Chalcogen-atom abstraction reactions of a Di-iron imidophosphorane complex.
Aguirre Quintana, Luis M.; Yang, Yan; Ramanathan, Arun; Jiang, Ningxin; Bacsa, John; Maron, Laurent; La Pierre, Henry S.; Chemical communications (Cambridge, England) 57 (2021) 6664–6667; doi:10.1039/d1cc02195h

data_7128455
_publ_section_title
;
 Chalcogen-atom abstraction reactions of a Di-iron imidophosphorane
 complex.
;
_journal_issue                   54
_journal_name_full
'Chemical communications (Cambridge, England)'
_journal_page_first              6664
_journal_page_last               6667
_journal_paper_doi               10.1039/d1cc02195h
_journal_volume                  57
_journal_year                    2021
_chemical_formula_moiety         'C60 H120 Fe2 N16 O P4'
_chemical_formula_sum            'C60 H120 Fe2 N16 O P4'
_chemical_formula_weight         1317.29
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_audit_creation_date             2021-02-23
_audit_creation_method
;
Olex2 1.3-alpha
(compiled 2020.11.12 svn.r5f609507 for OlexSys, GUI svn.r6272)
;
_audit_update_record
;
2021-04-14 deposited with the CCDC.	2021-06-07 downloaded from the CCDC.
;
_cell_angle_alpha                100.590(7)
_cell_angle_beta                 95.542(7)
_cell_angle_gamma                109.567(6)
_cell_formula_units_Z            2
_cell_length_a                   13.069(2)
_cell_length_b                   13.560(2)
_cell_length_c                   21.307(4)
_cell_measurement_reflns_used    9971
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      30.935
_cell_measurement_theta_min      2.671
_cell_volume                     3445.9(10)
_computing_cell_refinement       'SAINT V8.40A (Bruker, 2019)'
_computing_data_collection       'APEX2  v2016.5-1 (Bruker, 2014)'
_computing_data_reduction        'SAINT V8.40A (Bruker, 2019)'
_computing_molecular_graphics    'Olex2 1.3-alpha (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.3-alpha (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL-2014 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT (Sheldrick, 2015)'
_diffrn_ambient_temperature      100(2)
_diffrn_detector_area_resol_mean 7.495
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.996
_diffrn_measurement_device_type  'Bruker D8 VENTURE diffractometer'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_monochromator  'multilayer mirror'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0556
_diffrn_reflns_av_unetI/netI     0.0787
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.996
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       27
_diffrn_reflns_limit_l_min       -28
_diffrn_reflns_number            41434
_diffrn_reflns_point_group_measured_fraction_full 0.997
_diffrn_reflns_point_group_measured_fraction_max 0.996
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         28.281
_diffrn_reflns_theta_min         2.256
_diffrn_source                   'microfocus sealed tube'
_diffrn_source_current           1.4
_diffrn_source_power             0.07
_diffrn_source_voltage           50
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.565
_exptl_absorpt_correction_T_max  0.7462
_exptl_absorpt_correction_T_min  0.6726
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2016/2 (Bruker,2016/2) was used for absorption correction.
wR2(int) was 0.0744 before and 0.0627 after correction.
The Ratio of minimum to maximum transmission is 0.9014.
The \l/2 correction factor is Not present.
;
_exptl_crystal_colour            orange
_exptl_crystal_colour_primary    orange
_exptl_crystal_density_diffrn    1.270
_exptl_crystal_description       plate
_exptl_crystal_F_000             1424
_exptl_crystal_recrystallization_method
'The material was recrystallised from --- by as supplied'
_exptl_crystal_size_max          0.243
_exptl_crystal_size_mid          0.118
_exptl_crystal_size_min          0.117
_refine_diff_density_max         0.492
_refine_diff_density_min         -0.494
_refine_diff_density_rms         0.092
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.028
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     808
_refine_ls_number_reflns         17044
_refine_ls_number_restraints     7828
_refine_ls_restrained_S_all      0.874
_refine_ls_R_factor_all          0.0883
_refine_ls_R_factor_gt           0.0558
_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^)+(0.0161P)^2^+6.3078P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1039
_refine_ls_wR_factor_ref         0.1199
_reflns_Friedel_coverage         0.000
_reflns_number_gt                12478
_reflns_number_total             17044
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d1cc02195h2.cif
_cod_data_source_block           laq-2-095
_cod_depositor_comments
'Adding full bibliography for 7128454--7128458.cif.'
