‘Inverse crown ether’ complexes: extension to potassium through the synthesis of [{[(Me3Si)2N]4K2Mg2(O2)}∞ ], a peroxo-centred macrocycle linked into infinite chains by intermolecular K⋯CH3(SiMe2) interactions
Kennedy, Alan R.; Mulvey, Robert E.; Roberts, Brett A.; Rowlings, René B.; Raston, Colin L.; Chemical Communications  (1999) 353–; doi:10.1039/a809681c

data_7110439
_publ_contact_author
;
Alan Kennedy
Dept of P  & A Chemistry
University of Strathclyde
295 Cathedral St
Glasgow
G1 1XL
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_publ_section_title
;
 &#x2018;Inverse crown ether&#x2019; complexes: extension to potassium
 through the synthesis of [{[(Me3Si)2N]4K2Mg2(O2)}\\infty ], a
 peroxo-centred macrocycle linked into infinite chains by intermolecular
 K&#x22EF;CH3(SiMe2) interactions
;
_journal_issue                   4
_journal_name_full               'Chemical Communications'
_journal_page_first              353
_journal_paper_doi               10.1039/a809681c
_journal_year                    1999
_chemical_formula_sum            'C24 H72 K2 Mg2 N4 O2 Si8'
_chemical_formula_weight         800.34
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_symmetry_Int_Tables_number      2
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_audit_creation_date             'Wed Dec  9 13:13:40 1998'
_audit_creation_method           'from TEXRAY.INF file'
_cell_angle_alpha                107.63(3)
_cell_angle_beta                 100.47(3)
_cell_angle_gamma                96.34(4)
_cell_formula_units_Z            1
_cell_length_a                   11.102(4)
_cell_length_b                   12.907(6)
_cell_length_c                   8.906(3)
_cell_measurement_reflns_used    24
_cell_measurement_temperature    123
_cell_measurement_theta_max      22.35
_cell_measurement_theta_min      16.70
_cell_volume                     1177.2(9)
_computing_cell_refinement       'MSC/AFC Diffractometer Control'
_computing_data_collection       'MSC/AFC Diffractometer Control'
_computing_data_reduction        teXsan
_computing_publication_material  teXsan
_computing_structure_refinement  teXsan
_computing_structure_solution    SIR
_diffrn_ambient_temperature      123
_diffrn_measurement_device       'Rigaku AFC7S'
_diffrn_measurement_method       'omega/2-theta scans'
_diffrn_orient_matrix_UB_11      0.04150
_diffrn_orient_matrix_UB_12      -0.01934
_diffrn_orient_matrix_UB_13      -0.09303
_diffrn_orient_matrix_UB_21      -0.08201
_diffrn_orient_matrix_UB_22      -0.01224
_diffrn_orient_matrix_UB_23      -0.07701
_diffrn_orient_matrix_UB_31      0.01455
_diffrn_orient_matrix_UB_32      0.07936
_diffrn_orient_matrix_UB_33      0.00704
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'X-ray tube'
_diffrn_radiation_type           MoKalpha
_diffrn_radiation_wavelength     0.71069
_diffrn_reflns_av_R_equivalents  0.0108
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       0
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -16
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_diffrn_reflns_limit_l_min       -11
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_diffrn_reflns_theta_max         27.50
_diffrn_reflns_theta_min         2.50
_diffrn_standards_decay_%        -0.25
_diffrn_standards_interval_count 150
_diffrn_standards_number         3
_exptl_absorpt_coefficient_mu    0.457
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.925
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_process_details   psi-scan
_exptl_crystal_colour            colorless
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_exptl_crystal_description       rhomb
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_exptl_crystal_size_max          0.700
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_refine_ls_extinction_method     none
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_refine_ls_hydrogen_treatment    refall
_refine_ls_matrix_type           full
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_refine_ls_number_parameters     334
_refine_ls_number_reflns         5156
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0243
_refine_ls_R_factor_obs          0.0229
_refine_ls_shift/esd_max         0.0010
_refine_ls_structure_factor_coef F
_refine_ls_weighting_details     'w = 1/\s^2^(F)'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.0410
_refine_ls_wR_factor_obs         0.0404
_reflns_number_observed          5156
_reflns_number_total             5394
_reflns_observed_criterion       2.00
_cod_data_source_file            809681csup1.cif
_cod_data_source_block           1
_cod_depositor_comments
;
The following automatic conversions were performed:

'_refine_ls_weighting_scheme' value '1/\s^2^(F)' 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^(F)'.

Automatic conversion script
Id: cif_fix_values 3143 2015-03-26 13:38:13Z robertas 
;
_cod_original_cell_volume        1177.3(10)
_cod_original_sg_symbol_H-M      'P -1       '
_cod_original_formula_sum        'C24 H72 K2 N4 Mg2 O2 Si8 '
_cod_database_code               7110439