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_7039403
_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         'C46 H67 Fe N3 P2'
_chemical_formula_sum            'C46 H67 Fe N3 P2'
_chemical_formula_weight         779.81
_chemical_properties_physical    Air-sensitive
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2yn'
_space_group_name_H-M_alt        'P 1 21/n 1'
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_audit_creation_date             2016-04-13
_audit_creation_method
;
Olex2 1.2
(compiled 2016.02.19 svn.r3266 for OlexSys, GUI svn.r5155)
;
_audit_update_record
;
2016-04-22 deposited with the CCDC.
2016-06-01 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 112.138(3)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   19.562(3)
_cell_length_b                   11.2091(14)
_cell_length_c                   20.674(3)
_cell_measurement_reflns_used    7061
_cell_measurement_temperature    90(2)
_cell_measurement_theta_max      27.55
_cell_measurement_theta_min      2.25
_cell_volume                     4199.0(10)
_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      90.0
_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 0.994
_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  0.1579
_diffrn_reflns_av_unetI/netI     0.1611
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.994
_diffrn_reflns_limit_h_max       24
_diffrn_reflns_limit_h_min       -25
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -10
_diffrn_reflns_limit_l_max       26
_diffrn_reflns_limit_l_min       -26
_diffrn_reflns_number            37081
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.994
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.579
_diffrn_reflns_theta_min         1.222
_diffrn_source                   'sealed X-ray tube'
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.471
_exptl_absorpt_correction_T_max  0.7456
_exptl_absorpt_correction_T_min  0.4114
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2014/5 (Bruker,2014/5) was used for absorption correction.
wR2(int) was 0.1270 before and 0.0844 after correction.
The Ratio of minimum to maximum transmission is 0.5518.
The \l/2 correction factor is 0.00150.
;
_exptl_crystal_colour            red
_exptl_crystal_colour_primary    red
_exptl_crystal_density_diffrn    1.234
_exptl_crystal_description       needle
_exptl_crystal_F_000             1680
_exptl_crystal_recrystallization_method 'Re-crystallisation from solvent'
_exptl_crystal_size_max          0.24
_exptl_crystal_size_mid          0.03
_exptl_crystal_size_min          0.025
_refine_diff_density_max         1.232
_refine_diff_density_min         -0.889
_refine_diff_density_rms         0.112
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.974
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     483
_refine_ls_number_reflns         9688
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.974
_refine_ls_R_factor_all          0.1598
_refine_ls_R_factor_gt           0.0807
_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^)+(0.1019P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1703
_refine_ls_wR_factor_ref         0.2062
_reflns_Friedel_coverage         0.000
_reflns_number_gt                5266
_reflns_number_total             9688
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c6dt01673a2.cif
_cod_data_source_block           mf1203
_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        4199.1(9)
_cod_database_code               7039403
_shelx_estimated_absorpt_t_max   0.988
_shelx_estimated_absorpt_t_min   0.895
_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:
 C14(H14), C17(H17), C44(H44), C41(H41)
2.b Secondary CH2 refined with riding coordinates:
 C3(H3a,H3b), C4(H4a,H4b), C5(H5a,H5b), C32(H32a,H32b), C31(H31a,H31b),
 C30(H30a,H30b)
2.c Aromatic/amide H refined with riding coordinates:
 C23(H23), C24(H24), C25(H25), C9(H9), C10(H10), C11(H11), C36(H36), C37(H37),
 C38(H38)
2.d Idealised Me refined as rotating group:
 C22(H22a,H22b,H22c), C27(H27a,H27b,H27c), C15(H15a,H15b,H15c), C16(H16a,H16b,
 H16c), C18(H18a,H18b,H18c), C19(H19a,H19b,H19c), C8(H8a,H8b,H8c), C13(H13a,
 H13b,H13c), C35(H35a,H35b,H35c), C40(H40a,H40b,H40c), C45(H45a,H45b,H45c),
 C46(H46a,H46b,H46c), C42(H42a,H42b,H42c), C43(H43a,H43b,H43c)
;
_shelx_res_checksum              52757
_shelx_shelxl_version_number     2014/7
_olex2_submission_special_instructions 'No special instructions were received'
_solvent_exptl_crystal_recrystallization_method n-pentane