_cod_database_code               7128455
_shelx_shelxl_version_number     2018/3
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H,H) groups
2. Restrained distances
 C1_1-H1A_1 \\sim C1_1-H1B_1 \\sim C5_1-H5A_1 \\sim C5_1-H5B_1 \\sim C6_1-H6A_1
\\sim C6_1-H6B_1 ~
 C10_1-H10A_1 \\sim C10_1-H10B_1 \\sim C11_1-H11A_1 \\sim C11_1-H11B_1 \\sim
C15_1-H15A_1 ~
 C15_1-H15B_1 \\sim C2_1-H2A_1 \\sim C2_1-H2B_1 \\sim C4_1-H4A_1 \\sim
C4_1-H4B_1 \\sim C7_1-H7A_1
 \\sim C7_1-H7B_1 \\sim C9_1-H9A_1 \\sim C9_1-H9B_1 \\sim C12_1-H12A_1 \\sim
C12_1-H12B_1 \\sim C14_1-
 H14A_1 \\sim C14_1-H14B_1 \\sim C3_1-H3A_1 \\sim C3_1-H3B_1 \\sim C8_1-H8A_1
\\sim C8_1-H8B_1 ~
 C13_1-H13A_1 \\sim C13_1-H13B_1 \\sim C1_2-H1A_2 \\sim C1_2-H1B_2 \\sim
C5_2-H5A_2 \\sim C5_2-
 H5B_2 \\sim C6_2-H6A_2 \\sim C6_2-H6B_2 \\sim C10_2-H10A_2 \\sim C10_2-H10B_2
\\sim C11_2-H11A_2 ~
 C11_2-H11B_2 \\sim C15_2-H15A_2 \\sim C15_2-H15B_2 \\sim C2_2-H2A_2 \\sim
C2_2-H2B_2 \\sim C4_2-
 H4A_2 \\sim C4_2-H4B_2 \\sim C7_2-H7A_2 \\sim C7_2-H7B_2 \\sim C9_2-H9A_2
\\sim C9_2-H9B_2 \\sim C12_2-
 H12A_2 \\sim C12_2-H12B_2 \\sim C14_2-H14A_2 \\sim C14_2-H14B_2 \\sim
C3_2-H3A_2 \\sim C3_2-H3B_2
 \\sim C8_2-H8A_2 \\sim C8_2-H8B_2 \\sim C13_2-H13A_2 \\sim C13_2-H13B_2 \\sim
C16_3-H16A_3 \\sim C16_3-
 H16B_3 \\sim C20_3-H20A_3 \\sim C20_3-H20B_3 \\sim C21_3-H21A_3 \\sim
C21_3-H21B_3 \\sim C25_3-
 H25A_3 \\sim C25_3-H25B_3 \\sim C26_3-H26A_3 \\sim C26_3-H26B_3 \\sim
C30_3-H30A_3 \\sim C30_3-
 H30B_3 \\sim C17_3-H17A_3 \\sim C17_3-H17B_3 \\sim C19_3-H19A_3 \\sim
C19_3-H19B_3 \\sim C22_3-
 H22A_3 \\sim C22_3-H22B_3 \\sim C24_3-H24A_3 \\sim C24_3-H24B_3 \\sim
C27_3-H27A_3 \\sim C27_3-
 H27B_3 \\sim C29_3-H29A_3 \\sim C29_3-H29B_3 \\sim C18_3-H18A_3 \\sim
C18_3-H18B_3 \\sim C23_3-
 H23A_3 \\sim C23_3-H23B_3 \\sim C28_3-H28A_3 \\sim C28_3-H28B_3 \\sim
C16_4-H16A_4 \\sim C16_4-
 H16B_4 \\sim C20_4-H20A_4 \\sim C20_4-H20B_4 \\sim C21_4-H21A_4 \\sim
C21_4-H21B_4 \\sim C25_4-
 H25A_4 \\sim C25_4-H25B_4 \\sim C26_4-H26A_4 \\sim C26_4-H26B_4 \\sim
C30_4-H30A_4 \\sim C30_4-
 H30B_4 \\sim C17_4-H17A_4 \\sim C17_4-H17B_4 \\sim C19_4-H19A_4 \\sim
C19_4-H19B_4 \\sim C22_4-
 H22A_4 \\sim C22_4-H22B_4 \\sim C24_4-H24A_4 \\sim C24_4-H24B_4 \\sim
C27_4-H27A_4 \\sim C27_4-
 H27B_4 \\sim C29_4-H29A_4 \\sim C29_4-H29B_4 \\sim C18_4-H18A_4 \\sim
C18_4-H18B_4 \\sim C23_4-
 H23A_4 \\sim C23_4-H23B_4 \\sim C28_4-H28A_4 \\sim C28_4-H28B_4
 with sigma of 0.002
3. Rigid body (RIGU) restrains
 P1_1, N1_1, N2_1, N3_1, N4_1, C1_1, C2_1, C3_1, C4_1, C5_1, C6_1, C7_1, C8_1,
 C9_1, C10_1, C11_1, C12_1, C13_1, C14_1, C15_1
 P1_2, N1_2, N2_2, N3_2, N4_2, C1_2, C2_2, C3_2, C4_2, C5_2, C6_2, C7_2, C8_2,
 C9_2, C10_2, C11_2, C12_2, C13_2, C14_2, C15_2
 with sigma for 1-2 distances of 0.001 and sigma for 1-3 distances of 0.002
