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_7053747
_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            'C12 H31.5 Cs O13 P0.5 S0.5'
_chemical_formula_weight         548.30
_chemical_name_systematic
;
?
;
_space_group_IT_number           15
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-C 2yc'
_symmetry_space_group_name_H-M   'C 1 2/c 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                 101.14(6)
_cell_angle_gamma                90.00
_cell_formula_units_Z            8
_cell_length_a                   19.840(7)
_cell_length_b                   8.460(4)
_cell_length_c                   26.190(18)
_cell_measurement_temperature    293(2)
_cell_volume                     4313(4)
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 0.843
_diffrn_measured_fraction_theta_max 0.843
_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  0.0411
_diffrn_reflns_av_sigmaI/netI    0.0195
_diffrn_reflns_limit_h_max       23
_diffrn_reflns_limit_h_min       -23
_diffrn_reflns_limit_k_max       10
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       27
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_number            3288
_diffrn_reflns_theta_full        24.99
_diffrn_reflns_theta_max         24.99
_diffrn_reflns_theta_min         3.17
_exptl_absorpt_coefficient_mu    1.861
_exptl_absorpt_correction_T_max  0.803
_exptl_absorpt_correction_T_min  0.648
_exptl_absorpt_correction_type   psi-scan
_exptl_crystal_density_diffrn    1.689
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             2224
_exptl_crystal_size_max          0.30
_exptl_crystal_size_mid          0.24
_exptl_crystal_size_min          0.20
_refine_diff_density_max         2.274
_refine_diff_density_min         -2.850
_refine_diff_density_rms         0.213
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.040
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     244
_refine_ls_number_reflns         3196
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.040
_refine_ls_R_factor_all          0.0765
_refine_ls_R_factor_gt           0.0661
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.1636P)^2^+31.6815P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2049
_refine_ls_wR_factor_ref         0.2168
_reflns_number_gt                2702
_reflns_number_total             3196
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            b805203dsup1.cif
_cod_data_source_block           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 2.4.2 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_sg_symbol_H-M      C2/c
_cod_original_formula_sum        'C12 H31.50 Cs O13 P0.50 S0.50'
_cod_database_code               7053747