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_7039404
_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         'C35.5 H55.5 Fe N2 P'
_chemical_formula_sum            'C35.5 H55.5 Fe N2 P'
_chemical_formula_weight         597.14
_chemical_properties_physical
Air-sensitive,Moisture-sensitive,Oxygen-sensitive
_space_group_crystal_system      monoclinic
_space_group_IT_number           15
_space_group_name_Hall           '-C 2yc'
_space_group_name_H-M_alt        'C 1 2/c 1'
_symmetry_space_group_name_Hall  '-C 2yc'
_symmetry_space_group_name_H-M   'C 1 2/c 1'
_atom_sites_solution_hydrogens   mixed
_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
_cell_angle_beta                 106.786(3)
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   26.340(3)
_cell_length_b                   11.8226(16)
_cell_length_c                   24.864(3)
_cell_measurement_reflns_used    9770
_cell_measurement_temperature    90
_cell_measurement_theta_max      27.54
_cell_measurement_theta_min      2.40
_cell_volume                     7412.9(16)
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_computing_structure_solution    'ShelXT (Sheldrick, 2015)'
_diffrn_ambient_temperature      90.15
_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 0.990
_diffrn_measured_fraction_theta_max 0.990
_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  0.0389
_diffrn_reflns_av_unetI/netI     0.0248
_diffrn_reflns_Laue_measured_fraction_full 0.990
_diffrn_reflns_Laue_measured_fraction_max 0.990
_diffrn_reflns_limit_h_max       21
_diffrn_reflns_limit_h_min       -31
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       29
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_number            51121
_diffrn_reflns_point_group_measured_fraction_full 0.990
_diffrn_reflns_point_group_measured_fraction_max 0.990
_diffrn_reflns_theta_full        25.180
_diffrn_reflns_theta_max         25.180
_diffrn_reflns_theta_min         1.615
_diffrn_source                   'sealed X-ray tube'
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.473
_exptl_absorpt_correction_T_max  0.7456
_exptl_absorpt_correction_T_min  0.6239
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2014/5 (Bruker,2014/5) was used for absorption correction.
wR2(int) was 0.0733 before and 0.0593 after correction.
The Ratio of minimum to maximum transmission is 0.8368.
The \l/2 correction factor is 0.00150.
;
_exptl_crystal_colour            red
_exptl_crystal_colour_primary    red
_exptl_crystal_density_diffrn    1.070
_exptl_crystal_description       block
_exptl_crystal_F_000             2588
_exptl_crystal_recrystallization_method 'Re-crystallisation from solvent'
_exptl_crystal_size_max          0.52
_exptl_crystal_size_mid          0.45
_exptl_crystal_size_min          0.41
_refine_diff_density_max         0.670
_refine_diff_density_min         -1.768
_refine_diff_density_rms         0.120
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.066
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     682
_refine_ls_number_reflns         6599
_refine_ls_number_restraints     651
_refine_ls_restrained_S_all      1.025
_refine_ls_R_factor_all          0.1488
_refine_ls_R_factor_gt           0.1319
_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^)+(0.1156P)^2^+146.4393P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.3467
_refine_ls_wR_factor_ref         0.3535
_reflns_Friedel_coverage         0.000
_reflns_number_gt                5191
_reflns_number_total             6599
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c6dt01673a2.cif
