Anion-Dependent Formation of Helicates versus Mesocates of Triple-Stranded M2L3 (M = Fe2+, Cu2+) Complexes
Fengjuan Cui; Shaoguang Li; Chuandong Jia; Jennifer S. Mathieson; Leroy Cronin; Xiao-Juan Yang; Biao Wu; Inorganic Chemistry 51 (2012) 179–187; doi:10.1021/ic201417y

data_4327750
_publ_section_title
;
 Anion-Dependent Formation of Helicates versus Mesocates of
 Triple-Stranded M2L3 (M = Fe2+, Cu2+) Complexes
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              179
_journal_page_last               187
_journal_paper_doi               10.1021/ic201417y
_journal_volume                  51
_journal_year                    2012
_chemical_formula_sum            'C81 H72 B7 F28 Fe2 N21'
_chemical_formula_weight         2058.97
_space_group_IT_number           146
_symmetry_cell_setting           rhombohedral
_symmetry_space_group_name_Hall  'R 3'
_symmetry_space_group_name_H-M   'R 3 :H'
_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                 90.00
_cell_angle_gamma                120.00
_cell_formula_units_Z            3
_cell_length_a                   20.542(2)
_cell_length_b                   20.542(2)
_cell_length_c                   17.928(2)
_cell_measurement_reflns_used    6647
_cell_measurement_temperature    153(2)
_cell_measurement_theta_max      26.37
_cell_measurement_theta_min      2.54
_cell_volume                     6551.6(12)
_computing_cell_refinement       'Bruker SMART'
_computing_data_collection       'Bruker SMART APEX II'
_computing_data_reduction        'Bruker SAINT'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      153(2)
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device_type  'Bruker APEX II area detector'
_diffrn_measurement_method       '\w 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  0.0295
_diffrn_reflns_av_sigmaI/netI    0.0450
_diffrn_reflns_limit_h_max       23
_diffrn_reflns_limit_h_min       -25
_diffrn_reflns_limit_k_max       25
_diffrn_reflns_limit_k_min       -25
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_number            15403
_diffrn_reflns_theta_full        26.37
_diffrn_reflns_theta_max         26.37
_diffrn_reflns_theta_min         1.61
_exptl_absorpt_coefficient_mu    0.451
_exptl_absorpt_correction_T_max  0.8765
_exptl_absorpt_correction_T_min  0.8401
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   SADABS
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    1.566
_exptl_crystal_description       block
_exptl_crystal_F_000             3132
_exptl_crystal_size_max          0.40
_exptl_crystal_size_mid          0.35
_exptl_crystal_size_min          0.30
_refine_diff_density_max         0.651
_refine_diff_density_min         -0.352
_refine_diff_density_rms         0.062
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   0.026(18)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.045
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     474
_refine_ls_number_reflns         5944
_refine_ls_number_restraints     39
_refine_ls_restrained_S_all      1.115
_refine_ls_R_factor_all          0.0533
_refine_ls_R_factor_gt           0.0461
_refine_ls_shift/su_max          0.054
_refine_ls_shift/su_mean         0.006
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0734P)^2^+4.7547P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1185
_refine_ls_wR_factor_ref         0.1238
_reflns_number_gt                5269
_reflns_number_total             5944
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic201417y_si_002_2.cif
_cod_data_source_block           LFeBF4
_cod_original_cell_volume        6551.6(13)
_cod_original_sg_symbol_H-M      'R 3'
_cod_database_code               4327750