A novel pyramidal multiple alkali metal cluster [K3(H2O)]3+ stabilized within a capsule containing 16-nitrogen donors
Bing-guang, Zhang; Dong, Guo; Chun-ying, Duan; Ping, Cai; Qing-jin, Meng; Chemical Communications (Cambridge, United Kingdom)  (2003) 1836–1837; doi:10.1039/b305001g

data_7103823
_publ_section_title
; 
 A novel pyramidal multiple alkali metal cluster [K3(H2O)]3+ stabilized within
 a capsule containing 16-nitrogen donors
;
_journal_coden_ASTM              CHCOFS
_journal_issue                   15
_journal_name_full
;
 Chemical Communications (Cambridge, United Kingdom)
;
_journal_page_first              1836
_journal_page_last               1837
_journal_paper_doi               10.1039/b305001g
_journal_year                    2003
_chemical_formula_moiety         '(C36H72N16) (H2OK3) (CdI4) (ClO4)2 (H3O)'
_chemical_formula_sum            'C36 H77 Cd Cl2 I4 K3 N16 O10'
_chemical_formula_weight         1702.34
_space_group_IT_number           57
_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_Hall  '-P 2c 2b'
_symmetry_space_group_name_H-M   'P b c m'
_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                 90.00
_cell_angle_gamma                90.00
_cell_formula_units_Z            8
_cell_length_a                   13.512(3)
_cell_length_b                   27.115(5)
_cell_length_c                   31.756(6)
_cell_measurement_reflns_used    1342
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      22.43
_cell_measurement_theta_min      2.65
_cell_volume                     11635(4)
_computing_cell_refinement       'Bruker SMART'
_computing_data_collection       'Bruker SMART'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'Bruker SHELXTL'
_computing_structure_solution    'Bruker SHELXTL'
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 0.991
_diffrn_measured_fraction_theta_max 0.991
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       'phi and omega 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  0.0856
_diffrn_reflns_av_sigmaI/netI    0.1668
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       32
_diffrn_reflns_limit_k_min       -26
_diffrn_reflns_limit_l_max       37
_diffrn_reflns_limit_l_min       -35
_diffrn_reflns_number            51644
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         25.00
_diffrn_reflns_theta_min         3.42
_exptl_absorpt_coefficient_mu    2.868
_exptl_absorpt_correction_T_max  0.7432
_exptl_absorpt_correction_T_min  0.6684
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_process_details   SADABS
_exptl_crystal_colour            pale-yellow
_exptl_crystal_density_diffrn    1.944
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             6688
_exptl_crystal_size_max          0.15
_exptl_crystal_size_mid          0.10
_exptl_crystal_size_min          0.10
_refine_diff_density_max         '2.175 (1.61\%A from K3)'
_refine_diff_density_min         -0.944
_refine_diff_density_rms         0.147
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.022
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     987
_refine_ls_number_reflns         10351
_refine_ls_number_restraints     1131
_refine_ls_restrained_S_all      1.066
_refine_ls_R_factor_all          0.1504
_refine_ls_R_factor_gt           0.0759
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0650P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1863
_refine_ls_wR_factor_ref         0.2020
_reflns_number_gt                4202
_reflns_number_total             10351
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            b305001g.txt
_cod_data_source_block           compound_1
_cod_depositor_comments
;
The following automatic conversions were performed:
'_symmetry_cell_setting' value 'Orthorhombic' changed to 'orthorhombic'
according to '/home/saulius/struct/CIF-dictionaries/cif_core.dic'
dictionary named 'cif_core.dic' version 2.4.1 from 2010-06-29.

Automatic conversion script
Id: cif_fix_enum 1527 2010-12-29 10:47:43Z saulius 
;
_cod_original_sg_symbol_H-M      'Pbcm '
_cod_database_code               7103823