The Planar Cyclooctatetraene Bridge in Bis-Metallic Macrocycles: Isolating or Conjugating?
Bhowmik, Susovan; Kosa, Monica; Mizrahi, Amir; Fridman, Natalia; Saphier, Magal; Stanger, Amnon; Gross, Zeev; Inorganic chemistry 56 (2017) 2287–2296; doi:10.1021/acs.inorgchem.6b02944

data_4345371
_publ_section_title
;
 The Planar Cyclooctatetraene Bridge in Bis-Metallic Macrocycles:
 Isolating or Conjugating?
;
_journal_issue                   4
_journal_name_full               'Inorganic chemistry'
_journal_page_first              2287
_journal_page_last               2296
_journal_paper_doi               10.1021/acs.inorgchem.6b02944
_journal_volume                  56
_journal_year                    2017
_chemical_formula_moiety         'C74 H18 F30 N8'
_chemical_formula_sum            'C74 H18 F30 N8'
_chemical_formula_weight         1588.96
_chemical_name_common            'Gross71 (Susovan)'
_chemical_name_systematic
; 
 ? 
;
_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                113.361(6)
_cell_angle_beta                 94.325(4)
_cell_angle_gamma                97.777(10)
_cell_formula_units_Z            1
_cell_length_a                   6.331(6)
_cell_length_b                   15.802(6)
_cell_length_c                   15.896(9)
_cell_measurement_reflns_used    4156
_cell_measurement_temperature    200(2)
_cell_measurement_theta_max      24.14
_cell_measurement_theta_min      1.41
_cell_volume                     1431.8(17)
_computing_cell_refinement       'DENZO HKL2000 (Otwinowski & Minor 1997)'
_computing_data_collection       'Collect (Nonius, 2006)'
_computing_data_reduction        'DENZO HKL2000 (Otwinowski & Minor 1997)'
_computing_molecular_graphics    'Mercury 3.5'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      200(2)
_diffrn_detector_area_resol_mean 95
_diffrn_measured_fraction_theta_full 0.985
_diffrn_measured_fraction_theta_max 0.985
_diffrn_measurement_device_type  'Nonius KappaCCD'
_diffrn_measurement_method       'phi- and omega-scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0830
_diffrn_reflns_av_sigmaI/netI    0.0566
_diffrn_reflns_limit_h_max       7
_diffrn_reflns_limit_h_min       0
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            4311
_diffrn_reflns_theta_full        24.14
_diffrn_reflns_theta_max         24.14
_diffrn_reflns_theta_min         1.41
_diffrn_standards_decay_%        none
_diffrn_standards_interval_count none
_diffrn_standards_interval_time  none
_diffrn_standards_number         none
_exptl_absorpt_coefficient_mu    0.179
_exptl_absorpt_correction_T_max  0.9741
_exptl_absorpt_correction_T_min  0.9238
_exptl_absorpt_process_details
; 
'HKL Denzo and Scalepack (Otwinowski & Minor 1997)'  
;
_exptl_crystal_colour            brown
_exptl_crystal_density_diffrn    1.843
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             788
_exptl_crystal_size_max          0.45
_exptl_crystal_size_mid          0.15
_exptl_crystal_size_min          0.09
_refine_diff_density_max         0.365
_refine_diff_density_min         -0.269
_refine_diff_density_rms         0.066
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.045
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     517
_refine_ls_number_reflns         4311
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.045
_refine_ls_R_factor_all          0.1011
_refine_ls_R_factor_gt           0.0673
_refine_ls_shift/su_max          0.020
_refine_ls_shift/su_mean         0.004
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.1115P)^2^+1.0115P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1750
_refine_ls_wR_factor_ref         0.1955
_reflns_number_gt                2978
_reflns_number_total             4311
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic6b02944_si_004.cif
_cod_data_source_block           Gross71
_cod_original_cell_volume        1431.8(16)
_cod_database_code               4345371