([2.2.2]Cryptand-κ^6^<i>O</i>)potassium (η^4^-cyclooctadiene)bis(η^2^-pyrene)cobaltate(1{-}) pentane hemisolvate
Brennessel, William W.; Ellis, John E.; Acta Crystallographica Section E 68 (2012) m1013–m1014; doi:10.1107/S1600536812029078

data_2235513
_publ_section_title
;
 ([2.2.2]Cryptand-\k^6^<i>O</i>)potassium
 (\h^4^-cyclooctadiene)bis(\h^2^-pyrene)cobaltate(1{-}) pentane
 hemisolvate
;
_journal_coeditor_code           IM2388
_journal_issue                   7
_journal_name_full               'Acta Crystallographica Section E'
_journal_page_first              m1013
_journal_page_last               m1014
_journal_paper_doi               10.1107/S1600536812029078
_journal_volume                  68
_journal_year                    2012
_chemical_formula_iupac
'[K (C18 H36 N2 O6)] [Co (C8 H12) (C16 H10)2], 0.5C5 H12'
_chemical_formula_moiety         'C40 H32 Co, C18 H36 K N2 O6, 0.5(C5 H12)'
_chemical_formula_sum            'C60.5 H72 Co K N2 O6'
_chemical_formula_weight         1023.25
_chemical_name_common            5297
_chemical_name_systematic
;
([2.2.2]Cryptand-\k^6^<i>O</i>)potassium
(\h^4^-cyclooctadiene)bis(\h^2^-pyrene)cobaltate(1-)
pentane hemisolvate
;
_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                72.0640(10)
_cell_angle_beta                 81.5950(10)
_cell_angle_gamma                68.5580(10)
_cell_formula_units_Z            2
_cell_length_a                   12.1007(9)
_cell_length_b                   12.9869(10)
_cell_length_c                   18.7501(14)
_cell_measurement_reflns_used    3044
_cell_measurement_temperature    173(2)
_cell_measurement_theta_max      26.25
_cell_measurement_theta_min      2.47
_cell_volume                     2607.5(3)
_computing_cell_refinement       'SAINT (Bruker, 2003)'
_computing_data_collection       'SMART (Bruker, 2003)'
_computing_data_reduction        'SAINT (Bruker, 2003)'
_computing_molecular_graphics    'SHELXTL (Sheldrick, 2008)'
_computing_publication_material  'SHELXTL (Sheldrick, 2008)'
_computing_structure_refinement  'SHELXL97 (Sheldrick, 2008)'
_computing_structure_solution    'SIR97 (Altomare <i>et al.</i>, 1999)'
_diffrn_ambient_temperature      173(2)
_diffrn_measured_fraction_theta_full 0.986
_diffrn_measured_fraction_theta_max 0.986
_diffrn_measurement_device_type  'Bruker SMART CCD Platform'
_diffrn_measurement_method       'area detector, \w scans per \f'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'normal-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0369
_diffrn_reflns_av_sigmaI/netI    0.0508
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_number            29850
_diffrn_reflns_theta_full        27.10
_diffrn_reflns_theta_max         27.10
_diffrn_reflns_theta_min         1.75
_exptl_absorpt_coefficient_mu    0.463
_exptl_absorpt_correction_T_max  0.9639
_exptl_absorpt_correction_T_min  0.8365
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   '(SADABS; Sheldrick, 2008)'
_exptl_crystal_colour            purple-black
_exptl_crystal_density_diffrn    1.303
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             1090
_exptl_crystal_size_max          0.40
_exptl_crystal_size_mid          0.24
_exptl_crystal_size_min          0.08
_refine_diff_density_max         0.740
_refine_diff_density_min         -0.480
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.005
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     678
_refine_ls_number_reflns         11375
_refine_ls_number_restraints     5
_refine_ls_restrained_S_all      1.005
_refine_ls_R_factor_all          0.0750
_refine_ls_R_factor_gt           0.0422
_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^)+(0.0421P)^2^+1.3440P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0917
_refine_ls_wR_factor_ref         0.1076
_reflns_number_gt                7919
_reflns_number_total             11375
_reflns_threshold_expression     I>2sigma(I)
_cod_data_source_file            im2388.cif
_cod_data_source_block           I
_cod_original_formula_sum        'C60.5 H72 Co1 K1 N2 O6'
_cod_database_code               2235513
_cod_database_fobs_code          2235513