Sila-polyethers as innocent crystallization reagents for heavy alkali metal compounds
Dankert, Fabian; Heine, Johanna; Rienmüller, Julia; von Hänisch, Carsten; CrystEngComm 20 (2018) 5370–; doi:10.1039/C8CE01097H

data_7231401
_publ_section_title
;
 Sila-polyethers as innocent crystallization reagents for heavy alkali
 metal compounds
;
_journal_issue                   36
_journal_name_full               CrystEngComm
_journal_page_first              5370
_journal_paper_doi               10.1039/C8CE01097H
_journal_volume                  20
_journal_year                    2018
_chemical_formula_moiety         'C13 H22 F9 O15 Rb3 S3'
_chemical_formula_sum            'C13 H22 F9 O15 Rb3 S3'
_chemical_formula_weight         941.89
_chemical_properties_physical    Moisture-sensitive
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     dual
_audit_creation_date             2018-02-20
_audit_creation_method
;
Olex2 1.2
(compiled 2017.08.10 svn.r3458 for OlexSys, GUI svn.r5381)
;
_audit_update_record
;
2018-06-28 deposited with the CCDC.
2018-08-13 downloaded from the CCDC.
;
_cell_angle_alpha                112.79(2)
_cell_angle_beta                 100.47(3)
_cell_angle_gamma                102.10(2)
_cell_formula_units_Z            2
_cell_length_a                   11.520(4)
_cell_length_b                   12.109(4)
_cell_length_c                   12.548(3)
_cell_measurement_reflns_used    26699
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      63.8
_cell_measurement_theta_min      3.8
_cell_volume                     1509.3(9)
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'XL (Sheldrick, 2008)'
_computing_structure_solution    'ShelXT (Sheldrick, 2015)'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device_type  'STOE IPDS 2T'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0635
_diffrn_reflns_av_unetI/netI     0.0487
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            23023
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         29.998
_diffrn_reflns_theta_min         1.918
_exptl_absorpt_coefficient_mu    5.169
_exptl_absorpt_correction_T_max  0.6809
_exptl_absorpt_correction_T_min  0.2706
_exptl_absorpt_correction_type   numerical
_exptl_absorpt_process_details   'STOE X AREA, XRED32'
_exptl_crystal_colour            colourless
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    2.072
_exptl_crystal_description       platelet
_exptl_crystal_F_000             920
_exptl_crystal_recrystallization_method 'Re-crystallisation from solvent: DCM'
_exptl_crystal_size_max          0.343
_exptl_crystal_size_mid          0.135
_exptl_crystal_size_min          0.096
_refine_diff_density_max         1.260
_refine_diff_density_min         -0.764
_refine_diff_density_rms         0.110
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.001
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     396
_refine_ls_number_reflns         8793
_refine_ls_number_restraints     2
_refine_ls_restrained_S_all      1.001
_refine_ls_R_factor_all          0.0481
_refine_ls_R_factor_gt           0.0328
_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^)+(0.0461P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0778
_refine_ls_wR_factor_ref         0.0818
_reflns_Friedel_coverage         0.000
_reflns_number_gt                7068
_reflns_number_total             8793
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c8ce01097h2.cif
_cod_data_source_block           compound5
_cod_depositor_comments          'Adding full bibliography for 7231401.cif.'
_cod_original_cell_volume        1509.3(8)
_cod_database_code               7231401
_shelx_shelxl_version_number     2014/7
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H,H) groups
2. Restrained distances
 O1-H1
 0.83 with sigma of 0.02
 H6-O6
 0.83 with sigma of 0.02
3.a Secondary CH2 refined with riding coordinates:
 C4(H4A,H4B), C3(H3A,H3B), C7(H7A,H7B), C8(H8A,H8B), C6(H6A,H6B), C9(H9A,H9B),
 C1(H1A,H1B), C2(H2A,H2B), C10(H10A,H10B), C5(H5A,H5B)
;
_shelx_res_checksum              91126
_olex2_submission_special_instructions 'No special instructions were received'