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_7708676
_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         'C33 H53 Fe P3 Si'
_chemical_formula_sum            'C33 H53 Fe P3 Si'
_chemical_formula_weight         626.60
_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   mixed
_atom_sites_solution_primary     iterative
_audit_creation_date             2019-12-13
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_audit_update_record
;
2019-12-18 deposited with the CCDC.	2021-11-02 downloaded from the CCDC.
;
_cell_angle_alpha                69.372(3)
_cell_angle_beta                 87.284(3)
_cell_angle_gamma                74.966(3)
_cell_formula_units_Z            4
_cell_length_a                   11.0515(4)
_cell_length_b                   17.3189(6)
_cell_length_c                   19.6938(6)
_cell_measurement_reflns_used    12748
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      76.1660
_cell_measurement_theta_min      2.9660
_cell_volume                     3402.9(2)
_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      293(2)
_diffrn_detector                 'CCD plate'
_diffrn_detector_type            HyPix
_diffrn_measured_fraction_theta_full 0.982
_diffrn_measured_fraction_theta_max 0.924
_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    -96.00 -53.00   1.00    0.18    --  -48.45-154.00 177.00   43
  2  \w   -109.00 -73.00   1.00    0.18    --  -48.45 154.00-143.00   36
  3  \w   -107.00 -78.00   1.00    0.18    --  -48.45-120.00 -24.00   29
  4  \w    -85.00 -22.00   1.00    0.18    --  -48.45 120.00  59.00   63
  5  \w     58.00  83.00   1.00    0.18    --   48.45-154.00 177.00   25
  6  \w     29.00  63.00   1.00    0.18    --   48.45-120.00 -24.00   34
  7  \w     82.00 108.00   1.00    0.18    --   48.45 154.00-143.00   26
  8  \w   -120.00 -26.00   1.00    0.18    --  -48.45 -77.00-120.00   94
  9  \w   -121.00 -36.00   1.00    0.18    --  -48.45 -38.00 -60.00   85
 10  \w   -141.00-116.00   1.00    0.60    --  -86.25-120.00 -24.00   25
 11  \w    -81.00 -55.00   1.00    0.60    --  -86.25 120.00  59.00   26
 12  \w   -151.00 -50.00   1.00    0.60    --  -86.25-154.00 177.00  101
 13  \w   -153.00 -73.00   1.00    0.60    --  -86.25 -38.00-150.00   80
 14  \w    -90.00 -65.00   1.00    0.60    --  -86.25 154.00-143.00   25
 15  \w   -159.00 -74.00   1.00    0.60    --  -86.25 -38.00 -30.00   85
 16  \w     73.00 102.00   1.00    0.60    --  106.49 154.00-143.00   29
 17  \w     93.00 136.00   1.00    0.60    --  106.49-154.00 177.00   43
 18  \w     62.00 112.00   1.00    0.60    --  106.49-120.00 -24.00   50
 19  \w     96.00 163.00   1.00    0.60    --  106.49 120.00  59.00   67
 20  \w     50.00  84.00   1.00    0.60    --  106.49-154.00 177.00   34
 21  \w     36.00 120.00   1.00    0.60    --  106.49 -57.00 -30.00   84
 22  \w     41.00 129.00   1.00    0.60    --  106.49 -77.00 120.00   88
 23  \w     92.00 176.00   1.00    0.60    --  106.49  57.00 -30.00   84
 24  \w     34.00 117.00   1.00    0.60    --  106.49-125.00  90.00   83
 25  \w     93.00 178.00   1.00    0.60    --  106.49  38.00-150.00   85
 26  \w     34.00 121.00   1.00    0.60    --  106.49 -57.00 120.00   87
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      -0.0365271000
_diffrn_orient_matrix_UB_12      0.0164773000
_diffrn_orient_matrix_UB_13      -0.0793685000
_diffrn_orient_matrix_UB_21      0.1212419000
_diffrn_orient_matrix_UB_22      0.0278893000
_diffrn_orient_matrix_UB_23      -0.0246636000
_diffrn_orient_matrix_UB_31      0.0696379000
