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_7115649
_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_absolute_configuration ad
_chemical_formula_moiety         '2(C64 H74 Fe2 N8), C5 H5 N, 3(C4 H10 O)'
_chemical_formula_sum            'C145 H183 Fe4 N17 O3'
_chemical_formula_weight         2435.47
_chemical_name_systematic
; 
 ? 
;
_space_group_crystal_system      orthorhombic
_space_group_IT_number           29
_space_group_name_Hall           'P 2c -2ac'
_space_group_name_H-M_alt        'P c a 21'
_symmetry_space_group_name_Hall  'P 2c -2ac'
_symmetry_space_group_name_H-M   'P c a 21'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-2013
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   27.6897(2)
_cell_length_b                   11.5655(5)
_cell_length_c                   42.052(3)
_cell_measurement_reflns_used    146873
_cell_measurement_temperature    93(2)
_cell_measurement_theta_max      68.0
_cell_measurement_theta_min      1.9
_cell_volume                     13467.0(11)
_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 0.945
_diffrn_measured_fraction_theta_max 1.000
_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  0.2488
_diffrn_reflns_av_unetI/netI     0.1083
_diffrn_reflns_Laue_measured_fraction_full 0.945
_diffrn_reflns_Laue_measured_fraction_max 1.000
_diffrn_reflns_limit_h_max       32
_diffrn_reflns_limit_h_min       -32
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       49
_diffrn_reflns_limit_l_min       -49
_diffrn_reflns_number            447121
_diffrn_reflns_point_group_measured_fraction_full 0.945
_diffrn_reflns_point_group_measured_fraction_max 1.000
_diffrn_reflns_theta_full        67.687
_diffrn_reflns_theta_max         65.086
_diffrn_reflns_theta_min         2.101
_diffrn_source                   'Rotating Anode'
_exptl_absorpt_coefficient_mu    3.832
_exptl_absorpt_correction_T_max  0.894
_exptl_absorpt_correction_T_min  0.630
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'Jacobson, R. (1998) Private Communication'
_exptl_crystal_colour            Red
_exptl_crystal_density_diffrn    1.201
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       Block
_exptl_crystal_F_000             5200
_exptl_crystal_size_max          0.050
_exptl_crystal_size_mid          0.030
_exptl_crystal_size_min          0.030
_refine_diff_density_max         0.556
_refine_diff_density_min         -0.397
_refine_diff_density_rms         0.096
_refine_ls_abs_structure_details
; 
 Flack x determined using 4731 quotients [(I+)-(I-)]/[(I+)+(I-)] 
 (Parsons and Flack (2004), Acta Cryst. A60, s61). 
;
_refine_ls_abs_structure_Flack   0.083(3)
_refine_ls_extinction_coef       0.00137(9)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     SHELXL
_refine_ls_goodness_of_fit_ref   0.947
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1621
_refine_ls_number_reflns         22989
_refine_ls_number_restraints     765
_refine_ls_restrained_S_all      0.937
_refine_ls_R_factor_all          0.1250
_refine_ls_R_factor_gt           0.0756
_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^)+(0.1166P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1701
_refine_ls_wR_factor_ref         0.2021
_reflns_Friedel_coverage         0.969
_reflns_Friedel_fraction_full    0.944
_reflns_Friedel_fraction_max     1.000
_reflns_number_gt                12937
_reflns_number_total             22989
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c4cc05495d2.cif
_cod_data_source_block           007-14047
_cod_original_cell_volume        13467.1(11)
_cod_database_code               7115649
_shelx_estimated_absorpt_t_min   0.832
_shelx_estimated_absorpt_t_max   0.894
_shelxl_version_number           2013-3
_shelx_res_checksum              52560