Crystal structure of tris[([2.2.2]crypt)potassium] nonastannide ethylenediamine hemisolvate, [K(C~18~H~36~N~2~O~6~)]~3~Sn~9~ · ½C~2~H~8~N~2~
L. Yong; S. D. Hoffmann; T. F. Fässler; Zeitschrift für Kristallographie - New Crystal Structures 220 (2005) 49–52; doi:

data_8101694
_publ_section_title
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Crystal structure of tris[([2.2.2]crypt)potassium] nonastannide ethylenediamine 
hemisolvate, [K(C~18~H~36~N~2~O~6~)]~3~Sn~9~ &#x00B7; &#x00BD;C~2~H~8~N~2~
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_journal_issue                   1
_journal_name_full
'Zeitschrift f\"ur Kristallographie - New Crystal Structures'
_journal_page_first              49
_journal_page_last               52
_journal_volume                  220
_journal_year                    2005
_chemical_formula_moiety         '[K([2.2.2]crypt)]3[Sn9](C2H8N2)0.5'
_chemical_formula_sum            'C55 H112 K3 N7 O18 Sn9'
_chemical_formula_weight         2345.03
_chemical_melting_point          ?
_chemical_name_systematic
;
tri[potassium([2.2.2]crypt)]nonastannide ethylenediamine hemisolvate
;
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_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
_audit_creation_method           SHELXL-97
_cell_angle_alpha                92.7499(3)
_cell_angle_beta                 96.5942(3)
_cell_angle_gamma                111.6478(2)
_cell_formula_units_Z            2
_cell_length_a                   14.8163(1)
_cell_length_b                   16.1125(1)
_cell_length_c                   20.1823(1)
_cell_measurement_reflns_used    16282
_cell_measurement_temperature    120(2)
_cell_measurement_theta_max      25.35
_cell_measurement_theta_min      1.00
_cell_volume                     4427.28(5)
_computing_cell_refinement       'DENZO (Nonius, 2001b)'
_computing_data_collection       'Kappa-CCD Control Software (Nonius, 2001a)'
_computing_data_reduction        'DENZO (Nonius, 2001b)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      120(2)
_diffrn_detector                 'CCD plate '
_diffrn_detector_area_resol_mean '18 # 9 for binned mode'
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measurement_device       '\k-geometry diffractometer '
_diffrn_measurement_device_type  'Nonius \k-CCD'
_diffrn_measurement_method       'phi and omega rotation '
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'NONIUS FR 591 rotating anode'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.058
_diffrn_reflns_av_sigmaI/netI    0.0341
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_number            16285
_diffrn_reflns_theta_full        25.41
_diffrn_reflns_theta_max         25.41
_diffrn_reflns_theta_min         1.02
_diffrn_standards_decay_%        0
_exptl_absorpt_coefficient_mu    2.691
_exptl_absorpt_correction_T_max  none
_exptl_absorpt_correction_T_min  none
_exptl_absorpt_correction_type   none
_exptl_absorpt_process_details   none
_exptl_crystal_colour            'dark brown'
_exptl_crystal_density_diffrn    1.759
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             2284
_exptl_crystal_size_max          0.50
_exptl_crystal_size_mid          0.40
_exptl_crystal_size_min          0.20
_refine_diff_density_max         3.247
_refine_diff_density_min         -1.496
_refine_diff_density_rms         0.164
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.056
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     829
_refine_ls_number_reflns         16285
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.056
_refine_ls_R_factor_all          0.0528
_refine_ls_R_factor_gt           0.0391
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0531P)^2^+13.1542P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1015
_refine_ls_wR_factor_ref         0.1064
_reflns_number_gt                13197
_reflns_number_total             16285
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            1267-1422.cff
_cod_data_source_block           li_003a
_cod_depositor_comments
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The following automatic conversions were performed:

'_chemical_melting_point' value 'not measured' was changed to '?' -
the value is undefined or not given.

Automatic conversion script
Id: cif_fix_values 1569 2011-02-09 13:29:24Z adriana 

The following automatic conversions were performed:

'_exptl_crystal_density_meas' value 'not measured' was changed to '?'
- the value is perceived as not measured.

Automatic conversion script
Id: cif_fix_values 3008 2015-01-20 13:52:24Z robertas 
;
_cod_original_sg_symbol_H-M      P-1
_cod_database_code               8101694