Redox behaviour of ([fc(NP<sup>i</sup>Pr<sub>2</sub>)<sub>2</sub>]Fe)<sub>2</sub>, formation of an iron-iron bond and cleavage of azobenzene.
Pick, Fraser S.; Leznoff, Daniel B.; Fryzuk, Michael D.; Dalton transactions (Cambridge, England : 2003) 47 (2018) 10925–10931; doi:10.1039/c8dt00828k

data_7046853
_publ_section_title
;
 Redox behaviour of
 ([fc(NP<sup>i</sup>Pr<sub>2</sub>)<sub>2</sub>]Fe)<sub>2</sub>, formation
 of an iron-iron bond and cleavage of azobenzene.
;
_journal_issue                   32
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              10925
_journal_page_last               10931
_journal_paper_doi               10.1039/c8dt00828k
_journal_volume                  47
_journal_year                    2018
_chemical_formula_moiety         '0.5(C22 H36 Fe2 I4 N2 P2), 0.5(C7 H8)'
_chemical_formula_sum            'C14.5 H22 Fe I2 N P'
_chemical_formula_weight         550.95
_space_group_crystal_system      monoclinic
_space_group_IT_number           9
_space_group_name_Hall           'C -2yc'
_space_group_name_H-M_alt        'C 1 c 1'
_symmetry_space_group_name_Hall  'C -2yc'
_symmetry_space_group_name_H-M   'C 1 c 1'
_atom_sites_solution_hydrogens   geom
_audit_creation_date             2016-07-02
_audit_creation_method
;
Olex2 1.2
(compiled 2016.02.19 svn.r3266 for OlexSys, GUI svn.r5155)
;
_audit_update_record
;
2018-02-05 deposited with the CCDC.
2018-06-26 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90.654(2)
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   14.8284(13)
_cell_length_b                   17.0000(15)
_cell_length_c                   14.5439(13)
_cell_measurement_reflns_used    9927
_cell_measurement_temperature    296(2)
_cell_measurement_theta_max      26.093
_cell_measurement_theta_min      2.396
_cell_volume                     3666.0(6)
_computing_cell_refinement       'SAINT v8.34A (Bruker, 2013)'
_computing_data_reduction        'SAINT v8.34A (Bruker, 2013)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'XL (Sheldrick, 2008)'
_diffrn_ambient_temperature      296.15
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0280
_diffrn_reflns_av_unetI/netI     0.0269
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -18
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            26127
_diffrn_reflns_point_group_measured_fraction_full 0.871
_diffrn_reflns_point_group_measured_fraction_max 0.867
_diffrn_reflns_theta_full        26.000
_diffrn_reflns_theta_max         26.099
_diffrn_reflns_theta_min         1.822
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    4.268
_exptl_absorpt_correction_T_max  0.7453
_exptl_absorpt_correction_T_min  0.6284
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2014/4 (Bruker,2014/4) was used for absorption correction.
wR2(int) was 0.0573 before and 0.0393 after correction.
The Ratio of minimum to maximum transmission is 0.8432.
The \l/2 correction factor is 0.00150.
;
_exptl_crystal_colour            orange
_exptl_crystal_colour_primary    orange
_exptl_crystal_density_diffrn    1.996
_exptl_crystal_description       Needle
_exptl_crystal_F_000             2104
_exptl_crystal_size_max          0.06
_exptl_crystal_size_mid          0.06
_exptl_crystal_size_min          0.02
_refine_diff_density_max         0.564
_refine_diff_density_min         -0.507
_refine_diff_density_rms         0.119
_refine_ls_abs_structure_details
;
 Flack x determined using 2530 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   0.020(10)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.136
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     302
_refine_ls_number_reflns         6304
_refine_ls_number_restraints     2
_refine_ls_restrained_S_all      1.136
_refine_ls_R_factor_all          0.0252
_refine_ls_R_factor_gt           0.0243
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0062P)^2^+35.6017P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0572
_refine_ls_wR_factor_ref         0.0575
_reflns_Friedel_coverage         0.736
_reflns_Friedel_fraction_full    0.742
_reflns_Friedel_fraction_max     0.736
_reflns_number_gt                6168
_reflns_number_total             6304
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c8dt00828k2.cif
_cod_data_source_block           mf1069
_cod_depositor_comments
'Adding full bibliography for 7046853--7046855.cif.'
_cod_original_formula_sum        'C14.50 H22 Fe I2 N P'
_cod_database_code               7046853
_shelxl_version_number           2014-3
_shelx_estimated_absorpt_t_max   0.919
_shelx_estimated_absorpt_t_min   0.784
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Uiso/Uaniso restraints and constraints
Uanis(C2) = Uanis(C1) = Uanis(C5) = Uanis(C4) = Uanis(C3)
Uanis(C16) = Uanis(C12) = Uanis(C13) = Uanis(C14) = Uanis(C15)
Uanis(C23) = Uanis(C24) = Uanis(C25) = Uanis(C26) = Uanis(C27) = Uanis(C28)
3. Others
 Sof(I3B)=Sof(I4B)=1-FVAR(1)
 Sof(I4)=Sof(I3)=FVAR(1)
4.a Ternary CH refined with riding coordinates:
 C6(H6), C17(H17), C9(H9), C20(H20)
4.b Aromatic/amide H refined with riding coordinates:
 C2(H2), C5(H5), C28(H28), C4(H4), C25(H25), C24(H24), C16(H16), C14(H14),
 C13(H13), C26(H26), C3(H3), C15(H15), C27(H27)
4.c Idealised Me refined as rotating group:
 C18(H18A,H18B,H18C), C29(H29A,H29B,H29C), C19(H19A,H19B,H19C), C7(H7A,H7B,
 H7C), C22(H22A,H22B,H22C), C8(H8A,H8B,H8C), C11(H11A,H11B,H11C), C21(H21A,H21B,
 H21C), C10(H10A,H10B,H10C)
;
_shelx_res_checksum              4247
_olex2_submission_special_instructions 'No special instructions were received'