One-Pot Synthesis of an Fe(II) Bis-Terpyridine Complex with Allosterically Regulated Electronic Properties
Charles W. Machan; Mario Adelhardt; Amy A. Sarjeant; Charlotte L. Stern; Jörg Sutter; Karsten Meyer; Chad A. Mirkin; Journal of the American Chemical Society 134 (2012) 16921–16924; doi:10.1021/ja3045019

data_4118752
_publ_section_title
;
 One-Pot Synthesis of an Fe(II) Bis-Terpyridine Complex with
 Allosterically Regulated Electronic Properties
;
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              16921
_journal_page_last               16924
_journal_paper_doi               10.1021/ja3045019
_journal_volume                  134
_journal_year                    2012
_chemical_formula_moiety         '2(C88 H82 Cl2 Fe N6 P4 Pt2 S4), 7(F6 P), Cl '
_chemical_formula_sum            'C176 H164 Cl5 F42 Fe2 N12 P15 Pt4 S8'
_chemical_formula_weight         5035.53
_space_group_IT_number           60
_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_Hall  '-P 2n 2ab'
_symmetry_space_group_name_H-M   'P b c n'
_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                90.00
_cell_formula_units_Z            4
_cell_length_a                   24.3421(5)
_cell_length_b                   16.6719(4)
_cell_length_c                   51.6817(10)
_cell_measurement_reflns_used    8599
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      62.57
_cell_measurement_theta_min      3.32
_cell_volume                     20973.9(8)
_computing_cell_refinement       'Bruker SAINT'
_computing_data_collection       'Bruker APEX2'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 0.980
_diffrn_measured_fraction_theta_max 0.980
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_monochromator  'MX optics'
_diffrn_radiation_source         microsource
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54178
_diffrn_reflns_av_R_equivalents  0.0000
_diffrn_reflns_av_sigmaI/netI    0.1618
_diffrn_reflns_limit_h_max       28
_diffrn_reflns_limit_h_min       0
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       60
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_number            17712
_diffrn_reflns_theta_full        65.49
_diffrn_reflns_theta_max         65.49
_diffrn_reflns_theta_min         2.49
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    9.110
_exptl_absorpt_correction_T_max  0.7526
_exptl_absorpt_correction_T_min  0.5495
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS, Bruker'
_exptl_crystal_colour            purple
_exptl_crystal_density_diffrn    1.595
_exptl_crystal_description       plate
_exptl_crystal_F_000             9936
_exptl_crystal_size_max          0.12
_exptl_crystal_size_mid          0.07
_exptl_crystal_size_min          0.02
_platon_squeeze_details
;
 Diffuse, disordered solvent molecules could not be adequately modeled.  The
 bypass procedure in Platon (Spek, 1990) was used to remove the electronic
 contribution from these solvents. The total potential solvent accessible void
 volume was 3104.0 Ang^3^ and the electron count / cell = 1236. As the exact
 solvent content is not known, the reported formula reflects only the atoms
 used in the refinement.
;
_refine_diff_density_max         2.670
_refine_diff_density_min         -3.176
_refine_diff_density_rms         0.205
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.973
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1234
_refine_ls_number_reflns         17712
_refine_ls_number_restraints     1148
_refine_ls_restrained_S_all      0.946
_refine_ls_R_factor_all          0.1655
_refine_ls_R_factor_gt           0.0845
_refine_ls_shift/su_max          0.005
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.1222P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2033
_refine_ls_wR_factor_ref         0.2341
_reflns_number_gt                9002
_reflns_number_total             17712
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja3045019_si_002_2.cif
_cod_data_source_block           n1147
_cod_database_code               4118752