High-Connectivity Networks and Hybrid Inorganic Rod Materials Built from Potassium and Rubidium p-Halide-Substituted Aryloxides
J. Jacob Morris; Bruce C. Noll; Kenneth W. Henderson; Inorganic Chemistry 47 (2008) 9583–9591; doi:10.1021/ic801140u

data_4306299
_publ_contact_author_address
;University of Notre Dame
Department of Chemistry
Notre Dame, IN 46556-5670
;
_publ_contact_author_email       khenders@nd.edu
_publ_contact_author_fax         574.631.6652
_publ_contact_author_name        'Kenneth W. Henderson'
_publ_contact_author_phone       574.631.8025
_publ_section_title
;
High-Connectivity Networks and Hybrid Inorganic Rod Materials Built from
Potassium and Rubidium p-Halide-Substituted Aryloxides
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              9583
_journal_page_last               9591
_journal_paper_doi               10.1021/ic801140u
_journal_volume                  47
_journal_year                    2008
_chemical_compound_source        synthesized
_chemical_formula_moiety         'C22 H20 Br3 K3 O5'
_chemical_formula_sum            'C22 H20 Br3 K3 O5'
_chemical_formula_weight         721.41
_chemical_name_common
;
Potassium 4-Br-phenoxide dioxane
;
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           62
_symmetry_cell_setting           orthorhombic
_symmetry_Int_Tables_number      62
_symmetry_space_group_name_Hall  '-P 2ac 2n'
_symmetry_space_group_name_H-M   'P n m a'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   7.1981(4)
_cell_length_b                   17.5149(8)
_cell_length_c                   21.2140(10)
_cell_measurement_reflns_used    9523
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      29.306
_cell_measurement_theta_min      2.988
_cell_volume                     2674.5(2)
_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    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      100(2)
_diffrn_detector_area_resol_mean 8.33
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 1.000
_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  0.0436
_diffrn_reflns_av_sigmaI/netI    0.0188
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_k_max       22
_diffrn_reflns_limit_k_min       -21
_diffrn_reflns_limit_l_max       27
_diffrn_reflns_limit_l_min       -27
_diffrn_reflns_number            54582
_diffrn_reflns_theta_full        27.10
_diffrn_reflns_theta_max         27.10
_diffrn_reflns_theta_min         1.92
_diffrn_source                   'fine-focus sealed tube'
_diffrn_source_type              'Siemens KFFMO2K-90'
_exptl_absorpt_coefficient_mu    5.022
_exptl_absorpt_correction_T_max  0.521
_exptl_absorpt_correction_T_min  0.266
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
'Blessing, R. H. (1995) Acta Cryst. A51, 33-38.'
_exptl_crystal_colour            'clear colourless'
_exptl_crystal_density_diffrn    1.792
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       parallelepiped
_exptl_crystal_F_000             1416
_exptl_crystal_size_max          0.33
_exptl_crystal_size_mid          0.19
_exptl_crystal_size_min          0.13
_refine_diff_density_max         0.695
_refine_diff_density_min         -0.430
_refine_diff_density_rms         0.064
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.082
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     173
_refine_ls_number_reflns         3050
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.082
_refine_ls_R_factor_all          0.0347
_refine_ls_R_factor_gt           0.0245
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0173P)^2^+2.8746P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0517
_refine_ls_wR_factor_ref         0.0558
_reflns_number_gt                2614
_reflns_number_total             3050
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic801140u_si_001_5.cif
_cod_data_source_block           jjm101
_cod_database_code               4306299