Anion-templated self-assembly of highly stable Fe(II) pentagonal metallacycles with short anion–π contacts
Giles, Ian D.; Chifotides, Helen T.; Shatruk, Michael; Dunbar, Kim R.; Chemical Communications (Cambridge, United Kingdom) 47 (2011) 12604–12606; doi:10.1039/c1cc15868f

data_7107088
_publ_section_title
;
 Anion-templated self-assembly of highly stable Fe(II) pentagonal
 metallacycles with short anion--\p contacts
;
_journal_coden_ASTM              CHCOFS
_journal_issue                   47
_journal_name_full
;
 Chemical Communications (Cambridge, United Kingdom)
;
_journal_page_first              12604
_journal_page_last               12606
_journal_paper_doi               10.1039/c1cc15868f
_journal_volume                  47
_journal_year                    2011
_chemical_formula_moiety         'C70 H60 N50 Fe5, 5(Sb F6), 6.5(CH3CN), C7H8'
_chemical_formula_sum            'C90 H87.5 F60 Fe5 N56.5 Sb10'
_chemical_formula_weight         4597.42
_chemical_name_common
;
pentakis(3,6-bis(pyrimid-2-yl)-1,2,4,5-tetrazine-
N,N',N'',N''')-decakis(acetonitrile-N)-
pentairon(ii)hexafluoroantimonate(V) clathrate
nonakis(hexafluoroantimonate(V)) acetonitrile toluene solvate'
;
_chemical_name_systematic
;
pentakis(3,6-bis(pyrimid-2-yl)-1,2,4,5-tetrazine-N,N',N'',N''')-
decakis(acetonitrile-N)-pentairon(II)hexafluoroantimonate(V) clathrate
nonakis(hexafluoroantimonate(V)) acetonitrile toluene solvate'
;
_chemical_properties_physical    'air-sensitive, moisture-sensitive'
_space_group_IT_number           7
_symmetry_cell_setting           monoclinic
_symmetry_Int_Tables_number      7
_symmetry_space_group_name_Hall  'P -2yc'
_symmetry_space_group_name_H-M   'P 1 c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 106.198(2)
_cell_angle_gamma                90.00
_cell_formula_units_Z            2
_cell_length_a                   16.180(3)
_cell_length_b                   21.569(4)
_cell_length_c                   23.123(4)
_cell_measurement_reflns_used    727
_cell_measurement_temperature    163(2)
_cell_measurement_theta_max      31.81
_cell_measurement_theta_min      2.53
_cell_volume                     7749(2)
_computing_cell_refinement       'APEXII, (Bruker 2008)'
_computing_data_collection       'APEXII, (Bruker 2008)'
_computing_data_reduction        XPREP
_computing_molecular_graphics    'X-Seed (Barbour, 1999)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      163(2)
_diffrn_detector_area_resol_mean 66
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measurement_device_type
;
Bruker APEX2 CCD area-detector, SMART 3 circle goniometer'
;
_diffrn_measurement_method       'profile data from \w scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.1453
_diffrn_reflns_av_sigmaI/netI    0.2149
_diffrn_reflns_limit_h_max       20
_diffrn_reflns_limit_h_min       -20
_diffrn_reflns_limit_k_max       26
_diffrn_reflns_limit_k_min       -26
_diffrn_reflns_limit_l_max       28
_diffrn_reflns_limit_l_min       -28
_diffrn_reflns_number            82034
_diffrn_reflns_theta_full        26.41
_diffrn_reflns_theta_max         26.41
_diffrn_reflns_theta_min         1.31
_exptl_absorpt_coefficient_mu    2.295
_exptl_absorpt_correction_T_max  0.9555
_exptl_absorpt_correction_T_min  0.7863
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'Bruker AXS Scale, SADABS (Bruker 2008)'
_exptl_crystal_colour            dark-blue
_exptl_crystal_density_diffrn    1.970
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       needle
_exptl_crystal_F_000             4406
_exptl_crystal_recrystallization_method
;
acetonitrile solution layered over toluene
;
_exptl_crystal_size_max          0.11
_exptl_crystal_size_mid          0.04
_exptl_crystal_size_min          0.02
_refine_diff_density_max         1.536
_refine_diff_density_min         -1.604
_refine_diff_density_rms         0.160
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   0.34(2)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.940
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1870
_refine_ls_number_reflns         31659
_refine_ls_number_restraints     2
_refine_ls_restrained_S_all      0.940
_refine_ls_R_factor_all          0.1960
_refine_ls_R_factor_gt           0.0780
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0817P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1599
_refine_ls_wR_factor_ref         0.2097
_reflns_number_gt                13427
_reflns_number_total             31659
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c1cc15868f.txt
_cod_data_source_block           pc_sept15_michael_bmtz_pentagon
_cod_original_sg_symbol_H-M      'P c'
_cod_original_formula_sum        'C90 H87.50 F60 Fe5 N56.50 Sb10'
_cod_database_code               7107088