Sodium thioether macrocyclic chemistry: remarkable homoleptic octathia coordination to Na(+).
Champion, Martin J. D.; Dyke, John M.; Levason, William; Light, Mark E.; Pugh, David; Bhakhoa, Hanusha; Rhyman, Lydia; Ramasami, Ponnadurai; Reid, Gillian; Inorganic chemistry 54 (2015) 2497–2499; doi:10.1021/acs.inorgchem.5b00156

data_4346067
_publ_section_title
;
 Sodium thioether macrocyclic chemistry: remarkable homoleptic octathia
 coordination to Na(+).
;
_journal_issue                   6
_journal_name_full               'Inorganic chemistry'
_journal_page_first              2497
_journal_page_last               2499
_journal_paper_doi               10.1021/acs.inorgchem.5b00156
_journal_volume                  54
_journal_year                    2015
_chemical_formula_moiety         'C16 H32 Na S8, C32 H12 B F24'
_chemical_formula_sum            'C48 H44 B F24 Na S8'
_chemical_formula_weight         1367.11
_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   geom
_atom_sites_solution_primary     direct
_audit_creation_date             2014-09-04
_audit_creation_method
;
Olex2 1.2
(compiled 2014.08.28 svn.r2986 for OlexSys, GUI svn.r4874)
;
_cell_angle_alpha                80.074(5)
_cell_angle_beta                 72.780(4)
_cell_angle_gamma                89.917(6)
_cell_formula_units_Z            2
_cell_length_a                   12.8461(16)
_cell_length_b                   12.9256(17)
_cell_length_c                   18.696(2)
_cell_measurement_reflns_used    7007
_cell_measurement_temperature    100
_cell_measurement_theta_max      27.5
_cell_measurement_theta_min      2.4
_cell_volume                     2916.8(6)
_computing_cell_refinement
;
CrystalClear-SM Expert 2.1 b29 (Rigaku, 2013)
;
_computing_data_collection
;
CrystalClear-SM Expert 2.1 b29 (Rigaku, 2013)
;
_computing_data_reduction
;
CrystalClear-SM Expert 2.1 b29 (Rigaku, 2013)
;
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2008)'
_computing_structure_solution    'ShelXS (Sheldrick, 2008)'
_diffrn_ambient_temperature      100
_diffrn_detector                 CCD
_diffrn_detector_area_resol_mean 28.5714
_diffrn_measured_fraction_theta_full 0.981
_diffrn_measured_fraction_theta_max 0.983
_diffrn_measurement_details
;
scan:
	Number of images: 128
	           Slice: -110.0000 - 18.0000
	     Image width: 1.0000
	        Exp time: 6.0000
	   Rotation axis: Omega
	           Omega: 0.0000
	           Kappa: -70.0000
	             Phi: 225.0000
	             XTD: 44.9421
	          2theta: -19.8956
scan:
	Number of images: 99
	           Slice: -85.0000 - 14.0000
	     Image width: 1.0000
	        Exp time: 6.0000
	   Rotation axis: Omega
	           Omega: 0.0000
	           Kappa: -70.0000
	             Phi: 90.0000
	             XTD: 44.9421
	          2theta: -19.8956
scan:
	Number of images: 60
	           Slice: -80.0000 - -20.0000
	     Image width: 1.0000
	        Exp time: 6.0000
	   Rotation axis: Omega
	           Omega: 0.0000
	           Kappa: 0.0000
	             Phi: 270.0000
	             XTD: 44.9421
	          2theta: -19.8956
scan:
	Number of images: 55
	           Slice: -67.0000 - -12.0000
	     Image width: 1.0000
	        Exp time: 6.0000
	   Rotation axis: Omega
	           Omega: 0.0000
	           Kappa: -70.0000
	             Phi: 0.0000
	             XTD: 44.9421
	          2theta: -19.8956
scan:
	Number of images: 30
	           Slice: -20.0000 - 10.0000
	     Image width: 1.0000
	        Exp time: 6.0000
	   Rotation axis: Omega
	           Omega: 0.0000
	           Kappa: 0.0000
	             Phi: 0.0000
	             XTD: 44.9421
	          2theta: -19.8956
;
_diffrn_measurement_device
;
AFC12 (Right): Kappa 3 circle
;
_diffrn_measurement_device_type  'Rigaku Saturn724+ (2x2 bin mode)'
_diffrn_measurement_method       'profile data from \w-scans'
_diffrn_measurement_specimen_support Fiber
_diffrn_orient_matrix_type       d*Trek
_diffrn_orient_matrix_UB_11      0.014677
_diffrn_orient_matrix_UB_12      0.069622
_diffrn_orient_matrix_UB_13      0.039971
_diffrn_orient_matrix_UB_21      0.076661
_diffrn_orient_matrix_UB_22      -0.015766
_diffrn_orient_matrix_UB_23      0.007773
_diffrn_orient_matrix_UB_31      -0.002347
_diffrn_orient_matrix_UB_32      0.012335
_diffrn_orient_matrix_UB_33      -0.055525
_diffrn_radiation_monochromator  Confocal
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0440
_diffrn_reflns_av_unetI/netI     0.0640
_diffrn_reflns_Laue_measured_fraction_full 0.981
_diffrn_reflns_Laue_measured_fraction_max 0.983
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_number            24927
_diffrn_reflns_point_group_measured_fraction_full 0.981
_diffrn_reflns_point_group_measured_fraction_max 0.983
_diffrn_reflns_theta_full        27.500
_diffrn_reflns_theta_max         27.484
_diffrn_reflns_theta_min         2.964
_diffrn_source                   'Sealed Tube'
_diffrn_source_current           55.0
_diffrn_source_power             2.5
_diffrn_source_voltage           45.0
_exptl_absorpt_coefficient_mu    0.425
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.770
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrystalClear-SM Expert 2.1 b29 (Rigaku, 2013)
;
_exptl_crystal_colour            colourless
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.555
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             1384
_exptl_crystal_size_max          0.12
_exptl_crystal_size_mid          0.12
_exptl_crystal_size_min          0.07
_refine_diff_density_max         1.054
_refine_diff_density_min         -0.512
_refine_diff_density_rms         0.122
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.084
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     739
_refine_ls_number_reflns         13164
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.084
_refine_ls_R_factor_all          0.0989
_refine_ls_R_factor_gt           0.0847
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0640P)^2^+22.2120P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2255
_refine_ls_wR_factor_ref         0.2316
_reflns_Friedel_coverage         0.000
_reflns_number_gt                10581
_reflns_number_total             13164
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ic5b00156_si_002.cif
_cod_data_source_block           '[Na([24]aneS8)][BArF]'
_cod_depositor_comments
;
The following automatic conversions were performed:

