Low coordinate iron derivatives stabilized by a β-diketiminate mimic. Synthesis and coordination chemistry of enamidophosphinimine scaffolds to generate diiron dinitrogen complexes.
Hein, Nicholas M.; Suzuki, Tatsuya; Ogawa, Takahiko; Fryzuk, Michael D.; Dalton transactions (Cambridge, England : 2003) 45 (2016) 14697–14708; doi:10.1039/c6dt01673a

data_7039402
_publ_section_title
;
 Low coordinate iron derivatives stabilized by a \b-diketiminate mimic.
 Synthesis and coordination chemistry of enamidophosphinimine scaffolds to
 generate diiron dinitrogen complexes.
;
_journal_issue                   37
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              14697
_journal_page_last               14708
_journal_paper_doi               10.1039/c6dt01673a
_journal_volume                  45
_journal_year                    2016
_chemical_formula_moiety         '0.5(C54 H76 Br2 Fe2 N4 P2)'
_chemical_formula_sum            'C27 H38 Br Fe N2 P'
_chemical_formula_weight         557.32
_chemical_properties_physical
Air-sensitive,Moisture-sensitive,Oxygen-sensitive
_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
_audit_creation_date             2015-11-13
_audit_creation_method
;
Olex2 1.2
(compiled 2015.09.30 svn.r3233 for OlexSys, GUI svn.r5103)
;
_audit_update_record
;
2016-04-22 deposited with the CCDC.
2016-06-01 downloaded from the CCDC.
;
_cell_angle_alpha                90.837(4)
_cell_angle_beta                 109.446(4)
_cell_angle_gamma                101.917(4)
_cell_formula_units_Z            4
_cell_length_a                   13.121(3)
_cell_length_b                   15.896(4)
_cell_length_c                   16.706(4)
_cell_measurement_reflns_used    6750
_cell_measurement_temperature    90(2)
_cell_measurement_theta_max      26.13
_cell_measurement_theta_min      2.33
_cell_volume                     3201.7(13)
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2008)'
_computing_structure_solution    'ShelXT (Sheldrick, 2015)'
_diffrn_ambient_temperature      90.0
_diffrn_detector                 'Bruker APEX2 area detector'
_diffrn_detector_area_resol_mean 7.9
_diffrn_detector_type            'Bruker-Nonius APEXII CCD area detector'
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.985
_diffrn_measurement_device
'Bruker-Nonius APEXII CCD area detector and D8 diffractometer'
_diffrn_measurement_device_type  'Bruker D8 diffractometer'
_diffrn_measurement_method       '\w and \f scans'
_diffrn_radiation_monochromator  'TRIUMPH curved-crystal'
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.1318
_diffrn_reflns_av_unetI/netI     0.1376
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.985
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            44303
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.985
_diffrn_reflns_theta_full        26.000
_diffrn_reflns_theta_max         26.518
_diffrn_reflns_theta_min         1.298
_diffrn_source                   'sealed X-ray tube'
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    1.783
_exptl_absorpt_correction_T_max  0.7454
_exptl_absorpt_correction_T_min  0.5555
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2014/5 (Bruker,2014/5) was used for absorption correction.
wR2(int) was 0.0817 before and 0.0632 after correction.
The Ratio of minimum to maximum transmission is 0.7452.
The \l/2 correction factor is 0.00150.
;
_exptl_crystal_colour            yellow
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    1.156
_exptl_crystal_description       block
_exptl_crystal_F_000             1160
_exptl_crystal_recrystallization_method 'Re-crystallisation from solvent'
_exptl_crystal_size_max          0.09
_exptl_crystal_size_mid          0.08
_exptl_crystal_size_min          0.04
_refine_diff_density_max         2.173
_refine_diff_density_min         -1.043
_refine_diff_density_rms         0.175
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.909
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     545
_refine_ls_number_reflns         13084
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.909
_refine_ls_R_factor_all          0.1452
_refine_ls_R_factor_gt           0.0827
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.1394P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2030
_refine_ls_wR_factor_ref         0.2298
_reflns_Friedel_coverage         0.000
_reflns_number_gt                6855
_reflns_number_total             13084
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c6dt01673a2.cif
_cod_data_source_block           mf1189
_cod_depositor_comments
;
The following automatic conversions were performed:

'_diffrn_radiation_probe' value 'X-ray' changed to 'x-ray' according
to
/usr/data/users/saulius/crontab/automatic-downloads/rss-feeds/RSC/lib/dictionaries/cif_core.dic
dictionary named 'cif_core.dic' version 2.4.2 from 2011-04-26.

Automatic conversion script
Id: cif_fix_values 4268 2015-11-12 08:31:59Z antanas 

 Adding full bibliography for 7039398--7039404.cif.
;
_cod_original_cell_volume        3201.6(14)
_cod_database_code               7039402
_shelx_estimated_absorpt_t_max   0.932
_shelx_estimated_absorpt_t_min   0.856
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Uiso/Uaniso restraints and constraints
Uanis(C29) = Uanis(C28) = Uanis(C32) = Uanis(C31) = Uanis(C30)
Uanis(C2) = Uanis(C3) = Uanis(C4) = Uanis(C5) = Uanis(C1)
3.a Ternary CH refined with riding coordinates:
 C41(H41), C44(H44), C14(H14), C17(H17)
3.b Secondary CH2 refined with riding coordinates:
 C5(H5A,H5B), C31(H31A,H31B), C4(H4A,H4B), C32(H32A,H32B), C30(H30A,H30B),
 C3(H3A,H3B)
3.c Aromatic/amide H refined with riding coordinates:
 C9(H9), C11(H11), C10(H10), C38(H38), C23(H23), C25(H25), C24(H24), C36(H36),
 C52(H52), C37(H37), C51(H51), C50(H50)
3.d Idealised Me refined as rotating group:
 C13(H13A,H13B,H13C), C46(H46A,H46C,H46B), C22(H22A,H22B,H22C), C45(H45A,H45B,
 H45C), C19(H19A,H19B,H19C), C42(H42A,H42B,H42C), C54(H54A,H54B,H54C), C40(H40A,
 H40B,H40C), C8(H8A,H8B,H8C), C018(H01A,H01C,H01B), C27(H27A,H27B,H27C),
 C16(H16A,H16B,H16C), C43(H43A,H43B,H43C), C35(H35A,H35B,H35C), C18(H18A,H18B,
 H18C), C49(H49A,H49B,H49C)
;
_shelx_res_checksum              95406
_shelx_shelxl_version_number     2014/7
_olex2_submission_special_instructions 'No special instructions were received'
_solvent_exptl_crystal_recrystallization_method n-pentane/toluene