Formation of separated versus contact ion pairs in alkali metal thiolates and selenolates
Chadwick, Scott; Englich, Ulrich; Ruhlandt-Senge, Karin; Watson, Charles; Bruce, Alice E.; Bruce, Mitchell R. M.; Journal of the Chemical Society, Dalton Transactions  (2000) 2167–; doi:10.1039/b000665n

data_7009400
_publ_section_title
;
 Formation of separated versus contact ion pairs in alkali metal
 thiolates and selenolates
;
_journal_issue                   13
_journal_name_full
'Journal of the Chemical Society, Dalton Transactions'
_journal_page_first              2167
_journal_paper_doi               10.1039/b000665n
_journal_year                    2000
_chemical_formula_sum            'C38 H69 Na O8 S'
_chemical_formula_weight         708.98
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL
_cell_angle_alpha                90.00
_cell_angle_beta                 92.41(3)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   10.598(3)
_cell_length_b                   16.124(6)
_cell_length_c                   24.430(8)
_cell_measurement_reflns_used    28
_cell_measurement_temperature    126(2)
_cell_measurement_theta_max      13
_cell_measurement_theta_min      11
_cell_volume                     4171(2)
_computing_cell_refinement       'Siemens P4'
_computing_data_collection       'Siemens P4'
_computing_data_reduction        'XDISK, SHELXTL-Plus, Siemens (1994)'
_computing_molecular_graphics    'XP, SHELXTL-Plus, Siemens (1994)'
_computing_publication_material  'XCIF, SHELXTL-Plus, Siemens (1994)'
_computing_structure_refinement  'XL-93 (Sheldrick, 1994)'
_computing_structure_solution    'XS-94 (Sheldrick, 1994)'
_diffrn_ambient_temperature      126(2)
_diffrn_measurement_device       'Siemens P4'
_diffrn_measurement_method       Wyckoff
_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  0.0665
_diffrn_reflns_av_sigmaI/netI    0.0890
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       29
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_number            8533
_diffrn_reflns_theta_max         25.51
_diffrn_reflns_theta_min         1.51
_diffrn_standards_decay_%        stable
_diffrn_standards_interval_count 197
_diffrn_standards_number         3
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_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.129
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    n/d
_exptl_crystal_description       block
_exptl_crystal_F_000             1552
_exptl_crystal_size_max          1.00
_exptl_crystal_size_mid          0.80
_exptl_crystal_size_min          0.80
_refine_diff_density_max         0.237
_refine_diff_density_min         -0.215
_refine_diff_density_rms         0.051
_refine_ls_extinction_coef       0.0001(2)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     SHELXL
_refine_ls_goodness_of_fit_all   1.015
_refine_ls_goodness_of_fit_obs   1.070
_refine_ls_hydrogen_treatment    none,riding
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_refine_ls_restrained_S_obs      1.070
_refine_ls_R_factor_all          0.1277
_refine_ls_R_factor_obs          0.0654
_refine_ls_shift/esd_max         0.000
_refine_ls_shift/esd_mean        0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0511P)^2^+1.7821P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.1687
_refine_ls_wR_factor_obs         0.1332
_reflns_number_observed          4511
_reflns_number_total             7768
_reflns_observed_criterion       >2sigma(I)
_cod_data_source_file            b000665n.txt
_cod_data_source_block           Compound_1
_cod_depositor_comments
;
The following automatic conversions were performed:

'_exptl_crystal_density_meas' value 'n/d' was changed to '?' - the
value is perceived as not measured.

Automatic conversion script
Id: cif_fix_values 3008 2015-01-20 13:52:24Z robertas 

The following automatic conversions were performed:

'_refine_ls_weighting_scheme' value 'calc
w=1/[\s^2^(Fo^2^)+(0.0511P)^2^+1.7821P] where P=(Fo^2^+2Fc^2^)/3' was
changed to 'calc'. New tag '_refine_ls_weighting_details' was
created. The value of the new tag was set to
'w=1/[\s^2^(Fo^2^)+(0.0511P)^2^+1.7821P] where P=(Fo^2^+2Fc^2^)/3'.

Automatic conversion script
Id: cif_fix_values 3143 2015-03-26 13:38:13Z robertas 
;
_cod_original_cell_volume        4171.0(24)
_cod_original_sg_symbol_H-M      P2(1)/n
_cod_database_code               7009400