Coordination structure and extraction behavior of a silver ion with N-substituted-9-aza-3,6,12,15-tetrathiaheptadecanes: significant effect of Ph-C-N framework on the extractability.
Iwatsuki, Satoshi; Ichiyama, Atsushi; Tanooka, Syogo; Toyama, Mari; Katagiri, Kosuke; Kawahata, Masatoshi; Yamaguchi, Kentaro; Danjo, Hiroshi; Chayama, Kenji; Dalton transactions (Cambridge, England : 2003) 45 (2016) 12548–12558; doi:10.1039/c6dt01535b

data_7039899
_publ_section_title
;
 Coordination structure and extraction behavior of a silver ion with
 N-substituted-9-aza-3,6,12,15-tetrathiaheptadecanes: significant effect
 of Ph-C-N framework on the extractability.
;
_journal_issue                   31
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              12548
_journal_page_last               12558
_journal_paper_doi               10.1039/c6dt01535b
_journal_volume                  45
_journal_year                    2016
_chemical_formula_moiety         'C25 H37 Ag N S4, B F4'
_chemical_formula_sum            'C25 H37 Ag B F4 N O0.5 S4'
_chemical_formula_weight         682.47
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_audit_creation_date             2016-06-23
_audit_creation_method
;
Olex2 1.2
(compiled Feb 16 2016 13:09:46 for OlexSys, GUI svn.r5155)
;
_audit_update_record
;
2016-06-24 deposited with the CCDC.
2016-07-12 downloaded from the CCDC.
;
_cell_angle_alpha                74.344(4)
_cell_angle_beta                 88.806(4)
_cell_angle_gamma                81.965(4)
_cell_formula_units_Z            2
_cell_length_a                   8.7519(5)
_cell_length_b                   10.4885(5)
_cell_length_c                   16.6546(8)
_cell_measurement_reflns_used    4939
_cell_measurement_temperature    173
_cell_measurement_theta_max      73.2300
_cell_measurement_theta_min      5.5030
_cell_volume                     1457.40(13)
_computing_cell_refinement       'CrysAlisPro 1.171.39.3a (Rigaku OD, 2015)'
_computing_data_collection       'CrysAlisPro 1.171.39.3a (Rigaku OD, 2015)'
_computing_data_reduction        'CrysAlisPro 1.171.39.3a (Rigaku OD, 2015)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_computing_structure_solution    'ShelXT (Sheldrick, 2015)'
_diffrn_ambient_temperature      173
_diffrn_detector                 'CCD plate'
_diffrn_measured_fraction_theta_full 0.989
_diffrn_measured_fraction_theta_max 0.938
_diffrn_measurement_details
;
List of Runs (angles in degrees, time in seconds):

  1  \w     18.00  89.00   0.50    1.74    --    0.00  38.00 -30.00  142
  2  \w     11.00 131.00   0.50    6.98    --   98.00 -61.00 -90.00  240
  3  \w    113.00 139.00   0.50    6.98    --   98.00 -82.00 -90.00   52
  4  \w     92.00 119.00   0.50    6.98    --   98.00 -82.00-150.00   54
  5  \w     80.00 107.00   0.50    6.98    --   98.00 -82.00-180.00   54
  6  \w     93.00 147.00   0.50    6.98    --   98.00 -30.00 -60.00  108
  7  \w    125.00 186.00   0.50    6.98    --   98.00  30.00 120.00  122
  8  \w     85.00 112.00   0.50    6.98    --   98.00 -82.00   0.00   54
  9  \w     61.00 137.00   0.50    6.98    --   98.00 -82.00 -60.00  152
 10  \w     52.00 146.00   0.50    6.98    --   98.00  30.00-120.00  188
 11  \w     51.00 112.00   0.50    6.98    --   98.00  30.00 120.00  122
 12  \w     23.00  60.00   0.50    6.98    --   98.00 -30.00 -60.00   74
 13  \w     17.00  78.00   0.50    6.98    --   98.00 -82.00-180.00  122
 14  \w     16.00  53.00   0.50    6.98    --   98.00 -82.00  30.00   74
 15  \w     43.00 126.00   0.50    6.98    --   98.00 -82.00  90.00  166
 16  \w     27.00 172.00   0.50    6.98    --   98.00  15.00-150.00  290
 17  \w     13.00  86.00   0.50    6.98    --   98.00 -82.00 -90.00  146
 18  \w      9.00 139.00   0.50    6.98    --   98.00 -82.00 120.00  260
 19  \w    -17.00  89.00   0.50    1.74    --    0.00  57.00 -90.00  212
 20  \w    -17.00  35.00   0.50    1.74    --    0.00 -57.00 -60.00  104
 21  \w    -66.00 -17.00   0.50    1.74    --    0.00 -82.00-120.00   98
