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_7708673
_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 H51 Fe N2 P3 Si'
_chemical_formula_sum            'C33 H51 Fe N2 P3 Si'
_chemical_formula_weight         652.60
_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             2019-05-27
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_audit_update_record
;
2019-05-27 deposited with the CCDC.	2021-11-02 downloaded from the CCDC.
;
_cell_angle_alpha                96.856(2)
_cell_angle_beta                 91.687(2)
_cell_angle_gamma                116.430(2)
_cell_formula_units_Z            4
_cell_length_a                   9.9876(3)
_cell_length_b                   10.4113(3)
_cell_length_c                   36.5579(6)
_cell_measurement_reflns_used    14779
_cell_measurement_temperature    172.99(10)
_cell_measurement_theta_max      76.0050
_cell_measurement_theta_min      4.7240
_cell_volume                     3365.15(16)
_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      172.99(10)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 10.0000
_diffrn_detector_type            HyPix
_diffrn_measured_fraction_theta_full 0.981
_diffrn_measured_fraction_theta_max 0.923
_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    -83.00 -55.00   1.00    0.10    --  -48.45 106.00  85.00   28
  2  \w     16.00  71.00   1.00    0.10    --   48.45-106.00 -13.00   55
  3  \w    -85.00 -13.00   1.00    0.45    --  -86.25 106.00  85.00   72
  4  \w   -136.00 -80.00   1.00    0.45    --  -86.25-106.00 -13.00   56
  5  \w    102.00 160.00   1.00    0.45    --  106.49 106.00  85.00   58
  6  \w     39.00 111.00   1.00    0.45    --  106.49-106.00 -13.00   72
  7  \w    -47.00   1.00   1.00    0.10    --  -48.45 106.00  85.00   48
  8  \w    -60.00  23.00   1.00    0.10    --  -48.45  38.00 120.00   83
  9  \w   -120.00 -74.00   1.00    0.10    --  -48.45-125.00 120.00   46
 10  \w    -60.00  27.00   1.00    0.10    --  -48.45  19.00  30.00   87
 11  \w   -156.00 -71.00   1.00    0.45    --  -86.25 -57.00   0.00   85
 12  \w   -158.00 -83.00   1.00    0.45    --  -86.25 -99.00  90.00   75
 13  \w     93.00 168.00   1.00    0.45    --  106.49 125.00  30.00   75
 14  \w     93.00 178.00   1.00    0.45    --  106.49  38.00-180.00   85
 15  \w     34.00 117.00   1.00    0.45    --  106.49-125.00 -30.00   83
 16  \w     34.00 120.00   1.00    0.45    --  106.49 -38.00 -30.00   86
 17  \w     37.00 115.00   1.00    0.45    --  106.49-125.00-150.00   78
 18  \w     35.00 117.00   1.00    0.45    --  106.49-125.00 150.00   82
 19  \w     35.00  88.00   1.00    0.45    --  106.49 -99.00-150.00   53
;
_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      0.1103119000
_diffrn_orient_matrix_UB_12      0.0240163000
_diffrn_orient_matrix_UB_13      0.0334397000
_diffrn_orient_matrix_UB_21      -0.1321602000
_diffrn_orient_matrix_UB_22      -0.0587899000
_diffrn_orient_matrix_UB_23      0.0241292000
_diffrn_orient_matrix_UB_31      -0.0171310000
_diffrn_orient_matrix_UB_32      -0.1545431000
_diffrn_orient_matrix_UB_33      -0.0108039000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0426
_diffrn_reflns_av_unetI/netI     0.0492
_diffrn_reflns_Laue_measured_fraction_full 0.981
_diffrn_reflns_Laue_measured_fraction_max 0.923
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       44
_diffrn_reflns_limit_l_min       -43
_diffrn_reflns_number            32434
_diffrn_reflns_point_group_measured_fraction_full 0.981
_diffrn_reflns_point_group_measured_fraction_max 0.923
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         76.525
_diffrn_reflns_theta_min         3.669
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'PhotonJet (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    5.463
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.67768
_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    1.288
_exptl_crystal_description       block
_exptl_crystal_F_000             1392
_refine_diff_density_max         0.435
_refine_diff_density_min         -0.384
_refine_diff_density_rms         0.072
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.073
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     751
_refine_ls_number_reflns         13063
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.073
_refine_ls_R_factor_all          0.0552
_refine_ls_R_factor_gt           0.0410
_refine_ls_shift/su_max          0.003
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0191P)^2^+4.8982P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0897
_refine_ls_wR_factor_ref         0.1003
_reflns_Friedel_coverage         0.000
_reflns_number_gt                11313
_reflns_number_total             13063
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d1dt02832d2.cif
_cod_data_source_block           190524f
_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 H102 Fe2 N4 P6 Si2'
_cod_original_formula_weight         1305.21
_cod_original_formula_moiety         '2(C33 H51 Fe N2 P3 Si)'
_cod_original_formula_units_Z            2
_cod_database_code               7708673
_shelxl_version_number           2013-4
_chemical_oxdiff_formula         FeSiPC
_reflns_odcompleteness_completeness 98.73
_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:
 C63(H63), C65(H65), C25(H25), C28(H28), C56(H56), C19(H19), C58(H58), C22(H22)
2.b Aromatic/amide H refined with riding coordinates:
 C15(H15), C8(H8), C44(H44), C17(H17), C6(H6), C37(H37), C40(H40), C38(H38),
 C2(H2), C48(H48), C14(H14), C47(H47), C16(H16), C11(H11), C51(H51), C53(H53),
 C46(H46), C54(H54), C52(H52), C5(H5), C9(H9), C45(H45), C10(H10), C39(H39),
 C3(H3), C4(H4)
2.c Idealised Me refined as rotating group:
 C31(H31A,H31B,H31C), C30(H30A,H30B,H30C), C29(H29A,H29B,H29C), C67(H67A,H67B,
 H67C), C68(H68A,H68B,H68C), C32(H32A,H32B,H32C), C60(H60A,H60B,H60C), C64(H64A,
 H64B,H64C), C21(H21A,H21B,H21C), C73(H73A,H73B,H73C), C26(H26A,H26B,H26C),
 C33(H33A,H33B,H33C), C66(H66A,H66B,H66C), C27(H27A,H27B,H27C), C75(H75A,H75B,
 H75C), C76(H76A,H76B,H76C), C61(H61A,H61B,H61C), C59(H59A,H59B,H59C), C57(H57A,
 H57B,H57C), C23(H23A,H23B,H23C), C24(H24A,H24B,H24C), C20(H20A,H20B,H20C)
;
_shelx_res_checksum              34871
_shelx_hkl_checksum              9250
_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 1.436
_oxdiff_exptl_absorpt_empirical_full_min 0.779