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_7009403
_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 K O8 Se'
_chemical_formula_weight         771.99
_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                 93.60(3)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   10.778(2)
_cell_length_b                   16.129(3)
_cell_length_c                   25.169(5)
_cell_measurement_reflns_used    25
_cell_measurement_temperature    213(2)
_cell_measurement_theta_max      22
_cell_measurement_theta_min      10
_cell_volume                     4366.7(14)
_computing_cell_refinement       'TEXSAN, Molecular Structure Corporation'
_computing_data_collection       'TEXSAN, Molecular Structure Corporation'
_computing_data_reduction        'XPREP, SHELXTL-Plus, Siemens (1994)'
_computing_molecular_graphics    'XP, SHELXTL-Plus, Siemens (1994)'
_computing_publication_material  'XCIF, SHELXTL-Plus, Siemens (1994)'
_computing_structure_refinement  'SHELXL-93 (Sheldrick, 1993)'
_computing_structure_solution    'SHELXS-86 (Sheldrick, 1990)'
_diffrn_ambient_temperature      213(2)
_diffrn_measurement_device       'Rigaku AFC5S'
_diffrn_measurement_method       omega
_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  0.0472
_diffrn_reflns_av_sigmaI/netI    0.0974
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       0
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       29
_diffrn_reflns_limit_l_min       -29
_diffrn_reflns_number            8114
_diffrn_reflns_theta_max         25.01
_diffrn_reflns_theta_min         1.50
_diffrn_standards_decay_%        -1.7
_diffrn_standards_interval_count 150
_diffrn_standards_number         3
_exptl_absorpt_coefficient_mu    0.998
_exptl_absorpt_correction_T_max  1.0000
_exptl_absorpt_correction_T_min  0.7129
_exptl_absorpt_correction_type   'Psi Scans'
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.174
_exptl_crystal_description       block
_exptl_crystal_F_000             1656
_exptl_crystal_size_max          0.4
_exptl_crystal_size_mid          0.2
_exptl_crystal_size_min          0.07
_refine_diff_density_max         0.474
_refine_diff_density_min         -0.368
_refine_diff_density_rms         0.065
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_all   1.008
_refine_ls_goodness_of_fit_obs   1.102
_refine_ls_hydrogen_treatment    riding
_refine_ls_matrix_type           full
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_refine_ls_number_reflns         7672
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_refine_ls_restrained_S_obs      1.102
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_refine_ls_R_factor_obs          0.0575
_refine_ls_shift/esd_max         -0.002
_refine_ls_shift/esd_mean        0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0617P)^2^+2.9628P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.1578
_refine_ls_wR_factor_obs         0.1280
_reflns_number_observed          4424
_reflns_number_total             7674
_reflns_observed_criterion       >2sigma(I)
_cod_data_source_file            b000665n.txt
_cod_data_source_block           Compound_4
_cod_depositor_comments
;
The following automatic conversions were performed:
'_symmetry_cell_setting' value 'Monoclinic' changed to 'monoclinic'
according to '/home/saulius/struct/CIF-dictionaries/cif_core.dic'
dictionary named 'cif_core.dic' version 2.4.1 from 2010-06-29.

Automatic conversion script
Id: cif_fix_enum 1527 2010-12-29 10:47:43Z saulius 

The following automatic conversions were performed:

'_refine_ls_weighting_scheme' value
'w=1/[&Gs&^2&0(Fo&^2&0)+(0.0617P)&^2&0+2.9628P]' was changed to
'calc'. New tag '_refine_ls_weighting_details' was created. The value
of the new tag was set to
'w=1/[&Gs&^2&0(Fo&^2&0)+(0.0617P)&^2&0+2.9628P]'.

Automatic conversion script
Id: cif_fix_values 3143 2015-03-26 13:38:13Z robertas 
;
_cod_original_sg_symbol_H-M      P2(1)/n
_cod_database_code               7009403