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_7120278
_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         'C50 H56 Cs2 O10'
_chemical_formula_sum            'C50 H56 Cs2 O10'
_chemical_formula_weight         1082.76
_chemical_name_systematic
'catena(bis(2,5,8,11,14-Pentaoxapentadecane-caesium)- diindeno[1,2,3-fg:1',2',3'-op]tetracene)'
_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'
_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                10171_DOPT_Cs_Tetraglyme_Wombacher_100K
_audit_creation_date             2016-07-25
_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                74.5693(19)
_cell_angle_beta                 77.5731(19)
_cell_angle_gamma                73.379(2)
_cell_formula_units_Z            2
_cell_length_a                   11.1914(14)
_cell_length_b                   11.5224(14)
_cell_length_c                   20.297(2)
_cell_measurement_reflns_used    9739
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      36.2642
_cell_measurement_theta_min      2.6413
_cell_volume                     2390.0(5)
_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 0.988
_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  0.0308
_diffrn_reflns_av_unetI/netI     0.0303
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.988
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_h_min       -18
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       33
_diffrn_reflns_limit_l_min       -33
_diffrn_reflns_number            92073
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.988
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         36.313
_diffrn_reflns_theta_min         3.309
_exptl_absorpt_coefficient_mu    1.581
_exptl_absorpt_correction_T_max  0.74870
_exptl_absorpt_correction_T_min  0.67407
_exptl_absorpt_correction_type   gaussian
_exptl_absorpt_process_details   'SADABS (Bruker AXS, 2012)'
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    1.505
_exptl_crystal_description       block
_exptl_crystal_F_000             1092
_exptl_crystal_recrystallization_method
'Re-crystallisation from solvent: tetraglyme'
_exptl_crystal_size_max          0.354
_exptl_crystal_size_mid          0.352
_exptl_crystal_size_min          0.344
_refine_diff_density_max         3.202
_refine_diff_density_min         -2.589
_refine_diff_density_rms         0.117
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.072
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     582
_refine_ls_number_reflns         22883
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.072
_refine_ls_R_factor_all          0.0634
_refine_ls_R_factor_gt           0.0431
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0362P)^2^+4.6289P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0984
_refine_ls_wR_factor_ref         0.1101
_reflns_Friedel_coverage         0.000
_reflns_number_gt                17653
_reflns_number_total             22883
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c7cc02320k2.cif
_cod_data_source_block           2
_cod_original_sg_symbol_Hall     '-p 1'
_cod_original_sg_symbol_H-M      'p -1'
_cod_database_code               7120278
_shelx_shelxl_version_number     2014/7
_shelx_estimated_absorpt_t_min   0.604
_shelx_estimated_absorpt_t_max   0.612
_shelx_res_checksum              6094