The first X-ray structurally characterized M3L2 cage-like complex with tetrahedral metal centres and its encapsulation of a neutral guest molecule
Liu, Hong-Ke; Sun, Wei-Yin; Ma, De-Jian; Tang, Wen-Xia; Yu, Kai-Bei; Chemical Communications  (2000) 591–; doi:10.1039/b000259n

data_7110841
_publ_section_title
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 The first X-ray structurally characterized M3L2 cage-like complex with
 tetrahedral metal centres and its encapsulation of a neutral guest
 molecule
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_journal_issue                   7
_journal_name_full               'Chemical Communications'
_journal_page_first              591
_journal_paper_doi               10.1039/b000259n
_journal_year                    2000
_chemical_formula_sum            'C48 H54 N12 O12 Zn3'
_chemical_formula_weight         1187.14
_chemical_name_systematic
; 
 ? 
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_space_group_IT_number           155
_symmetry_cell_setting           rhombohedral
_symmetry_space_group_name_Hall  'R 3 2"'
_symmetry_space_group_name_H-M   'R 3 2 :H'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                120.00
_cell_formula_units_Z            3
_cell_length_a                   17.661(2)
_cell_length_b                   17.661(2)
_cell_length_c                   20.722(4)
_cell_measurement_reflns_used    32
_cell_measurement_temperature    294(2)
_cell_measurement_theta_max      15.57
_cell_measurement_theta_min      3.31
_cell_volume                     5597.5(14)
_computing_cell_refinement       'Siemens XSCANS'
_computing_data_collection       'Siemens XSCANS'
_computing_data_reduction        'Siemens SHELXTL'
_computing_molecular_graphics    'Siemens SHELXTL'
_computing_publication_material  'Siemens SHELXTL'
_computing_structure_refinement  'SHELXL-93 (Sheldrick, 1993)'
_computing_structure_solution    'SHELXS-86 (Sheldrick, 1990)'
_diffrn_ambient_temperature      294(2)
_diffrn_measurement_device       'Siemens P4'
_diffrn_measurement_method       '\w scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'normal-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0231
_diffrn_reflns_av_sigmaI/netI    0.0627
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_h_min       0
_diffrn_reflns_limit_k_max       1
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_l_max       25
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_number            2385
_diffrn_reflns_theta_max         25.96
_diffrn_reflns_theta_min         1.65
_diffrn_standards_decay_%        1.89
_diffrn_standards_interval_count 97
_diffrn_standards_number         3
_exptl_absorpt_coefficient_mu    1.007
_exptl_absorpt_correction_T_max  0.9416
_exptl_absorpt_correction_T_min  0.8041
_exptl_absorpt_correction_type   empirical
_exptl_crystal_density_diffrn    1.057
_exptl_crystal_F_000             1836
_exptl_crystal_size_max          0.56
_exptl_crystal_size_mid          0.54
_exptl_crystal_size_min          0.24
_refine_diff_density_max         0.434
_refine_diff_density_min         -0.282
_refine_diff_density_rms         0.073
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   0.00
_refine_ls_extinction_coef       0.0069(8)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     SHELXL
_refine_ls_goodness_of_fit_all   0.811
_refine_ls_goodness_of_fit_obs   1.083
_refine_ls_hydrogen_treatment    none
_refine_ls_matrix_type           full
_refine_ls_number_parameters     115
_refine_ls_number_reflns         2041
_refine_ls_number_restraints     4
_refine_ls_restrained_S_all      1.582
_refine_ls_restrained_S_obs      1.084
_refine_ls_R_factor_all          0.1476
_refine_ls_R_factor_obs          0.0684
_refine_ls_shift/esd_max         -0.001
_refine_ls_shift/esd_mean        0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.1209P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.3411
_refine_ls_wR_factor_obs         0.1641
_reflns_number_observed          938
_reflns_number_total             2081
_reflns_observed_criterion       >2sigma(I)
_cod_data_source_file            b000259nsup1.cif
_cod_data_source_block           1
_cod_depositor_comments
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The following automatic conversions were performed:

'_symmetry_cell_setting' value 'Rhombohedral' changed to
'rhombohedral' according to
/home/saulius/struct/CIF-dictionaries/cif_core.dic dictionary named
'cif_core.dic' version 2.4.2 from 2011-04-26.

Automatic conversion script
Id: cif_fix_values 1891 2012-01-12 08:04:46Z andrius 

The following automatic conversions were performed:

'_refine_ls_weighting_scheme' value 'calc
w=1/[\s^2^(Fo^2^)+(0.1209P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' was
changed to 'calc'. New tag '_refine_ls_weighting_details' was
created. The value of the new tag was set to
'w=1/[\s^2^(Fo^2^)+(0.1209P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'.

Automatic conversion script
Id: cif_fix_values 3143 2015-03-26 13:38:13Z robertas 
;
_cod_original_sg_symbol_H-M      R32
_cod_database_code               7110841