 P2_3, N5_3, N6_3, N7_3, N8_3, C16_3, C17_3, C18_3, C19_3, C20_3, C21_3, C22_3,
  C23_3, C24_3, C25_3, C26_3, C27_3, C28_3, C29_3, C30_3
 P2_4, N5_4, N6_4, N7_4, N8_4, C16_4, C17_4, C18_4, C19_4, C20_4, C21_4, C22_4,
  C23_4, C24_4, C25_4, C26_4, C27_4, C28_4, C29_4, C30_4
 with sigma for 1-2 distances of 0.001 and sigma for 1-3 distances of 0.002
 N6_3, C16_3, C20_3
 with sigma for 1-2 distances of 0.001 and sigma for 1-3 distances of 0.001
 N7_3, C21_3, C25_3
 with sigma for 1-2 distances of 0.001 and sigma for 1-3 distances of 0.001
 N8_3, C26_3, C30_3
 with sigma for 1-2 distances of 0.001 and sigma for 1-3 distances of 0.001
 N6_4, C16_4, C20_4
 with sigma for 1-2 distances of 0.001 and sigma for 1-3 distances of 0.001
 N7_4, C21_4, C25_4
 with sigma for 1-2 distances of 0.001 and sigma for 1-3 distances of 0.001
 N8_4, C26_4, C30_4
 with sigma for 1-2 distances of 0.001 and sigma for 1-3 distances of 0.001
4. Same fragment restrains
{P1_2, N1_2, N2_2, N3_2, N4_2, C1_2, C2_2, C3_2, C4_2, C5_2, C6_2, C7_2, C8_2,
C9_2, C10_2, C11_2, C12_2, C13_2, C14_2, C15_2}
as
{P1_1, N1_1, N2_1, N3_1, N4_1, C1_1, C2_1, C3_1, C4_1, C5_1, C6_1, C7_1, C8_1,
C9_1, C10_1, C11_1, C12_1, C13_1, C14_1, C15_1} sigma for 1-2: 0.002 1-3: 0.004
{P2_4, N5_4, N6_4, N7_4, N8_4, C16_4, C17_4, C18_4, C19_4, C20_4, C21_4, C22_4,
C23_4, C24_4, C25_4, C26_4, C27_4, C28_4, C29_4, C30_4}
as
{P2_3, N5_3, N6_3, N7_3, N8_3, C16_3, C17_3, C18_3, C19_3, C20_3, C21_3, C22_3,
C23_3, C24_3, C25_3, C26_3, C27_3, C28_3, C29_3, C30_3} sigma for 1-2: 0.002
1-3: 0.004
5.a Secondary CH2 refined with riding coordinates and stretchable bonds:
 C1(H1A,H1B), C2(H2A,H2B), C3(H3A,H3B), C4(H4A,H4B), C5(H5A,H5B), C6(H6A,H6B),
 C7(H7A,H7B), C8(H8A,H8B), C9(H9A,H9B), C10(H10A,H10B), C11(H11A,H11B),
 C12(H12A,H12B), C13(H13A,H13B), C14(H14A,H14B), C15(H15A,H15B), C1(H1A,H1B),
 C2(H2A,H2B), C3(H3A,H3B), C4(H4A,H4B), C5(H5A,H5B), C6(H6A,H6B), C7(H7A,H7B),
 C8(H8A,H8B), C9(H9A,H9B), C10(H10A,H10B), C11(H11A,H11B), C12(H12A,H12B),
 C13(H13A,H13B), C14(H14A,H14B), C15(H15A,H15B), C16(H16A,H16B), C17(H17A,H17B),
  C18(H18A,H18B), C19(H19A,H19B), C20(H20A,H20B), C21(H21A,H21B), C22(H22A,
 H22B), C23(H23A,H23B), C24(H24A,H24B), C25(H25A,H25B), C26(H26A,H26B),
 C27(H27A,H27B), C28(H28A,H28B), C29(H29A,H29B), C30(H30A,H30B), C16(H16A,H16B),
  C17(H17A,H17B), C18(H18A,H18B), C19(H19A,H19B), C20(H20A,H20B), C21(H21A,
 H21B), C22(H22A,H22B), C23(H23A,H23B), C24(H24A,H24B), C25(H25A,H25B),
 C26(H26A,H26B), C27(H27A,H27B), C28(H28A,H28B), C29(H29A,H29B), C30(H30A,H30B)
;
_shelx_res_checksum              6926
_shelx_hkl_checksum              14920
_olex2_diffrn_ambient_temperature_device 'Oxford Cryosystems'
_olex2_exptl_crystal_mounting_method
'The crystal was mounted on a loop with paratone'
_olex2_submission_special_instructions 'No special instructions were received'