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_7039401
_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         'C70 H108 Fe2 N6 P2'
_chemical_formula_sum            'C70 H108 Fe2 N6 P2'
_chemical_formula_weight         1207.26
_chemical_properties_physical
Air-sensitive,Moisture-sensitive,Oxygen-sensitive
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2ybc'
_space_group_name_H-M_alt        'P 1 21/c 1'
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_audit_creation_date             2015-05-20
_audit_creation_method
;
Olex2 1.2
(compiled 2015.01.26 svn.r3150 for OlexSys, GUI svn.r4998)
;
_audit_update_record
;
2016-04-22 deposited with the CCDC.
2016-06-01 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 100.9200(10)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   10.3990(6)
_cell_length_b                   28.6698(15)
_cell_length_c                   22.9617(13)
_cell_measurement_reflns_used    9906
_cell_measurement_temperature    90(2)
_cell_measurement_theta_max      27.47
_cell_measurement_theta_min      2.30
_cell_volume                     6721.8(6)
_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 0.997
_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  0.0760
_diffrn_reflns_av_unetI/netI     0.0902
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.997
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_k_min       -37
_diffrn_reflns_limit_l_max       29
_diffrn_reflns_limit_l_min       -24
_diffrn_reflns_number            62062
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.997
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.555
_diffrn_reflns_theta_min         1.149
_diffrn_source                   'sealed X-ray tube'
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.523
_exptl_absorpt_correction_T_max  0.7456
_exptl_absorpt_correction_T_min  0.6741
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2014/5 (Bruker,2014/5) was used for absorption correction.
wR2(int) was 0.0568 before and 0.0523 after correction.
The Ratio of minimum to maximum transmission is 0.9041.
The \l/2 correction factor is 0.00150.
;
_exptl_crystal_colour            bronze
_exptl_crystal_density_diffrn    1.193
_exptl_crystal_description       plate
_exptl_crystal_F_000             2608
_exptl_crystal_recrystallization_method 'Re-crystallisation from solvent'
_exptl_crystal_size_max          0.1
_exptl_crystal_size_mid          0.08
_exptl_crystal_size_min          0.03
_refine_diff_density_max         0.479
_refine_diff_density_min         -0.387
_refine_diff_density_rms         0.074
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.001
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     745
_refine_ls_number_reflns         15498
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.001
_refine_ls_R_factor_all          0.0986
_refine_ls_R_factor_gt           0.0479
_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^)+(0.0327P)^2^+2.0843P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0833
_refine_ls_wR_factor_ref         0.0965
_reflns_Friedel_coverage         0.000
_reflns_number_gt                9980
_reflns_number_total             15498
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c6dt01673a2.cif
_cod_data_source_block           mf1148
_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_database_code               7039401
_shelx_estimated_absorpt_t_max   0.984
_shelx_estimated_absorpt_t_min   0.950
_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.a Ternary CH refined with riding coordinates:
 C33(H33), C26(H26), C18(H18), C21(H21), C8(H8), C15(H15), C61(H61), C68(H68),
 C53(H53), C56(H56), C43(H43), C50(H50)
2.b Secondary CH2 refined with riding coordinates:
 C3(H3A,H3B), C4(H4A,H4B), C5(H5A,H5B), C38(H38A,H38B), C39(H39A,H39B),
 C40(H40A,H40B)
2.c Aromatic/amide H refined with riding coordinates:
 C31(H31), C30(H30), C29(H29), C11(H11), C12(H12), C13(H13), C64(H64),
 C65(H65), C66(H66), C46(H46), C47(H47), C48(H48)
2.d Idealised Me refined as rotating group:
 C35(H35A,H35B,H35C), C34(H34A,H34B,H34C), C27(H27A,H27B,H27C), C28(H28A,H28B,
 H28C), C20(H20A,H20B,H20C), C19(H19A,H19B,H19C), C23(H23A,H23B,H23C), C22(H22A,
 H22B,H22C), C9(H9A,H9B,H9C), C10(H10A,H10B,H10C), C16(H16A,H16B,H16C),
 C17(H17A,H17B,H17C), C62(H62A,H62B,H62C), C63(H63A,H63B,H63C), C69(H69A,H69B,
 H69C), C70(H70A,H70B,H70C), C54(H54A,H54B,H54C), C55(H55A,H55B,H55C), C57(H57A,
 H57B,H57C), C58(H58A,H58B,H58C), C44(H44A,H44B,H44C), C45(H45A,H45B,H45C),
 C52(H52A,H52B,H52C), C51(H51A,H51B,H51C)
;
_shelx_res_checksum              52002
_shelx_shelxl_version_number     2014/7
_olex2_submission_special_instructions 'No special instructions were received'
_solvent_exptl_crystal_recrystallization_method n-pentane