Geometric and redox flexibility of pyridine as a redox-active ligand that can reversibly accept one or two electrons
Richard A. Lewis; K. Cory MacLeod; Brandon Q. Mercado; Patrick L. Holland; Chem.Commun. 50 (2014) 11114–; doi:10.1039/C4cc05495D

data_7115648
_publ_section_title
;
 Geometric and redox flexibility of pyridine as a redox-active ligand that
 can reversibly accept one or two electrons
;
_journal_name_full               Chem.Commun.
_journal_page_first              11114
_journal_paper_doi               10.1039/C4cc05495D
_journal_volume                  50
_journal_year                    2014
_chemical_formula_moiety         'C54 H64 Fe2 N6, 1/2(C5 H12)'
_chemical_formula_sum            'C56.5 H70 Fe2 N6'
_chemical_formula_weight         944.88
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2yn'
_space_group_name_H-M_alt        'P 1 21/n 1'
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 1'
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-2013
_cell_angle_alpha                90
_cell_angle_beta                 104.422(7)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   15.9655(3)
_cell_length_b                   14.7809(3)
_cell_length_c                   21.7126(15)
_cell_measurement_reflns_used    80981
_cell_measurement_temperature    93(2)
_cell_measurement_theta_max      66.8
_cell_measurement_theta_min      2.1
_cell_volume                     4962.4(4)
_computing_cell_refinement       'CrystalClear-SM Expert 2.0 r15 (Rigaku, 2011)'
_computing_data_collection       'CrystalClear-SM Expert 2.0 r15 (Rigaku, 2011)'
_computing_data_reduction        'CrystalClear-SM Expert 2.0 r15 (Rigaku, 2011)'
_computing_molecular_graphics
;
Dolomanov, O.V.; Bourhis, L.J.; Gildea, R.J.; Howard, J.A.K.; Puschmann, H., 
OLEX2: A complete structure solution, refinement and analysis program
(2009). J. Appl. Cryst., 42, 339-341.
;
_computing_publication_material  'SHELXL-2013 (Sheldrick, 2013)'
_computing_structure_refinement  'SHELXL-2013 (Sheldrick, 2013)'
_computing_structure_solution    'SHELXS-2013 (Sheldrick, 2013)'
_diffrn_ambient_temperature      93(2)
_diffrn_detector_area_resol_mean 22.2
_diffrn_measured_fraction_theta_full 0.972
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device_type  'Rigaku Saturn 944+ CCD'
_diffrn_measurement_method       \w
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54187
_diffrn_reflns_av_R_equivalents  0.0592
_diffrn_reflns_av_unetI/netI     0.0261
_diffrn_reflns_Laue_measured_fraction_full 0.972
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_h_min       -18
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       25
_diffrn_reflns_limit_l_min       -25
_diffrn_reflns_number            115206
_diffrn_reflns_point_group_measured_fraction_full 0.972
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_theta_full        67.687
_diffrn_reflns_theta_max         66.602
_diffrn_reflns_theta_min         3.097
_diffrn_source                   'Rotating Anode'
_exptl_absorpt_coefficient_mu    5.011
_exptl_absorpt_correction_T_max  0.483
_exptl_absorpt_correction_T_min  0.398
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'Jacobson, R. (1998) Private Communication'
_exptl_crystal_colour            Colorless
_exptl_crystal_density_diffrn    1.265
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       Block
_exptl_crystal_F_000             2012
_exptl_crystal_size_max          0.200
_exptl_crystal_size_mid          0.190
_exptl_crystal_size_min          0.170
_refine_diff_density_max         0.372
_refine_diff_density_min         -0.363
_refine_diff_density_rms         0.046
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.108
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     629
_refine_ls_number_reflns         8733
_refine_ls_number_restraints     31
_refine_ls_restrained_S_all      1.106
_refine_ls_R_factor_all          0.0402
_refine_ls_R_factor_gt           0.0361
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0420P)^2^+2.8228P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0916
_refine_ls_wR_factor_ref         0.0943
_reflns_Friedel_coverage         0.000
_reflns_number_gt                7916
_reflns_number_total             8733
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c4cc05495d2.cif
_cod_data_source_block           007-13130
_cod_original_formula_sum        'C56.50 H70 Fe2 N6'
_cod_database_code               7115648
_shelx_estimated_absorpt_t_min   0.434
_shelx_estimated_absorpt_t_max   0.483
_shelxl_version_number           2013-4
_shelx_res_checksum              81449