Rational Assembly of Primitive Cubic Networks Using Hexameric Stacks of Sodium Aryloxides as Nodes
Dugald J. MacDougall; Bruce C. Noll; Kenneth W. Henderson; Inorganic Chemistry 44 (2005) 1181–1183; doi:10.1021/ic048257b

data_4308632
_publ_section_title
;
Rational Assembly of Primitive Cubic Networks Using Hexameric Stacks of
Sodium Aryloxides as Nodes
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              1181
_journal_page_last               1183
_journal_paper_doi               10.1021/ic048257b
_journal_volume                  44
_journal_year                    2005
_chemical_formula_moiety         'C68 H88 F6 Na6 O14'
_chemical_formula_sum            'C68 H88 F6 Na6 O14'
_chemical_formula_weight         1381.32
_chemical_name_common            'sodium 4-fluorophenoxide THF solvate'
_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'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                65.713(1)
_cell_angle_beta                 67.411(1)
_cell_angle_gamma                64.905(1)
_cell_formula_units_Z            1
_cell_length_a                   11.9721(3)
_cell_length_b                   13.3007(3)
_cell_length_c                   13.9938(3)
_cell_measurement_reflns_used    7239
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      31.18
_cell_measurement_theta_min      2.21
_cell_volume                     1779.06(7)
_computing_cell_refinement       'APEX2/SAINT (Bruker, 2004)'
_computing_data_collection       'APEX2 (Bruker, 2004)'
_computing_data_reduction        'SAINT/XPREP (Bruker, 2004; Sheldrick, 2003)'
_computing_molecular_graphics    'XP (Sheldrick, 1998)'
_computing_publication_material  'XCIF (Sheldrick, 2001)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'XS (Sheldrick, 2001)'
_diffrn_ambient_temperature      100(2)
_diffrn_detector_area_resol_mean 8.33
_diffrn_measured_fraction_theta_full 0.993
_diffrn_measured_fraction_theta_max 0.993
_diffrn_measurement_device_type  'Bruker SMART APEX CCD area detector'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0419
_diffrn_reflns_av_sigmaI/netI    0.0252
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            83097
_diffrn_reflns_theta_full        31.52
_diffrn_reflns_theta_max         31.52
_diffrn_reflns_theta_min         1.65
_diffrn_source                   'fine-focus sealed tube'
_diffrn_source_type              'Siemens KFFMO2K-90'
_exptl_absorpt_coefficient_mu    0.129
_exptl_absorpt_correction_T_max  0.9796
_exptl_absorpt_correction_T_min  0.9383
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
'Blessing, R. H. (1995) Acta Cryst. A51, 33-38.'
_exptl_crystal_colour            clear
_exptl_crystal_density_diffrn    1.289
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       needle
_exptl_crystal_F_000             728
_exptl_crystal_recrystallization_method 'THF solution chilled to -40 centigrade'
_exptl_crystal_size_max          0.50
_exptl_crystal_size_mid          0.18
_exptl_crystal_size_min          0.16
_refine_diff_density_max         1.084
_refine_diff_density_min         -0.336
_refine_diff_density_rms         0.051
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.028
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     424
_refine_ls_number_reflns         11788
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.028
_refine_ls_R_factor_all          0.0557
_refine_ls_R_factor_gt           0.0409
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0528P)^2^+0.6490P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1051
_refine_ls_wR_factor_ref         0.1153
_reflns_number_gt                9381
_reflns_number_total             11788
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic048257bsi20041210_114350.cif
_cod_data_source_block           dmd38_0m
_cod_original_cell_volume        1779.07(7)
_cod_database_code               4308632