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_4345372
_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         'C84 H22 F30 Ga2 N10, 10 (C5 H5 N)'
_chemical_formula_sum            'C134 H72 F30 Ga2 N20'
_chemical_formula_weight         2671.56
_chemical_name_common            'Gross73 (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                96.33(5)
_cell_angle_beta                 98.49(3)
_cell_angle_gamma                90.73(12)
_cell_formula_units_Z            1
_cell_length_a                   9.22(3)
_cell_length_b                   15.59(6)
_cell_length_c                   20.27(4)
_cell_measurement_reflns_used    8464
_cell_measurement_temperature    200(2)
_cell_measurement_theta_max      24.14
_cell_measurement_theta_min      1.31
_cell_volume                     2863(16)
_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 0.986
_diffrn_measured_fraction_theta_max 0.986
_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  0.0910
_diffrn_reflns_av_sigmaI/netI    0.0447
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       0
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_number            8717
_diffrn_reflns_theta_full        24.14
_diffrn_reflns_theta_max         24.14
_diffrn_reflns_theta_min         1.31
_diffrn_standards_decay_%        none
_diffrn_standards_interval_count none
_diffrn_standards_interval_time  none
_diffrn_standards_number         none
_exptl_absorpt_coefficient_mu    0.584
_exptl_absorpt_correction_T_max  0.9075
_exptl_absorpt_correction_T_min  0.8342
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
; 
'HKL Denzo and Scalepack (Otwinowski & Minor 1997)'  
;
_exptl_crystal_colour            'dark violet'
_exptl_crystal_density_diffrn    1.550
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             1348
_exptl_crystal_size_max          0.30
_exptl_crystal_size_mid          0.24
_exptl_crystal_size_min          0.15
_refine_diff_density_max         0.677
_refine_diff_density_min         -0.529
_refine_diff_density_rms         0.070
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.074
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     838
_refine_ls_number_reflns         8717
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.074
_refine_ls_R_factor_all          0.0791
_refine_ls_R_factor_gt           0.0634
_refine_ls_shift/su_max          0.007
_refine_ls_shift/su_mean         0.001
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0850P)^2^+4.4780P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1632
_refine_ls_wR_factor_ref         0.1714
_reflns_number_gt                7157
_reflns_number_total             8717
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic6b02944_si_002.cif
_cod_data_source_block           Gross73
_cod_original_cell_volume        2862(15)
_cod_database_code               4345372