Synthesis, Characterization, and Electrochemistry of a Series of Iron(II) Complexes Containing Self-Assembled 1,5-Diaza-3,7-diphosphabicyclo[3.3.1]nonane Ligands
Andrew D. Burrows; Ross W. Harrington; Andrew S. Kirk; Mary F. Mahon; Frank Marken; John E. Warren; Michael K. Whittlesey; Inorganic Chemistry 48 (2009) 9924–9935; doi:10.1021/ic900874f

data_4303376
_publ_section_title
;
Synthesis, Characterization, and Electrochemistry of a Series of Iron(II)
Complexes Containing Self-Assembled
1,5-Diaza-3,7-diphosphabicyclo[3.3.1]nonane Ligands
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              9924
_journal_page_last               9935
_journal_paper_doi               10.1021/ic900874f
_journal_volume                  48
_journal_year                    2009
_chemical_formula_sum            'C35 H54 Fe N4 O10 P4'
_chemical_formula_weight         870.55
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_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_method           SHELXL-97
_cell_angle_alpha                87.925(1)
_cell_angle_beta                 79.223(1)
_cell_angle_gamma                65.600(1)
_cell_formula_units_Z            2
_cell_length_a                   9.4170(2)
_cell_length_b                   10.5490(2)
_cell_length_c                   22.2750(6)
_cell_measurement_reflns_used    45119
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      27.485
_cell_measurement_theta_min      2.910
_cell_volume                     1977.53(8)
_computing_cell_refinement       'HKL Scalepack (Otwinowski & Minor 1997)'
_computing_data_collection       'Collect (Bruker AXS BV, 1997-2004)'
_computing_data_reduction        'Denzo & Scalepack (Otwinowski & Minor,1997)'
_computing_molecular_graphics    'ORTEX (P.McArdle, 1995)'
_computing_publication_material  'SHELXL-97/2 (Sheldrick,1997)'
_computing_structure_refinement  'SHELXL-97/2 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      150(2)
_diffrn_measured_fraction_theta_full 0.964
_diffrn_measured_fraction_theta_max 0.964
_diffrn_measurement_device_type  '95mm CCD camera on \k-goniostat'
_diffrn_measurement_method       CCD
_diffrn_radiation_monochromator  'horizonally mounted graphite crystal'
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0707
_diffrn_reflns_av_sigmaI/netI    0.0737
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       28
_diffrn_reflns_limit_l_min       -28
_diffrn_reflns_number            23946
_diffrn_reflns_theta_full        27.54
_diffrn_reflns_theta_max         27.54
_diffrn_reflns_theta_min         3.97
_exptl_absorpt_coefficient_mu    0.604
_exptl_absorpt_correction_T_max  0.9704
_exptl_absorpt_correction_T_min  0.8637
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
multi-scan from symmetry-related measurements 
Sortav (Blessing 1995)
;
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    1.462
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             916
_exptl_crystal_size_max          0.25
_exptl_crystal_size_mid          0.15
_exptl_crystal_size_min          0.05
_refine_diff_density_max         0.784
_refine_diff_density_min         -0.691
_refine_diff_density_rms         0.095
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.128
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     529
_refine_ls_number_reflns         8787
_refine_ls_number_restraints     21
_refine_ls_restrained_S_all      1.126
_refine_ls_R_factor_all          0.0835
_refine_ls_R_factor_gt           0.0618
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0482P)^2^+3.6302P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1406
_refine_ls_wR_factor_ref         0.1517
_reflns_number_gt                6814
_reflns_number_total             8787
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic900874f_si_001_4.cif
_cod_data_source_block           compound_5_k07adb2
_cod_database_code               4303376