_cod_data_source_block           mf1134_a
_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        7413.1(17)
_cod_original_formula_sum        'C35.50 H55.50 Fe N2 P'
_cod_database_code               7039404
_shelx_estimated_absorpt_t_max   0.830
_shelx_estimated_absorpt_t_min   0.791
_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(C1) = Uanis(C36)
Uanis(N1) = Uanis(N3)
3. Rigid body (RIGU) restrains
 All non-hydrogen atoms
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
4. Others
 Fixed Sof: Fe1(0.5) P1(0.5) N2(0.5) N1(0.5) N3(0.5) N4(0.5) C68(0.5) H68(0.5)
 C35(0.5) H35A(0.5) H35B(0.5) H35C(0.5) C6(0.5) C7(0.5) C11(0.5) H11(0.5)
 C12(0.5) H12(0.5) C13(0.5) H13(0.5) C14(0.5) C43(0.5) H43(0.5) C44(0.5)
 H44A(0.5) H44B(0.5) H44C(0.5) C9(0.5) H9A(0.5) H9B(0.5) H9C(0.5) C15(0.5)
 H15(0.5) C17(0.5) H17A(0.5) H17B(0.5) H17C(0.5) C61(0.5) H61(0.5) C1(0.5)
 C36(0.5) C5(0.5) H5A(0.5) H5B(0.5) C39(0.5) H39A(0.5) H39B(0.5) C38(0.5)
 H38A(0.5) H38B(0.5) C63(0.5) H63A(0.5) H63B(0.5) H63C(0.5) C2(0.5) C21(0.5)
 H21(0.5) C23(0.5) H23A(0.5) H23B(0.5) H23C(0.5) C22(0.5) H22A(0.5) H22B(0.5)
 H22C(0.5) C18(0.5) H18(0.5) C19(0.5) H19A(0.5) H19B(0.5) H19C(0.5) C20(0.5)
 H20A(0.5) H20B(0.5) H20C(0.5) C24(0.5) C32(0.5) C31(0.5) H31(0.5) C30(0.5)
 H30(0.5) C29(0.5) H29(0.5) C25(0.5) C33(0.5) H33(0.5) C70(0.5) H70A(0.5)
 H70B(0.5) H70C(0.5) C69(0.5) H69A(0.5) H69B(0.5) H69C(0.5) C26(0.5) H26(0.5)
 C28(0.5) H28A(0.5) H28B(0.5) H28C(0.5) C27(0.5) H27A(0.5) H27B(0.5) H27C(0.5)
 C59(0.5) C67(0.5) C66(0.5) H66(0.5) C65(0.5) H65(0.5) C64(0.5) H64(0.5)
 C60(0.5) Fe2(0.5) P2(0.5) C37(0.5) C46(0.5) H46(0.5) C52(0.5) H52A(0.5)
 H52B(0.5) H52C(0.5) C49(0.5) C51(0.5) H51A(0.5) H51B(0.5) H51C(0.5) C8(0.5)
 H8(0.5) C41(0.5) C42(0.5) C48(0.5) H48(0.5) C50(0.5) H50(0.5) C53(0.5)
 H53(0.5) C54(0.5) H54A(0.5) H54B(0.5) H54C(0.5) C55(0.5) H55A(0.5) H55B(0.5)
 H55C(0.5) C45(0.5) H45A(0.5) H45B(0.5) H45C(0.5) C10(0.5) H10A(0.5) H10B(0.5)
 H10C(0.5) C3(0.5) H3A(0.5) H3B(0.5) C40(0.5) H40A(0.5) H40B(0.5) C4(0.5)
 H4A(0.5) H4B(0.5) C58(0.5) H58A(0.5) H58B(0.5) H58C(0.5) C56(0.5) H56(0.5)
 C57(0.5) H57A(0.5) H57B(0.5) H57C(0.5) C34(0.5) H34A(0.5) H34B(0.5) H34C(0.5)
 C47(0.5) H47(0.5) C62(0.5) H62A(0.5) H62B(0.5) H62C(0.5)
5.a Ternary CH refined with riding coordinates:
 C68(H68), C43(H43), C15(H15), C21(H21), C18(H18), C33(H33), C26(H26), C8(H8),
 C50(H50), C53(H53), C56(H56)
5.b Secondary CH2 refined with riding coordinates:
 C5(H5A,H5B), C39(H39A,H39B), C38(H38A,H38B), C3(H3A,H3B), C40(H40A,H40B),
 C4(H4A,H4B)
5.c Aromatic/amide H refined with riding coordinates:
 C11(H11), C12(H12), C13(H13), C31(H31), C30(H30), C29(H29), C66(H66),
 C65(H65), C64(H64), C46(H46), C48(H48), C47(H47)
5.d Fitted hexagon refined as free rotating group:
 C6(C7,C11,C12,C13,C14), C24(C32,C31,C30,C29,C25), C59(C67,C66,C65,C64,C60)
5.e Idealised Me refined as rotating group:
 C35(H35A,H35B,H35C), C44(H44A,H44B,H44C), C9(H9A,H9B,H9C), C17(H17A,H17B,
 H17C), C63(H63A,H63B,H63C), C23(H23A,H23B,H23C), C22(H22A,H22B,H22C), C19(H19A,
 H19B,H19C), C20(H20A,H20B,H20C), C70(H70A,H70B,H70C), C69(H69A,H69B,H69C),
 C28(H28A,H28B,H28C), C27(H27A,H27B,H27C), C52(H52A,H52B,H52C), C51(H51A,H51B,
 H51C), C54(H54A,H54B,H54C), C55(H55A,H55B,H55C), C45(H45A,H45B,H45C), C10(H10A,
 H10B,H10C), C58(H58A,H58B,H58C), C57(H57A,H57B,H57C), C34(H34A,H34B,H34C),
 C62(H62A,H62B,H62C), C16(H16A,H16B,H16C)
;
_shelx_res_checksum              25252
_shelx_shelxl_version_number     2014/7
_olex2_submission_special_instructions 'No special instructions were received'
_solvent_exptl_crystal_recrystallization_method n-pentane