Synthesis of Silyl Iron Dinitrogen Complexes for Activation of Dihydrogen and Catalytic Silylation of Dinitrogen
Chang, Guoliang; Zhang, Peng; Yang, Wenjing; Dong, Yanhong; Xie, Shangqing; Sun, Hongjian; Li, Xiaoyan; Fuhr, Olaf; Fenske, Dieter; Dalton Transactions  (2021) –; doi:10.1039/D1DT02832D

data_7708674
_publ_section_title
;
 Synthesis of Silyl Iron Dinitrogen Complexes for Activation of Dihydrogen
 and Catalytic Silylation of Dinitrogen
;
_journal_name_full               'Dalton Transactions'
_journal_paper_doi               10.1039/D1DT02832D
_journal_year                    2021
_chemical_formula_moiety         'C28 H51 Fe P3 Si'
_chemical_formula_sum            'C28 H51 Fe P3 Si'
_chemical_formula_weight         564.53
_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'
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     iterative
_audit_creation_date             2019-12-11
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_audit_update_record
;
2019-12-11 deposited with the CCDC.	2021-11-02 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 106.2564(19)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   13.3431(2)
_cell_length_b                   16.8555(3)
_cell_length_c                   14.1692(3)
_cell_measurement_reflns_used    7924
_cell_measurement_temperature    173.00(10)
_cell_measurement_theta_max      76.0610
_cell_measurement_theta_min      3.9840
_cell_volume                     3059.31(10)
_computing_cell_refinement       'CrysAlisPro 1.171.40.25a (Rigaku OD, 2018)'
_computing_data_collection       'CrysAlisPro 1.171.40.25a (Rigaku OD, 2018)'
_computing_data_reduction        'CrysAlisPro 1.171.40.25a (Rigaku OD, 2018)'
_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    'olex2.solve (Bourhis et al., 2015)'
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      173.00(10)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 10.0000
_diffrn_detector_type            HyPix
_diffrn_measured_fraction_theta_full 0.983
_diffrn_measured_fraction_theta_max 0.941
_diffrn_measurement_details
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  t~exp~   \w     \q     \k     \f   Frames
  1  \w   -121.00 -45.00   1.00    0.15    --  -48.45 -38.00 -52.00   76
  2  \w    -61.00 -36.00   1.00    0.15    --  -48.45  38.00 102.00   25
  3  \w     36.00  89.00   1.00    0.15    --   48.45  38.00 102.00   53
  4  \w     33.00  60.00   1.00    0.15    --   48.45 -38.00 -52.00   27
  5  \w   -106.00 -73.00   1.00    0.50    --  -86.25 -38.00 -52.00   33
  6  \w    -99.00 -74.00   1.00    0.50    --  -86.25  38.00 102.00   25
  7  \w     51.00 119.00   1.00    0.50    --  106.49 -38.00 -52.00   68
  8  \w     93.00 173.00   1.00    0.50    --  106.49  38.00 102.00   80
  9  \w    -20.00  12.00   1.00    0.15    --  -48.45  38.00 102.00   32
 10  \w     31.00  88.00   1.00    0.15    --   48.45-125.00 -30.00   57
 11  \w     39.00 113.00   1.00    0.50    --  106.49 -38.00 120.00   74
 12  \w     38.00 116.00   1.00    0.50    --  106.49 -19.00 150.00   78
 13  \w     38.00  97.00   1.00    0.50    --  106.49 -99.00 -30.00   59
 14  \w     34.00 109.00   1.00    0.50    --  106.49 -99.00 150.00   75
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'XtaLAB Synergy, Dualflex, HyPix'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      0.0138067000
_diffrn_orient_matrix_UB_12      0.0396300000
_diffrn_orient_matrix_UB_13      0.1008932000
_diffrn_orient_matrix_UB_21      -0.1176550000
_diffrn_orient_matrix_UB_22      0.0188393000
_diffrn_orient_matrix_UB_23      -0.0282743000
_diffrn_orient_matrix_UB_31      -0.0208954000
_diffrn_orient_matrix_UB_32      -0.0801694000
_diffrn_orient_matrix_UB_33      0.0429908000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0454
_diffrn_reflns_av_unetI/netI     0.0523
_diffrn_reflns_Laue_measured_fraction_full 0.983
_diffrn_reflns_Laue_measured_fraction_max 0.941
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       8
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_number            16325
_diffrn_reflns_point_group_measured_fraction_full 0.983
_diffrn_reflns_point_group_measured_fraction_max 0.941
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         76.323
_diffrn_reflns_theta_min         4.024
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'PhotonJet (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    5.905
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.70678
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.40.25a (Rigaku Oxford Diffraction, 2018)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            'clear light yellow'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   light
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    1.226
_exptl_crystal_description       block
_exptl_crystal_F_000             1216
_exptl_crystal_size_max          0.1
_exptl_crystal_size_mid          0.1
_exptl_crystal_size_min          0.1
_refine_diff_density_max         0.366
_refine_diff_density_min         -0.423
_refine_diff_density_rms         0.075
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.080
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     322
_refine_ls_number_reflns         6026
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.080
_refine_ls_R_factor_all          0.0537
_refine_ls_R_factor_gt           0.0375
_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^)+(0.0219P)^2^+2.9332P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0811
_refine_ls_wR_factor_ref         0.0910
_reflns_Friedel_coverage         0.000
_reflns_number_gt                5157
_reflns_number_total             6026
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d1dt02832d2.cif
_cod_data_source_block           191206h
_cod_database_code               7708674
_shelxl_version_number           2013-4
_chemical_oxdiff_formula         FeSiC
_shelx_estimated_absorpt_t_max   0.590
_shelx_estimated_absorpt_t_min   0.590
_reflns_odcompleteness_completeness 98.64
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     66.97
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2.a Ternary CH refined with riding coordinates:
 C10(H10), C7(H7), C23(H23), C20(H20)
2.b Aromatic/amide H refined with riding coordinates:
 C16(H16), C3(H3), C18(H18), C1(H1A), C6(H6), C15(H15), C2(H2), C17(H17)
2.c Idealised Me refined as rotating group:
 C8(H8A,H8B,H8C), C28(H28A,H28B,H28C), C12(H12A,H12B,H12C), C26(H26A,H26B,
 H26C), C24(H24A,H24B,H24C), C13(H13A,H13B,H13C), C25(H25A,H25B,H25C), C27(H27A,
 H27B,H27C), C9(H9A,H9B,H9C), C11(H11A,H11B,H11C), C21(H21A,H21B,H21C),
 C22(H22A,H22B,H22C)
;
_shelx_res_checksum              38806
_shelx_hkl_checksum              50782
_olex2_submission_special_instructions 'No special instructions were received'
_oxdiff_exptl_absorpt_empirical_details
;
Empirical correction (ABSPACK) includes:
- Absorption correction using spherical harmonics
- Frame scaling
;
_oxdiff_exptl_absorpt_empirical_full_max 1.658
_oxdiff_exptl_absorpt_empirical_full_min 0.719