‘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_7111048
_publ_section_title
;
 &#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 ]
;
_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 K2 N4 O1.82 Si8 Zn2'
_chemical_formula_weight         879.64
_chemical_name_systematic
;
 ?
;
_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                97.322(2)
_cell_angle_beta                 108.154(2)
_cell_angle_gamma                101.162(2)
_cell_formula_units_Z            1
_cell_length_a                   8.9898(4)
_cell_length_b                   10.9763(5)
_cell_length_c                   12.9529(6)
_cell_measurement_reflns_used    9259
_cell_measurement_temperature    160(2)
_cell_measurement_theta_max      28.44
_cell_measurement_theta_min      2.46
_cell_volume                     1167.11(9)
_computing_cell_refinement       'Siemens SAINT'
_computing_data_collection       'Siemens SMART'
_computing_data_reduction        'Siemens SAINT'
_computing_molecular_graphics    'Siemens SHELXTL'
_computing_publication_material  'SHELXTL and local programs'
_computing_structure_refinement  'Siemens SHELXTL'
_computing_structure_solution    'Siemens SHELXTL'
_diffrn_ambient_temperature      160(2)
_diffrn_measured_fraction_theta_full 0.983
_diffrn_measured_fraction_theta_max 0.898
_diffrn_measurement_device_type  'Siemens SMART CCD diffractometer'
_diffrn_measurement_method       '\w rotation with narrow frames'
_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  0.0112
_diffrn_reflns_av_sigmaI/netI    0.0205
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            10058
_diffrn_reflns_theta_full        26.00
_diffrn_reflns_theta_max         28.44
_diffrn_reflns_theta_min         1.69
_diffrn_standards_decay_%        0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    1.436
_exptl_absorpt_correction_T_max  0.591
_exptl_absorpt_correction_T_min  0.489
_exptl_absorpt_correction_type   empirical
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.252
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             469
_exptl_crystal_size_max          0.70
_exptl_crystal_size_mid          0.46
_exptl_crystal_size_min          0.36
_refine_diff_density_max         0.327
_refine_diff_density_min         -0.275
_refine_diff_density_rms         0.043
_refine_ls_extinction_coef       0.0047(6)
_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_ref   0.963
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     210
_refine_ls_number_reflns         5263
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.963
_refine_ls_R_factor_all          0.0205
_refine_ls_R_factor_gt           0.0188
_refine_ls_shift/su_max          0.024
_refine_ls_shift/su_mean         0.001
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0369P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0545
_refine_ls_wR_factor_ref         0.0549
_reflns_number_gt                4753
_reflns_number_total             5263
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            b005233gsup1.cif
_cod_data_source_block           rem294
_cod_original_sg_symbol_H-M      P-1
_cod_database_code               7111048