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_7708679
_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         'C30 H47 Fe N2 P3 Si'
_chemical_formula_sum            'C30 H47 Fe N2 P3 Si'
_chemical_formula_weight         612.54
_space_group_crystal_system      tetragonal
_space_group_IT_number           61
_space_group_name_Hall           '-P 2ac 2ab'
_space_group_name_H-M_alt        'P b c a'
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     dual
_audit_creation_date             2019-04-12
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_audit_update_record
;
2019-04-12 deposited with the CCDC.	2021-11-02 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   16.2215(6)
_cell_length_b                   16.2215(6)
_cell_length_c                   24.4132(11)
_cell_measurement_reflns_used    14415
_cell_measurement_temperature    173.0(5)
_cell_measurement_theta_max      75.9780
_cell_measurement_theta_min      4.2040
_cell_volume                     6424.0(4)
_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    'ShelXT (Sheldrick, 2015)'
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      173.0(5)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 10.0000
_diffrn_detector_type            HyPix
_diffrn_measured_fraction_theta_full 0.982
_diffrn_measured_fraction_theta_max 0.998
_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     22.00  63.00   1.00    0.50    --   48.45 -55.00 106.00   41
  2  \w    -22.00  13.00   1.00    0.50    --   48.45 -55.00 106.00   35
  3  \w   -140.00 -96.00   1.00    5.00    --  -86.25 -96.00-120.00   44
  4  \w   -120.00 -82.00   1.00    0.50    --  -48.45-125.00  60.00   38
  5  \w     50.00 115.00   1.00    5.00    --  106.49 -30.00  90.00   65
  6  \w    111.00 172.00   1.00    5.00    --  106.49  45.00  60.00   61
  7  \w     84.00 176.00   1.00    5.00    --  106.49  76.00 101.00   92
  8  \w    -83.00 -29.00   1.00   10.00    --  -86.25  96.00 -11.00   54
  9  \w    -60.00  25.00   1.00    4.00    --  -48.45  37.00-120.00   85
 10  \w     32.00  96.00   1.00    4.00    --   48.45-125.00  90.00   64
 11  \w     37.00 116.00   1.00   10.00    --  106.49-125.00-120.00   79
 12  \w     35.00 126.00   1.00   10.00    --  106.49 -77.00  30.00   91
 13  \w     37.00 107.00   1.00   10.00    --  106.49 -94.00 -90.00   70
 14  \w    116.00 141.00   1.00   10.00    --  106.49  96.00 -11.00   25
 15  \w    116.00 141.00   1.00   10.00    --  106.49  96.00 -11.00   25
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'XtaLAB Synergy, Dualflex, HyPix'
_diffrn_measurement_method       '\w scans'
_diffrn_measurement_specimen_support 'Mitegen 50um'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      0.0627654000
_diffrn_orient_matrix_UB_12      -0.0355618000
_diffrn_orient_matrix_UB_13      -0.0412878000
_diffrn_orient_matrix_UB_21      -0.0020767000
_diffrn_orient_matrix_UB_22      0.0808943000
_diffrn_orient_matrix_UB_23      -0.0325721000
_diffrn_orient_matrix_UB_31      0.0718341000
_diffrn_orient_matrix_UB_32      0.0333352000
_diffrn_orient_matrix_UB_33      0.0349790000
_diffrn_radiation_collimation    0.3
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0851
_diffrn_reflns_av_unetI/netI     0.0484
_diffrn_reflns_Laue_measured_fraction_full 0.982
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_limit_h_max       19
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       29
_diffrn_reflns_limit_l_min       -28
_diffrn_reflns_number            35686
_diffrn_reflns_point_group_measured_fraction_full 0.982
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         67.068
_diffrn_reflns_theta_min         4.259
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_current           24.0
_diffrn_source_power             1.2
_diffrn_source_target            Mo
_diffrn_source_type              'PhotonJet (Cu) X-ray Source'
_diffrn_source_voltage           50.0
_exptl_absorpt_coefficient_mu    5.689
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.33637
_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 yellowish yellow'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   yellowish
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    1.267
_exptl_crystal_description       block
_exptl_crystal_F_000             2608
_refine_diff_density_max         2.097
_refine_diff_density_min         -0.798
_refine_diff_density_rms         0.091
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.087
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     378
_refine_ls_number_reflns         5715
_refine_ls_number_restraints     117
_refine_ls_restrained_S_all      1.085
_refine_ls_R_factor_all          0.0775
_refine_ls_R_factor_gt           0.0670
_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^)+(0.0870P)^2^+12.8045P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1705
_refine_ls_wR_factor_ref         0.1829
_reflns_Friedel_coverage         0.000
_reflns_number_gt                4969
_reflns_number_total             5715
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d1dt02832d2.cif
_cod_data_source_block           190410f
_cod_database_code               7708679
_shelxl_version_number           2013-4
_chemical_oxdiff_formula         FeSiPC
_reflns_odcompleteness_completeness 99.67
_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. Restrained distances
 H21A-H24C
 2.45 with sigma of 0.01
3. Rigid bond restraints
 All non-hydrogen atoms
 with sigma for 1-2 distances of 0.001 and sigma for 1-3 distances of 0.001
4. Others
 Sof(C1AA)=Sof(H1AA)=Sof(C2AA)=Sof(H2AA)=Sof(H2AB)=Sof(H2AC)=1-FVAR(1)
 Sof(C23)=Sof(H23)=Sof(C22)=Sof(H22A)=Sof(H22B)=Sof(H22C)=FVAR(1)
 Fixed Sof: C24(0.5) H24A(0.5) H24B(0.5) H24C(0.5) C0AA(0.5) H0AA(0.5)
 H0AB(0.5) H0AC(0.5)
5.a Ternary CH refined with riding coordinates:
 C19(H19), C23(H23), C1AA(H1AA)
5.b Aromatic/amide H refined with riding coordinates:
 C5(H5), C12(H12), C14(H14), C18(H18), C2(H2), C8(H8), C4(H4), C17(H17),
 C16(H16), C3(H3), C9(H9), C10(H10), C11(H11), C15(H15)
5.c Idealised Me refined as rotating group:
 C30(H30A,H30B,H30C), C26(H26A,H26B,H26C), C28(H28A,H28B,H28C), C29(H29A,H29B,
 H29C), C27(H27A,H27B,H27C), C25(H25A,H25B,H25C), C20(H20A,H20B,H20C), C24(H24A,
 H24B,H24C), C21(H21A,H21B,H21C), C22(H22A,H22B,H22C), C2AA(H2AA,H2AB,H2AC),
 C0AA(H0AA,H0AB,H0AC)
;
_shelx_res_checksum              90920
_shelx_hkl_checksum              30394
_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 2.605
_oxdiff_exptl_absorpt_empirical_full_min 0.586