Crystal structure of tris[(4,7,13,16,21,24-hexaoxa-1,10-diazabicyclo[8.8.8]hexacosane-κ^8^<i>N</i>~2~,<i>O</i>~6~)rubidium] rubidium nonastannide
Klein, Wilhelm; He, Haiyan; Fässler, Thomas F.; Acta Crystallographica Section E 73 (2017) 147–151; doi:10.1107/S2056989017000172

data_2242010
_publ_section_title
;
 Crystal structure of
 tris[(4,7,13,16,21,24-hexaoxa-1,10-diazabicyclo[8.8.8]hexacosane-\k^8^<i>N</i>~2~,<i>O</i>~6~)rubidium]
 rubidium nonastannide
;
_journal_coeditor_code           WM5352
_journal_issue                   2
_journal_name_full               'Acta Crystallographica Section E'
_journal_page_first              147
_journal_page_last               151
_journal_paper_doi               10.1107/S2056989017000172
_journal_volume                  73
_journal_year                    2017
_chemical_formula_iupac          '[Rb (C18 H36 N2 O6)]3 Rb Sn9'
_chemical_formula_moiety         '3(C18 H36 N2 O6 Rb), Sn9, Rb'
_chemical_formula_sum            'C54 H108 N6 O18 Rb4 Sn9'
_chemical_formula_weight         2539.55
_chemical_name_systematic
'Tris[(4,7,13,16,21,24-hexaoxa-1,10-diazabicyclo[8.8.8]hexacosane-\k^8^N~2~,O~6~)rubidium] rubidium nonastannide'
_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   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_cell_angle_alpha                98.782(4)
_cell_angle_beta                 104.350(4)
_cell_angle_gamma                118.407(6)
_cell_formula_units_Z            2
_cell_length_a                   15.7287(8)
_cell_length_b                   16.1530(10)
_cell_length_c                   20.2896(8)
_cell_measurement_reflns_used    2671
_cell_measurement_temperature    123(2)
_cell_measurement_theta_max      32.8871
_cell_measurement_theta_min      2.8659
_cell_volume                     4165.4(5)
_computing_cell_refinement
;
CrysAlis RED (Oxford Diffraction, 2009)
;
_computing_data_collection
;
CrysAlis CCD (Oxford Diffraction, 2009)
;
_computing_data_reduction
;
CrysAlis RED (Oxford Diffraction, 2009)
;
_computing_molecular_graphics
;
DIAMOND (Brandenburg, 2012)
;
_computing_publication_material
;
publCIF (Westrip, 2010)
;
_computing_structure_refinement
;
<i>SHELXL2014/7</i> (Sheldrick, 2015)
;
_computing_structure_solution
;
SHELXS97 (Sheldrick, 2008)
;
_diffrn_ambient_temperature      123(2)
_diffrn_detector_area_resol_mean 16.0238
_diffrn_measured_fraction_theta_full 0.974
_diffrn_measured_fraction_theta_max 0.972
_diffrn_measurement_device_type  'Oxford Diffraction Xcalibur 3'
_diffrn_measurement_method       '\w and \p scans'
_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  0.1121
_diffrn_reflns_limit_h_max       19
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       25
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            29013
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         25.998
_diffrn_reflns_theta_min         2.870
_exptl_absorpt_coefficient_mu    5.031
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.83244
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
(CrysAlisRED; Oxford Diffraction, 2009)
;
_exptl_crystal_colour            brown
_exptl_crystal_density_diffrn    2.025
_exptl_crystal_description       plate
_exptl_crystal_F_000             2432
_exptl_crystal_size_max          0.15
_exptl_crystal_size_mid          0.12
_exptl_crystal_size_min          0.05
_refine_diff_density_max         2.854
_refine_diff_density_min         -2.194
_refine_ls_extinction_coef       0
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.622
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     823
_refine_ls_number_reflns         15902
_refine_ls_number_restraints     60
_refine_ls_restrained_S_all      0.625
_refine_ls_R_factor_all          0.1830
_refine_ls_R_factor_gt           0.0541
_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^)] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0758
_refine_ls_wR_factor_ref         0.0935
_reflns_number_gt                4724
_reflns_number_total             15902
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            wm5352sup1.cif
_cod_data_source_block           I
_cod_original_cell_volume        4165.4(4)
_cod_database_code               2242010
_cod_database_fobs_code          2242010
_shelx_hkl_checksum              71191
_shelx_res_checksum              47780