 22  \w    -58.00 -31.00   0.50    1.74    --    0.00 -57.00 -60.00   54
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'XtaLAB Pro: Kappa dual home'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      -0.0960502000
_diffrn_orient_matrix_UB_12      0.1012632000
_diffrn_orient_matrix_UB_13      -0.0718606000
_diffrn_orient_matrix_UB_21      0.1120316000
_diffrn_orient_matrix_UB_22      -0.0427799000
_diffrn_orient_matrix_UB_23      -0.0635592000
_diffrn_orient_matrix_UB_31      -0.0991754000
_diffrn_orient_matrix_UB_32      -0.1079123000
_diffrn_orient_matrix_UB_33      -0.0052531000
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0456
_diffrn_reflns_av_unetI/netI     0.0526
_diffrn_reflns_Laue_measured_fraction_full 0.989
_diffrn_reflns_Laue_measured_fraction_max 0.938
_diffrn_reflns_limit_h_max       7
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            13332
_diffrn_reflns_point_group_measured_fraction_full 0.989
_diffrn_reflns_point_group_measured_fraction_max 0.938
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         75.007
_diffrn_reflns_theta_min         4.421
_diffrn_source                   'fine-focus sealed X-ray tube'
_diffrn_source_type              'Enhance (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    8.606
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.62064
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.39.3a (Rigaku Oxford Diffraction, 2015)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            'clear colourless'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.555
_exptl_crystal_description       needle
_exptl_crystal_F_000             700
_exptl_crystal_size_max          0.15
_exptl_crystal_size_mid          0.07
_exptl_crystal_size_min          0.03
_refine_diff_density_max         1.243
_refine_diff_density_min         -0.487
_refine_diff_density_rms         0.100
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.064
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     327
_refine_ls_number_reflns         5618
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.064
_refine_ls_R_factor_all          0.0586
_refine_ls_R_factor_gt           0.0494
_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/[\s^2^(Fo^2^)+(0.0825P)^2^+0.3956P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1306
_refine_ls_wR_factor_ref         0.1381
_reflns_Friedel_coverage         0.000
_reflns_number_gt                4603
_reflns_number_total             5618
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c6dt01535b2.cif
_cod_data_source_block           exp_66
_cod_depositor_comments
'Adding full bibliography for 7039898--7039899.cif.'
_cod_original_formula_sum        'C25 H37 Ag B F4 N O0.50 S4'
_cod_database_code               7039899
_chemical_oxdiff_formula         C25H37AgBF4NS4
_chemical_oxdiff_usercomment     AgL3BF4_needle
_reflns_odcompleteness_completeness 98.99
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     66.97
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2.a Ternary CH refined with riding coordinates:
 C7(H7)
2.b Secondary CH2 refined with riding coordinates:
 C16(H16A,H16B), C21(H21A,H21B), C20(H20A,H20B), C14(H14A,H14B), C23(H23A,
 H23B), C15(H15A,H15B), C22(H22A,H22B), C17(H17A,H17B), C18(H18A,H18B),
 C24(H24A,H24B)
2.c Aromatic/amide H refined with riding coordinates:
 C9(H9), C2(H2), C6(H6), C13(H13), C11(H11), C4(H4), C10(H10), C12(H12),
 C5(H5), C3(H3)
2.d Idealised Me refined as rotating group:
 C25(H25A,H25B,H25C), C19(H19A,H19B,H19C)
;
_shelx_res_checksum              64101
_shelx_shelxl_version_number     2014/7
_olex2_submission_special_instructions 'No special instructions were received'
_oxdiff_exptl_absorpt_empirical_details
;
Empirical correction (ABSPACK) includes:
- Absorption correction using spherical harmonics
- Frame scaling
- Detector area scaling
;
_oxdiff_exptl_absorpt_empirical_full_max 2.045
_oxdiff_exptl_absorpt_empirical_full_min 0.601