Two crown-ether-coordinated caesium halogen salts
van Well, Natalija; Klein, Christian; Ritter, Franz; Assmus, Wolf; Krellner, Cornelius; Bolte, Michael; Acta Crystallographica Section C 70 (2014) 455–459; doi:10.1107/S2053229614006809

data_2019525
_publ_section_title
;
 Two crown-ether-coordinated caesium halogen salts
;
_journal_coeditor_code           SK3535
_journal_issue                   5
_journal_name_full               'Acta Crystallographica Section C'
_journal_page_first              455
_journal_page_last               459
_journal_paper_doi               10.1107/S2053229614006809
_journal_volume                  70
_journal_year                    2014
_chemical_formula_iupac          '[Cs Br (C12 H24 O6) (H2 O)] , H2 O'
_chemical_formula_moiety         'C12 H26 Br Cs O7, H2 O'
_chemical_formula_sum            'C12 H28 Br Cs O8'
_chemical_formula_weight         513.15
_chemical_name_systematic
;
Di-\m-bromido-bis[aqua(1,4,7,10,13,16-hexaoxacyclooctadecane)caesium(I)]
dihydrate
;
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2yn'
_space_group_name_H-M_alt        'P 1 21/n 1'
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 1'
_atom_sites_solution_hydrogens   mixed
_audit_creation_method           SHELXL2013
_cell_angle_alpha                90
_cell_angle_beta                 97.618(4)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   10.7379(5)
_cell_length_b                   8.4198(3)
_cell_length_c                   21.4724(11)
_cell_measurement_reflns_used    44249
_cell_measurement_temperature    173(2)
_cell_measurement_theta_max      30.6
_cell_measurement_theta_min      2.3
_cell_volume                     1924.21(15)
_computing_cell_refinement       'X-AREA (Stoe & Cie, 2001)'
_computing_data_collection       'X-AREA (Stoe & Cie, 2001)'
_computing_data_reduction        'X-AREA (Stoe & Cie, 2001)'
_computing_molecular_graphics    'XP in SHELXTL-Plus (Sheldrick, 2008)'
_computing_publication_material
;
SHELXL97 (Sheldrick, 2008), PLATON (Spek, 2009) and publCIF
(Westrip, 2010)
;
_computing_structure_refinement  'SHELXL97 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      173(2)
_diffrn_measured_fraction_theta_full 0.993
_diffrn_measured_fraction_theta_max 0.989
_diffrn_measurement_device_type  'Stoe IPDSII two-circle'
_diffrn_measurement_method       \w
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0731
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_l_max       30
_diffrn_reflns_limit_l_min       -30
_diffrn_reflns_number            32488
_diffrn_reflns_theta_full        25.000
_diffrn_reflns_theta_max         30.242
_diffrn_reflns_theta_min         2.601
_exptl_absorpt_coefficient_mu    4.032
_exptl_absorpt_correction_T_max  0.531
_exptl_absorpt_correction_T_min  0.398
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   '(X-AREA; Stoe & Cie, 2001)'
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.771
_exptl_crystal_description       block
_exptl_crystal_F_000             1016
_exptl_crystal_size_max          0.280
_exptl_crystal_size_mid          0.230
_exptl_crystal_size_min          0.180
_refine_diff_density_max         1.183
_refine_diff_density_min         -1.175
_refine_ls_extinction_coef       0.0154(7)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     'SHELXL97 (Sheldrick, 2008)'
_refine_ls_goodness_of_fit_ref   1.092
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     216
_refine_ls_number_reflns         5665
_refine_ls_number_restraints     4
_refine_ls_restrained_S_all      1.092
_refine_ls_R_factor_all          0.0371
_refine_ls_R_factor_gt           0.0346
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w = 1/[\s^2^(Fo^2^)+(0.0468P)^2^+1.7410P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0877
_refine_ls_wR_factor_ref         0.0895
_reflns_number_gt                5351
_reflns_number_total             5665
_reflns_threshold_expression     I>2\s(I)
_cod_depositor_comments
;
Adding full bibliography for 2019525--2019526.cif.

2017-07-22
Z value and formula fixed to values more according to usual
chemical conventions.                 miguel
;
_cod_original_formula_sum            'C24 H56 Br2 Cs2 O16'
_cod_original_formula_weight         1026.31
_cod_original_formula_moiety         'C24 H52 Br2 Cs2 O14, 2(H2 O)'
_cod_original_formula_iupac          '[Cs2 Br2 (C12 H24 O6)2 (H2 O)2] , 2H2 O'
_cod_original_formula_units_Z            2
_cod_data_source_file            sk3535sup1.cif
_cod_data_source_block           I
_cod_database_code               2019525
_cod_database_fobs_code          2019525
_shelx_estimated_absorpt_t_min   0.398
_shelx_estimated_absorpt_t_max   0.531
_shelx_hkl_checksum              35441
_shelx_res_checksum              63645
_shelxl_version_number           2.013