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_7009402
_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 S'
_chemical_formula_weight         725.09
_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                 92.72(4)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   10.680(5)
_cell_length_b                   16.110(1)
_cell_length_c                   24.857(1)
_cell_measurement_reflns_used    25
_cell_measurement_temperature    213(1)
_cell_measurement_theta_max      53
_cell_measurement_theta_min      22
_cell_volume                     4272(2)
_computing_cell_refinement       'Siemens XSCANS'
_computing_data_collection       'Siemens XSCANS'
_computing_data_reduction        'Siemens SHELXTL 5.0'
_computing_molecular_graphics    'Siemens SHELXTL 5.0'
_computing_publication_material  'Siemens SHELXTL 5.0'
_computing_structure_refinement  'SHELXL-93 (Sheldrick, 1993)'
_computing_structure_solution    'SHELXS-86 (Sheldrick, 1990)'
_diffrn_ambient_temperature      213(1)
_diffrn_measurement_device       'Siemens R3m/V'
_diffrn_measurement_method       omega
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54178
_diffrn_reflns_av_R_equivalents  0.0000
_diffrn_reflns_av_sigmaI/netI    0.1031
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       25
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_number            4865
_diffrn_reflns_theta_max         52.60
_diffrn_reflns_theta_min         3.27
_diffrn_standards_decay_%        No
_diffrn_standards_interval_count 198
_diffrn_standards_number         2
_exptl_absorpt_coefficient_mu    1.897
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.127
_exptl_crystal_description       needle
_exptl_crystal_F_000             1584
_exptl_crystal_size_max          0.35
_exptl_crystal_size_mid          0.10
_exptl_crystal_size_min          0.08
_refine_diff_density_max         0.722
_refine_diff_density_min         -0.818
_refine_diff_density_rms         0.093
_refine_ls_extinction_coef       N/A
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_all   1.068
_refine_ls_goodness_of_fit_obs   1.171
_refine_ls_hydrogen_treatment    riding
_refine_ls_matrix_type           full
_refine_ls_number_parameters     438
_refine_ls_number_reflns         4860
_refine_ls_number_restraints     41
_refine_ls_restrained_S_all      1.084
_refine_ls_restrained_S_obs      1.169
_refine_ls_R_factor_all          0.1471
_refine_ls_R_factor_obs          0.0999
_refine_ls_shift/esd_max         -0.001
_refine_ls_shift/esd_mean        0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.1528P)^2^+4.9246P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.2788
_refine_ls_wR_factor_obs         0.2416
_reflns_number_observed          3214
_reflns_number_total             4865
_reflns_observed_criterion       >2sigma(I)
_cod_data_source_file            b000665n.txt
_cod_data_source_block           Compound_3
_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 'calc
w=1/[\s^2^(Fo^2^)+(0.1528P)^2^+4.9246P] 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^)+(0.1528P)^2^+4.9246P] 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        4271.9(38)
_cod_original_sg_symbol_H-M      P2(1)/n
_cod_database_code               7009402
_diffrn_measurement_time         'constant; 15.00\%/min. in \w'
_diffrn_measurement_range        0.90
_refine_ls_weighting_scheme_1    0.1528
_refine_ls_weighting_scheme_2    4.9246