Spin Transitions in Fe(II) Metallogrids Modulated by Substituents, Counteranions, and Solvents
Yi-Tong Wang; Shu-Tao Li; Shu-Qi Wu; Ai-Li Cui; De-Zhong Shen; Hui-Zhong Kou; Journal of the American Chemical Society 135 (2013) 5942–5945; doi:10.1021/ja312622c

data_4119606
_publ_contact_author_address
;
Department of Chemistry
Tsinghua University
Beijing 100084
People's Republic of China
;
_publ_contact_author_email       kouhz@mail.tsinghua.edu.cn
_publ_contact_author_name        'Dr. Hui-Zhong Kou'
_publ_contact_author_phone       86-10-62771748
_publ_section_title
;
 Spin Transitions in Fe(II) Metallogrids Modulated by Substituents,
 Counteranions, and Solvents
;
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              5942
_journal_page_last               5945
_journal_paper_doi               10.1021/ja312622c
_journal_volume                  135
_journal_year                    2013
_chemical_formula_sum            'C64 H62 Br8 Cl4 Fe4 N32 O9'
_chemical_formula_weight         2427.94
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           167
_symmetry_cell_setting           rhombohedral
_symmetry_space_group_name_Hall  '-P 3* 2n'
_symmetry_space_group_name_H-M   'R -3 c :R'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                100.291(17)
_cell_angle_beta                 100.291(17)
_cell_angle_gamma                100.291(17)
_cell_formula_units_Z            6
_cell_length_a                   23.685(3)
_cell_length_b                   23.685(3)
_cell_length_c                   23.685(3)
_cell_measurement_reflns_used    32653
_cell_measurement_temperature    153(2)
_cell_measurement_theta_max      27.4956
_cell_measurement_theta_min      3.0112
_cell_volume                     12555(3)
_computing_cell_refinement       'CrystalClear (Rigaku Inc., 2008)'
_computing_data_collection       'CrystalClear (Rigaku Inc., 2008)'
_computing_data_reduction        'CrystalClear (Rigaku Inc., 2008)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      153(2)
_diffrn_detector_area_resol_mean 28.5714
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device_type  'Saturn724+ (2x2 bin mode)'
_diffrn_measurement_method       dtprofit.ref
_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  0.1071
_diffrn_reflns_av_sigmaI/netI    0.0493
_diffrn_reflns_limit_h_max       28
_diffrn_reflns_limit_h_min       -27
_diffrn_reflns_limit_k_max       28
_diffrn_reflns_limit_k_min       -21
_diffrn_reflns_limit_l_max       28
_diffrn_reflns_limit_l_min       -28
_diffrn_reflns_number            81724
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         25.00
_diffrn_reflns_theta_min         3.01
_exptl_absorpt_coefficient_mu    4.701
_exptl_absorpt_correction_T_max  1.0000
_exptl_absorpt_correction_T_min  0.5254
_exptl_absorpt_correction_type   empirical
_exptl_crystal_colour            black
_exptl_crystal_density_diffrn    1.927
_exptl_crystal_description       block
_exptl_crystal_F_000             7164
_exptl_crystal_size_max          0.30
_exptl_crystal_size_mid          0.30
_exptl_crystal_size_min          0.10
_refine_diff_density_max         1.323
_refine_diff_density_min         -1.241
_refine_diff_density_rms         0.138
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.021
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     556
_refine_ls_number_reflns         7357
_refine_ls_number_restraints     18
_refine_ls_restrained_S_all      1.020
_refine_ls_R_factor_all          0.1402
_refine_ls_R_factor_gt           0.1332
_refine_ls_shift/su_max          0.004
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0897P)^2^+391.1866P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2793
_refine_ls_wR_factor_ref         0.2849
_reflns_number_gt                6961
_reflns_number_total             7357
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja312622c_si_002_2.cif
_cod_data_source_block           1
_cod_original_cell_volume        12555(2)
_cod_original_sg_symbol_H-M      'R -3 c'
_cod_database_code               4119606