_diffrn_orient_matrix_UB_32      -0.0929374000
_diffrn_orient_matrix_UB_33      0.0097618000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0688
_diffrn_reflns_av_unetI/netI     0.0732
_diffrn_reflns_Laue_measured_fraction_full 0.982
_diffrn_reflns_Laue_measured_fraction_max 0.924
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_k_min       -21
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_number            37796
_diffrn_reflns_point_group_measured_fraction_full 0.982
_diffrn_reflns_point_group_measured_fraction_max 0.924
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         76.605
_diffrn_reflns_theta_min         2.993
_diffrn_source_type              'PhotonJet (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    5.361
_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    1.223
_exptl_crystal_description       block
_exptl_crystal_F_000             1344
_exptl_crystal_size_max          0.1
_exptl_crystal_size_mid          0.1
_exptl_crystal_size_min          0.1
_refine_diff_density_max         0.883
_refine_diff_density_min         -0.489
_refine_diff_density_rms         0.083
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.052
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     731
_refine_ls_number_reflns         13221
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.052
_refine_ls_R_factor_all          0.0675
_refine_ls_R_factor_gt           0.0500
_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^)+(0.0251P)^2^+6.2023P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1106
_refine_ls_wR_factor_ref         0.1273
_reflns_Friedel_coverage         0.000
_reflns_number_gt                10874
_reflns_number_total             13221
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d1dt02832d2.cif
_cod_data_source_block           191212k
_cod_depositor_comments
;

2024-09-23
Z value and formula fixed to values more according to usual
chemical conventions.                 miguel
;
_cod_original_formula_sum            'C66 H106 Fe2 P6 Si2'
_cod_original_formula_weight         1253.20
_cod_original_formula_moiety         '2(C33 H53 Fe P3 Si)'
_cod_original_formula_units_Z            2
_cod_database_code               7708676
_shelxl_version_number           2013-4
_chemical_oxdiff_formula         FeSiPC
_reflns_odcompleteness_completeness 98.61
_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:
 C20(H20), C1B(H1B), C4B(H4B), C26(H26), C3DA(H3DA), C9AA(H9AA), C29(H29),
 C23(H23)
2.b Aromatic/amide H refined with riding coordinates:
 C8(H8), C8DA(H8DA), C18(H18), C17(H17), C5DA(H5DA), C4DA(H4DA), C11(H11),
 C14(H14), C1(H1A), C9(H9), C7EA(H7EA), C10(H10), C4CA(H4CA), C4(H4),
 C1DA(H1DA), C0EA(H0EA), C8CA(H8CA), C9CA(H9CA), C16(H16), C15(H15), C1EA(H1EA),
  C6DA(H6DA), C2BA(H2BD), C3EA(H3EA), C3(H3), C2(H2A)
2.c Idealised Me refined as rotating group:
 C2B(H2BA,H2BB,H2BC), C22(H22A,H22B,H22C), C9DA(H9DA,H9DB,H9DC), C25(H25A,H25B,
 H25C), C19(H19A,H19B,H19C), C7CA(H7CA,H7CB,H7CC), C8BA(H8BA,H8BB,H8BC),
 C21(H21A,H21B,H21C), C27(H27A,H27B,H27C), C0BA(H0BA,H0BB,H0BC), C1BA(H1BA,H1BB,
 H1BC), C32(H32A,H32B,H32C), C0A(H0AA,H0AB,H0AC), C1A(H1AA,H1AB,H1AC), C2A(H2AA,
 H2AB,H2AC), C3A(H3AA,H3AB,H3AC), C24(H24A,H24B,H24C), C31(H31A,H31B,H31C),
 C6A(H6AA,H6AB,H6AC), C33(H33A,H33B,H33C), C28(H28A,H28B,H28C), C30(H30A,H30B,
 H30C)
;
_shelx_res_checksum              11132
_shelx_hkl_checksum              30177
_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 2.324
_oxdiff_exptl_absorpt_empirical_full_min 0.546