‘Inverse crown ether’ complexes extended to group 12 through the syntheses of [Na2Zn2(HMDS)4(O)] and [{K2Zn2(HMDS)4(O2)x(O)y}∞ ]
Forbes, Glenn C.; Kennedy, Alan R.; Mulvey, Robert E.; Rowlings, René B.; Clegg, William; Liddle, Stephen T.; Wilson, Chick C.; Chemical Communications  (2000) 1759–; doi:10.1039/b005233g

data_7111047
_publ_section_title
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 &#x2018;Inverse crown ether&#x2019; complexes extended to group 12
 through the syntheses of [Na2Zn2(HMDS)4(O)] and
 [{K2Zn2(HMDS)4(O2)x(O)y}\\infty ]
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_journal_issue                   18
_journal_name_full               'Chemical Communications'
_journal_page_first              1759
_journal_paper_doi               10.1039/b005233g
_journal_year                    2000
_chemical_formula_sum            'C24 H72 N4 Na2 O Si8 Zn2'
_chemical_formula_weight         834.30
_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                108.96(3)
_cell_angle_beta                 99.77(4)
_cell_angle_gamma                96.13(4)
_cell_formula_units_Z            1
_cell_length_a                   10.711(6)
_cell_length_b                   12.810(6)
_cell_length_c                   8.970(4)
_cell_measurement_reflns_used    25
_cell_measurement_temperature    183(2)
_cell_measurement_theta_max      20.01
_cell_measurement_theta_min      19.51
_cell_volume                     1129.7(10)
_computing_cell_refinement       ' " '
_computing_data_collection       'MSC/Rigaku Diffractometer Control'
_computing_data_reduction        Texsan
_computing_molecular_graphics    ORTEP-II
_computing_publication_material  SHELXL-97
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    SIR
_diffrn_ambient_temperature      183(2)
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device_type  'Rigaku AFC7S'
_diffrn_measurement_method       \w/2\q
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71069
_diffrn_reflns_av_R_equivalents  0.0134
_diffrn_reflns_av_sigmaI/netI    0.0438
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       0
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       12
_diffrn_reflns_limit_l_min       -12
_diffrn_reflns_number            6914
_diffrn_reflns_theta_full        30.04
_diffrn_reflns_theta_max         30.04
_diffrn_reflns_theta_min         2.79
_diffrn_standards_decay_%        1.470
_diffrn_standards_interval_count 150
_diffrn_standards_number         3
_exptl_absorpt_coefficient_mu    1.316
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.735
_exptl_absorpt_correction_type   'psi scans'
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.226
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             446
_exptl_crystal_size_max          0.50
_exptl_crystal_size_mid          0.40
_exptl_crystal_size_min          0.20
_refine_diff_density_max         1.113
_refine_diff_density_min         -1.423
_refine_diff_density_rms         0.098
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.072
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     199
_refine_ls_number_reflns         6590
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.072
_refine_ls_R_factor_all          0.0546
_refine_ls_R_factor_gt           0.0399
_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^)+(0.0723P)^2^+0.7678P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1231
_refine_ls_wR_factor_ref         0.1305
_reflns_number_gt                5530
_reflns_number_total             6590
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            b005233gsup1.cif
_cod_data_source_block           znna
_cod_depositor_comments
;
The following automatic conversions were performed:

'_refine_ls_weighting_scheme' value 'calc
w=1/[\s^2^(Fo^2^)+(0.0723P)^2^+0.7678P] 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^)+(0.0723P)^2^+0.7678P] where P=(Fo^2^+2Fc^2^)/3'.

Automatic conversion script
Id: cif_fix_values 3143 2015-03-26 13:38:13Z robertas 
;
_cod_original_cell_volume        1129.6(9)
_cod_original_sg_symbol_H-M      P-1
_cod_database_code               7111047