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_4118756
_publ_contact_author_name
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;
_publ_section_title
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 One-Pot Synthesis of an Fe(II) Bis-Terpyridine Complex with
 Allosterically Regulated Electronic Properties
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_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(C58 H48 Fe N6 P2 S2), 4(F6 P), C H2 Cl2'
_chemical_formula_sum            'C117 H98 Cl2 F24 Fe2 N12 P8 S4'
_chemical_formula_weight         2686.67
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_date             2012-01-18
_audit_creation_method
;
  Olex2 1.1
  (compiled Nov  1 2011 20:42:30, GUI svn.r3906)
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_audit_update_record
;
2012-01-17 # Formatted by publCIF
;
_cell_angle_alpha                81.963(2)
_cell_angle_beta                 75.9880(10)
_cell_angle_gamma                75.426(2)
_cell_formula_units_Z            4
_cell_length_a                   18.4572(6)
_cell_length_b                   20.9410(18)
_cell_length_c                   33.9256(11)
_cell_measurement_reflns_used    9435
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      64.53
_cell_measurement_theta_min      2.53
_cell_volume                     12269.6(12)
_computing_cell_refinement       'Bruker SAINT'
_computing_data_collection       'Bruker APEX2'
_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    'SHELXS-97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      99.99
_diffrn_detector_area_resol_mean 8
_diffrn_measured_fraction_theta_full 0.974
_diffrn_measured_fraction_theta_max 0.974
_diffrn_measurement_device_type  'Bruker Kappa APEX CCD area detector'
_diffrn_measurement_method       '\w and \f scans'
_diffrn_radiation_monochromator  'MX optics'
_diffrn_radiation_type           'CU K\a'
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0734
_diffrn_reflns_av_unetI/netI     0.0842
_diffrn_reflns_limit_h_max       21
_diffrn_reflns_limit_h_min       -20
_diffrn_reflns_limit_k_max       24
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       39
_diffrn_reflns_limit_l_min       -39
_diffrn_reflns_number            98215
_diffrn_reflns_theta_full        64.93
_diffrn_reflns_theta_max         64.93
_diffrn_reflns_theta_min         1.35
_diffrn_source                   microsource
_diffrn_source_current           0.65
_diffrn_source_power             0.02925
_diffrn_source_voltage           45.0
_exptl_absorpt_coefficient_mu    4.695
_exptl_absorpt_correction_T_max  0.7526
_exptl_absorpt_correction_T_min  0.5899
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2008/1 (Bruker,2008) was used for absorption correction.
R(int) was 0.0885 before and 0.0531 after correction.
The Ratio of minimum to maximum transmission is 0.7838.
The \l/2 correction factor is 0.0015.
;
_exptl_crystal_colour            violet
_exptl_crystal_colour_primary    violet
_exptl_crystal_density_diffrn    1.454
_exptl_crystal_description       block
_exptl_crystal_F_000             5480
_exptl_crystal_size_max          0.149
_exptl_crystal_size_mid          0.093
_exptl_crystal_size_min          0.038
_refine_diff_density_max         2.731
_refine_diff_density_min         -1.155
_refine_diff_density_rms         0.119
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.034
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     3200
_refine_ls_number_reflns         40649
_refine_ls_number_restraints     1449
_refine_ls_restrained_S_all      1.026
_refine_ls_R_factor_all          0.1252
_refine_ls_R_factor_gt           0.0816
_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^)+(0.1503P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2218
_refine_ls_wR_factor_ref         0.2458
_reflns_number_gt                25485
_reflns_number_total             40649
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja3045019_si_002_6.cif
_cod_data_source_block           n1539_dhj
_cod_database_code               4118756
_smtbx_masks_special_details
;
The solvent masking procedure as implemented in Olex2 was used to remove the
electronic contribution of solvent molecules from the refinement.  Only the
atoms used in the refinement model are reported in the formula here.

Total solvent accessible volume / cell = 1063.4 Ang^3^ [8.7%]
Total electron count / cell = 227.5
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