Crystal forms of highly “dynamic” 18-crown[6] complexes with M[HSO4] and M[H2PO4] (M+ = NH4+, Rb+, Cs+): thermal behaviour and solid-state preparation
Braga, Dario; Modena, Enrico; Polito, Marco; Rubini, Katia; Grepioni, Fabrizia; New Journal of Chemistry 32 (2008) 1718–; doi:10.1039/b805203d

data_7053748
_publ_section_title
;
 Crystal forms of highly &#x201C;dynamic&#x201D; 18-crown[6] complexes
 with M[HSO4] and M[H2PO4] (M+ = NH4+, Rb+, Cs+): thermal behaviour and
 solid-state preparation
;
_journal_issue                   10
_journal_name_full               'New Journal of Chemistry'
_journal_page_first              1718
_journal_paper_doi               10.1039/b805203d
_journal_volume                  32
_journal_year                    2008
_chemical_formula_sum            'C24 H58 Cs2 O24 S2'
_chemical_formula_weight         1060.64
_chemical_name_systematic
;
?
;
_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                 100.907(6)
_cell_angle_gamma                90.00
_cell_formula_units_Z            2
_cell_length_a                   11.064(4)
_cell_length_b                   8.655(3)
_cell_length_c                   22.644(8)
_cell_measurement_temperature    293(2)
_cell_volume                     2129.2(13)
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 0.924
_diffrn_measured_fraction_theta_max 0.924
_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  0.0427
_diffrn_reflns_av_sigmaI/netI    0.0494
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_l_max       29
_diffrn_reflns_limit_l_min       -28
_diffrn_reflns_number            16927
_diffrn_reflns_theta_full        27.95
_diffrn_reflns_theta_max         27.95
_diffrn_reflns_theta_min         2.24
_exptl_absorpt_coefficient_mu    1.890
_exptl_absorpt_correction_T_max  0.783
_exptl_absorpt_correction_T_min  0.598
_exptl_absorpt_correction_type   psi-scan
_exptl_crystal_density_diffrn    1.654
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             1072
_exptl_crystal_size_max          0.26
_exptl_crystal_size_mid          0.22
_exptl_crystal_size_min          0.14
_refine_diff_density_max         0.775
_refine_diff_density_min         -0.499
_refine_diff_density_rms         0.074
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.871
_refine_ls_hydrogen_treatment    riding
_refine_ls_matrix_type           full
_refine_ls_number_parameters     262
_refine_ls_number_reflns         4733
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.871
_refine_ls_R_factor_all          0.0524
_refine_ls_R_factor_gt           0.0333
_refine_ls_shift/su_max          0.004
_refine_ls_shift/su_mean         0.001
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0320P)^2^+2.6374P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0762
_refine_ls_wR_factor_ref         0.0835
_reflns_number_gt                3460
_reflns_number_total             4733
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            b805203dsup1.cif
_cod_data_source_block           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 2.4.2 from
2011-04-26.

'_exptl_absorpt_correction_type' value 'Psi-scan'
changed to 'psi-scan' according to
/home/saulius/struct/CIF-dictionaries/cif_core.dic dictionary named
'cif_core.dic' version 2.4.2 from 2011-04-26.

Automatic conversion script
Id: cif_fix_values 1891 2012-01-12 08:04:46Z andrius 
;
_cod_original_cell_volume        2129.1(13)
_cod_original_sg_symbol_H-M      P2(1)/n
_cod_database_code               7053748