.384(9) . ?
Na1 O2 2.416(9) . ?
Na1 O4 2.437(9) . ?
Na1 O3 2.479(9) . ?
Na1 O5 2.557(9) . ?
O1 C7 1.432(13) . ?
O1 C8 1.437(14) . ?
O2 C10 1.414(14) . ?
O2 C9 1.429(14) . ?
O3 C11 1.439(14) . ?
O3 C12 1.446(15) . ?
O4 C14 1.419(14) . ?
O4 C13 1.423(14) . ?
O5 C15 1.439(13) . ?
O5 C16 1.448(14) . ?
C1 C3 1.380(16) 2_565 ?
C1 C2 1.387(16) . ?
C2 C3 1.399(15) . ?
C2 C7 1.517(14) . ?
C3 C1 1.380(16) 2_565 ?
C3 C16 1.517(15) . ?
C8 C9 1.524(16) . ?
C10 C11 1.487(18) . ?
C12 C13 1.489(19) . ?
C14 C15 1.471(18) . ?