data item '_exptl_absorpt_correction_type' value 'Multi-scan' was
changed to 'multi-scan' in accordance with the
/home/saulius/struct/COD-crude-data/automatic-downloads/DataCite-retrospective/ACS/depositions/lib/dictionaries/cif_core.dic
dictionary named 'cif_core.dic' version 2.4.2 last updated on
2011-04-26.

Automatic conversion script
Id: cif_fix_values 6909 2019-04-08 15:41:33Z antanas 
;
_cod_database_code               4346067
_shelxl_version_number           2014-3
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
2.a Secondary CH2 refined with riding coordinates:
 C1(H1A,H1B), C2(H2A,H2B), C3(H3A,H3B), C4(H4A,H4B), C5(H5A,H5B), C6(H6A,H6B),
 C7(H7A,H7B), C8(H8A,H8B), C9(H9A,H9B), C10(H10A,H10B), C11(H11A,H11B),
 C12(H12A,H12B), C13(H13A,H13B), C14(H14A,H14B), C15(H15A,H15B), C16(H16A,H16B)
2.b Aromatic/amide H refined with riding coordinates:
 C18(H18), C20(H20), C22(H22), C26(H26), C28(H28), C30(H30), C34(H34),
 C36(H36), C38(H38), C42(H42), C44(H44), C46(H46)
;
_shelx_res_checksum              51118
_shelx_hkl_checksum              98603
_olex2_submission_special_instructions 'No special instructions were received'