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_4118753
_publ_contact_author_name
;
;
_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         'C88 H82 Fe N6 P4 Pt2 S4, 6(F6 P)'
_chemical_formula_sum            'C88 H82 F36 Fe N6 P10 Pt2 S4'
_chemical_formula_weight         2791.57
_chemical_name_systematic
;
 ? 
;
_space_group_crystal_system      orthorhombic
_space_group_IT_number           60
_space_group_name_Hall           '-P 2n 2ab'
_space_group_name_H-M_alt        'P b c n'
_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_date             2011-08-18
_audit_creation_method
;
  Olex2 1.1
  (compiled Aug 18 2011 06:34:35, GUI svn.r3819)
;
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   23.0433(14)
_cell_length_b                   13.5812(9)
_cell_length_c                   43.188(2)
_cell_measurement_reflns_used    9959
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      26.47
_cell_measurement_theta_min      2.32
_cell_volume                     13515.9(14)
_computing_cell_refinement       'SAINT V7.23A (Bruker, 2005)'
_computing_data_collection       'APEX2 V2.1-4 (Bruker, 2007)'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics
;
O. V. Dolomanov, L. J. Bourhis, R. J. Gildea, J. A. K. Howard and H. Puschmann,
OLEX2: a complete structure solution, refinement and analysis program.
J. Appl. Cryst. (2009). 42, 339-341.
;
_computing_publication_material
;
O. V. Dolomanov, L. J. Bourhis, R. J. Gildea, J. A. K. Howard and H. Puschmann,
OLEX2: a complete structure solution, refinement and analysis program.
J. Appl. Cryst. (2009). 42, 339-341.
;
_computing_structure_refinement
;
XL, G.M. Sheldrick, Acta Cryst.
(2008). A64, 112-122
;
_computing_structure_solution
;
XM, G.M. Sheldrick, Acta Cryst.
(2008). A64, 112-122
;
_diffrn_ambient_temperature      99.99
_diffrn_detector_area_resol_mean 8
_diffrn_measured_fraction_theta_full 0.992
_diffrn_measured_fraction_theta_max 0.992
_diffrn_measurement_device_type  'Bruker SMART APEX CCD area detector'
_diffrn_measurement_method       '\w and \f scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.1810
_diffrn_reflns_av_unetI/netI     0.1140
_diffrn_reflns_limit_h_max       28
_diffrn_reflns_limit_h_min       -28
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       53
_diffrn_reflns_limit_l_min       -54
_diffrn_reflns_number            115182
_diffrn_reflns_theta_full        26.61
_diffrn_reflns_theta_max         26.61
_diffrn_reflns_theta_min         0.88
_diffrn_source                   'sealed tube'
_diffrn_source_current           30.0
_diffrn_source_power             1.5
_diffrn_source_voltage           50.0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    2.437
_exptl_absorpt_correction_T_max  0.5567
_exptl_absorpt_correction_T_min  0.4524
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
"SADABS-2008/1 (Bruker,2008) was used for absorption correction.
R(int) was 0.1054 before and 0.0877 after correction.
The Ratio of minimum to maximum transmission is 0.8126.
The \l/2 correction factor is 0.00.
{Info from Y:\Amy\n1254\n1254.abs}
;
_exptl_crystal_colour            purple
_exptl_crystal_density_diffrn    1.372
_exptl_crystal_description       block
_exptl_crystal_F_000             5488
_exptl_crystal_size_max          0.252
_exptl_crystal_size_mid          0.1
_exptl_crystal_size_min          0.083
_refine_diff_density_max         2.428
_refine_diff_density_min         -2.976
_refine_diff_density_rms         0.180
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.017
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     664
_refine_ls_number_reflns         14060
_refine_ls_number_restraints     223
_refine_ls_restrained_S_all      1.013
_refine_ls_R_factor_all          0.1231
_refine_ls_R_factor_gt           0.0715
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0976P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1766
_refine_ls_wR_factor_ref         0.1940
_reflns_number_gt                7761
_reflns_number_total             14060
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja3045019_si_002_3.cif
_cod_data_source_block           n1254
_cod_original_cell_volume        13516.0(14)
_cod_database_code               4118753
_smtbx_masks_special_details
;
Total solvent accessible volume / cell = 4684.3 Ang^3^ [34.7%]
Total electron count / cell = 1167.5
;