Organometallic rubidium and cesium compounds of the 5,6;11,12-di-o-phenylene-tetracene dianion
Wombacher, T.; Goddard, R.; Lehmann, C. W.; Schneider, J. J.; Chem. Commun.  (2017) –; doi:10.1039/C7CC02320K

data_7120279
_publ_section_title
;
 Organometallic rubidium and cesium compounds of the
 5,6;11,12-di-o-phenylene-tetracene dianion
;
_journal_name_full               'Chem. Commun.'
_journal_paper_doi               10.1039/C7CC02320K
_journal_year                    2017
_chemical_formula_moiety         'C54 H64 O12 Rb2, 2(C4 H8 O)'
_chemical_formula_sum            'C62 H80 O14 Rb2'
_chemical_formula_weight         1220.20
_chemical_name_systematic
'Bis(cyclo-1,4,7,10,13,16-hexaoxy-octakiadecane-rubidium)- diindeno[1,2,3-fg:1',2',3'-op]tetracene tetrahydrofuran solute'
_chemical_properties_physical
', Air-sensitive,Moisture-sensitive,Heat-sensitive,Oxygen-sensitive'
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_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_block_code                10119_Wombacher_DOPT_Rb_18C8_THF_100K
_audit_creation_date             2016-06-15
_audit_creation_method           SHELXL-2014/7
_audit_update_record
;
2017-02-23 deposited with the CCDC.
2017-05-19 downloaded from the CCDC.
;
_cell_angle_alpha                98.144(3)
_cell_angle_beta                 97.696(3)
_cell_angle_gamma                109.057(3)
_cell_formula_units_Z            2
_cell_length_a                   10.9805(18)
_cell_length_b                   12.636(2)
_cell_length_c                   22.734(4)
_cell_measurement_reflns_used    9947
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      36.3025
_cell_measurement_theta_min      3.0789
_cell_volume                     2896.2(8)
_computing_cell_refinement       'SAINT software (Bruker AXS, 2004)'
_computing_data_collection       'APEX2 (Bruker AXS, 2005-2013)'
_computing_data_reduction        'SAINT software (Bruker AXS, 2004)'
_computing_molecular_graphics    'DIAMOND (Crystal Impact GbR, 1997-2014)'
_computing_structure_refinement  'SHELXL (G. M. Sheldrick, 2015)'
_computing_structure_solution    'SHELXT (G. M. Sheldrick, 2015)'
_diffrn_ambient_temperature      100(2)
_diffrn_detector_area_resol_mean 66.67
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device_type  'Bruker-AXS Kappa Mach3 APEX-II'
_diffrn_measurement_method       'CCD \f- and \w-scans'
_diffrn_radiation_monochromator  'Incoatec Helios mirrors'
_diffrn_radiation_source         1\mS
_diffrn_radiation_type           Mo-K\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.1152
_diffrn_reflns_av_unetI/netI     0.1127
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       32
_diffrn_reflns_limit_l_min       -32
_diffrn_reflns_number            81216
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         30.507
_diffrn_reflns_theta_min         2.997
_exptl_absorpt_coefficient_mu    1.755
_exptl_absorpt_correction_T_max  0.91815
_exptl_absorpt_correction_T_min  0.69583
_exptl_absorpt_correction_type   gaussian
_exptl_absorpt_process_details   'SADABS (Bruker AXS, 2012)'
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    1.399
_exptl_crystal_description       plate
_exptl_crystal_F_000             1276
_exptl_crystal_recrystallization_method
'Re-crystallisation from solvent: tetrahydrofuran'
_exptl_crystal_size_max          0.267
_exptl_crystal_size_mid          0.110
_exptl_crystal_size_min          0.083
_refine_diff_density_max         1.935
_refine_diff_density_min         -1.038
_refine_diff_density_rms         0.096
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.854
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     703
_refine_ls_number_reflns         17652
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.854
_refine_ls_R_factor_all          0.1123
_refine_ls_R_factor_gt           0.0494
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0869P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1132
_refine_ls_wR_factor_ref         0.1427
_reflns_Friedel_coverage         0.000
_reflns_number_gt                10491
_reflns_number_total             17652
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c7cc02320k2.cif
_cod_data_source_block           1
_cod_original_cell_volume        2896.1(8)
_cod_original_sg_symbol_Hall     '-p 1'
_cod_original_sg_symbol_H-M      'p -1'
_cod_database_code               7120279
_shelx_shelxl_version_number     2014/7
_shelx_estimated_absorpt_t_min   0.651
_shelx_estimated_absorpt_t_max   0.868
_shelx_res_checksum              39632