Tris[(1,4,7,10,13,16-hexaoxacyclooctadecane)rubidium] heptaantimonide–ammonia (1/4)
Mutzbauer, Fabian; Korber, Nikolaus; Acta Crystallographica Section E 67 (2011) m1551–; doi:10.1107/S1600536811041237

data_2232334
_publ_section_title
;
 Tris[(1,4,7,10,13,16-hexaoxacyclooctadecane)rubidium]
 heptaantimonide--ammonia (1/4)
;
_journal_coeditor_code           HP2013
_journal_issue                   11
_journal_name_full               'Acta Crystallographica Section E'
_journal_page_first              m1551
_journal_paper_doi               10.1107/S1600536811041237
_journal_volume                  67
_journal_year                    2011
_chemical_formula_iupac          '[Rb (C12 H24 O6)]3 [Sb7], 4N H3'
_chemical_formula_moiety         '3(C12 H24 O6 Rb +), Sb7 3-, 4(H3 N)'
_chemical_formula_sum            'C36 H84 N4 O18 Rb3 Sb7'
_chemical_formula_weight         1969.73
_chemical_name_common
;
Trirubidium--tris-18-crown-6-heptaantimonide--ammonia (1/4)
;
_chemical_name_systematic
;
Tris[(1,4,7,10,13,16-hexaoxacyclooctadecane)rubidium] heptaantimonide--
ammonia (1/4)
;
_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                 90.98(3)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   15.000(3)
_cell_length_b                   17.484(4)
_cell_length_c                   25.158(5)
_cell_measurement_reflns_used    12127
_cell_measurement_temperature    123(2)
_cell_measurement_theta_max      25.47
_cell_measurement_theta_min      1.95
_cell_volume                     6597(2)
_computing_cell_refinement       'X-AREA (Stoe & Cie, 2005)'
_computing_data_collection       'X-AREA (Stoe & Cie, 2005)'
_computing_data_reduction        'X-AREA (Stoe & Cie, 2005)'
_computing_molecular_graphics    'DIAMOND (Brandenburg, 2001)'
_computing_publication_material  'publCIF (Westrip, 2010)'
_computing_structure_refinement  'SHELXL97 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      123(2)
_diffrn_measured_fraction_theta_full 0.958
_diffrn_measured_fraction_theta_max 0.958
_diffrn_measurement_device_type  'Stoe IPDS1'
_diffrn_measurement_method       rotation
_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  0.0898
_diffrn_reflns_av_sigmaI/netI    0.0513
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_h_min       -18
_diffrn_reflns_limit_k_max       21
_diffrn_reflns_limit_k_min       -21
_diffrn_reflns_limit_l_max       30
_diffrn_reflns_limit_l_min       -30
_diffrn_reflns_number            88182
_diffrn_reflns_theta_full        25.77
_diffrn_reflns_theta_max         25.77
_diffrn_reflns_theta_min         1.95
_diffrn_standards_decay_%        0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    5.079
_exptl_absorpt_correction_T_max  0.6483
_exptl_absorpt_correction_T_min  0.4529
_exptl_absorpt_correction_type   numerical
_exptl_absorpt_process_details   '(X-SHAPE in X-AREA; Stoe & Cie, 2005)'
_exptl_crystal_colour            'clear brown'
_exptl_crystal_density_diffrn    1.983
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             3760
_exptl_crystal_size_max          0.3
_exptl_crystal_size_mid          0.2
_exptl_crystal_size_min          0.1
_refine_diff_density_max         1.660
_refine_diff_density_min         -0.735
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.962
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     617
_refine_ls_number_reflns         12127
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.962
_refine_ls_R_factor_all          0.0540
_refine_ls_R_factor_gt           0.0361
_refine_ls_shift/su_max          0.005
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0446P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0779
_refine_ls_wR_factor_ref         0.0825
_reflns_number_gt                9417
_reflns_number_total             12127
_reflns_threshold_expression     I>2sigma(I)
_cod_data_source_file            hp2013.cif
_cod_data_source_block           I
_cod_original_sg_symbol_H-M      'P 21/n'
_cod_database_code               2232334
_cod_database_fobs_code          2232334