Bis[(1,4,7,10,13,16-hexaoxocyclooctadecane)caesium(I)] di-μ~2~-diselenido-bis[selenidoarsenate(III)]
Tobias Van Almsick; William S. Sheldrick; Acta Crystallographica Section E 61 (2005) m2431–m2433; doi:10.1107/S1600536805034604

data_2207163
_publ_section_title
;
 Bis[(1,4,7,10,13,16-hexaoxocyclooctadecane)caesium(I)]
 di-\m~2~-diselenido-bis[selenidoarsenate(III)]
;
_journal_coeditor_code           BT6769
_journal_issue                   11
_journal_name_full               'Acta Crystallographica Section E'
_journal_page_first              m2431
_journal_page_last               m2433
_journal_paper_doi               10.1107/S1600536805034604
_journal_volume                  61
_journal_year                    2005
_chemical_formula_iupac          '[Cs (C12 H24 O6)]2 [As2 Se6]'
_chemical_formula_moiety         'C24 H48 As2 Cs2 O12 Se6'
_chemical_formula_sum            'C24 H48 As2 Cs2 O12 Se6'
_chemical_formula_weight         1418.04
_chemical_name_common            'not relevant'
_chemical_name_systematic
;
Bis[(1,4,7,10,13,16-hexaoxocyclooctadecane)caesium(I)]
di-\m~2~-diselenido-bis[selenidoarsenate(III)]
;
_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-97
_cell_angle_alpha                90.00
_cell_angle_beta                 102.77(3)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   21.930(4)
_cell_length_b                   8.4753(17)
_cell_length_c                   24.041(5)
_cell_measurement_reflns_used    36
_cell_measurement_temperature    292(2)
_cell_measurement_theta_max      17.135
_cell_measurement_theta_min      4.583
_cell_volume                     4357.8(16)
_computing_cell_refinement       'Siemens R3m/V'
_computing_data_collection       'Siemens R3m/V (Siemens, 1989)'
_computing_data_reduction        'XDISK (Siemens, 1989)'
_computing_molecular_graphics    'SHELXTL-Plus (Sheldrick, 1995)'
_computing_publication_material  SHELXL97
_computing_structure_refinement  'SHELXL97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS97 (Sheldrick, 1997)'
_diffrn_ambient_temperature      292(2)
_diffrn_measured_fraction_theta_full 0.989
_diffrn_measured_fraction_theta_max 0.989
_diffrn_measurement_device_type  'Siemens P4 four-circle'
_diffrn_measurement_method       \w
_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  0.0591
_diffrn_reflns_av_sigmaI/netI    0.0796
_diffrn_reflns_limit_h_max       26
_diffrn_reflns_limit_h_min       0
_diffrn_reflns_limit_k_max       10
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       27
_diffrn_reflns_limit_l_min       -28
_diffrn_reflns_number            7836
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         25.10
_diffrn_reflns_theta_min         2.56
_diffrn_standards_decay_%        20
_diffrn_standards_interval_count 100
_diffrn_standards_number         3
_exptl_absorpt_coefficient_mu    8.239
_exptl_absorpt_correction_T_max  0.315
_exptl_absorpt_correction_T_min  0.175
_exptl_absorpt_correction_type   psi-scan
_exptl_absorpt_process_details   '(XPREP in SHELXTL-Plus; Sheldrick, 1995)'
_exptl_crystal_colour            orange
_exptl_crystal_density_diffrn    2.161
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             2672
_exptl_crystal_size_max          0.23
_exptl_crystal_size_mid          0.19
_exptl_crystal_size_min          0.14
_refine_diff_density_max         0.698
_refine_diff_density_min         -1.245
_refine_ls_extinction_coef       0.00070(7)
_refine_ls_extinction_expression
'Fc^*^ = kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^'
_refine_ls_extinction_method     SHELXL97
_refine_ls_goodness_of_fit_ref   0.944
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     416
_refine_ls_number_reflns         7578
_refine_ls_number_restraints     36
_refine_ls_restrained_S_all      0.943
_refine_ls_R_factor_all          0.1107
_refine_ls_R_factor_gt           0.0515
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w = 1/[\s^2^(Fo^2^)+(0.061P)^2^] where P = (Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1060
_refine_ls_wR_factor_ref         0.1226
_reflns_number_gt                4539
_reflns_number_total             7613
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            bt6769.cif
_cod_data_source_block           I
_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:

'_chemical_melting_point' value 'not measured' was changed to '?' -
the value is undefined or not given.

Automatic conversion script
Id: cif_fix_values 1646 2011-03-28 12:23:43Z adriana 

The following automatic conversions were performed:

'_chemical_melting_point' value 'not measured' was changed to '?' -
the value is undefined or not given.

'_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_values 1715 2011-07-08 13:25:40Z adriana 
;
_cod_original_cell_volume        4357.8(15)
_cod_original_sg_symbol_H-M      'P 21/n'
_cod_database_code               2207163
_cod_database_fobs_code          2207163