#------------------------------------------------------------------------------
#$Date: 2021-11-03 02:00:04 +0200 (Wed, 03 Nov 2021) $
#$Revision: 270219 $
#$URL: file:///home/coder/svn-repositories/cod/cif/7/70/86/7708678.cif $
#------------------------------------------------------------------------------
#
# This file is available in the Crystallography Open Database (COD),
# http://www.crystallography.net/
#
# All data on this site have been placed in the public domain by the
# contributors.
#
data_7708678
loop_
_publ_author_name
'Chang, Guoliang'
'Zhang, Peng'
'Yang, Wenjing'
'Dong, Yanhong'
'Xie, Shangqing'
'Sun, Hongjian'
'Li, Xiaoyan'
'Fuhr, Olaf'
'Fenske, Dieter'
_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 P3 Si'
_chemical_formula_sum            'C30 H47 Fe P3 Si'
_chemical_formula_weight         584.52
_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   difmap
_atom_sites_solution_primary     dual
_audit_creation_date             2019-06-11
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_audit_update_record
;
2019-06-24 deposited with the CCDC.	2021-11-02 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 101.511(2)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   9.1689(2)
_cell_length_b                   16.6564(3)
_cell_length_c                   21.0278(5)
_cell_measurement_reflns_used    57520
_cell_measurement_temperature    180
_cell_measurement_theta_max      64.45
_cell_measurement_theta_min      1.87
_cell_volume                     3146.79(12)
_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_temperature      180
_diffrn_detector                 'Eiger R 4M'
_diffrn_detector_area_resol_mean 13.33
_diffrn_detector_type            DECTRIS
_diffrn_measured_fraction_theta_full 0.995
_diffrn_measured_fraction_theta_max 0.989
_diffrn_measurement_device       'Eulerian 4-circle diffractometer'
_diffrn_measurement_device_type  'Stoe StadiVari'
_diffrn_measurement_method       'rotation method, ω scans'
_diffrn_radiation_collimation    '1.2 0.6 mm diameter'
_diffrn_radiation_monochromator  'Graded multilayer mirror'
_diffrn_radiation_polarisn_norm  0
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           GaK\a
_diffrn_radiation_wavelength     1.34143
_diffrn_reflns_av_R_equivalents  0.0150
_diffrn_reflns_av_unetI/netI     0.0106
_diffrn_reflns_Laue_measured_fraction_full 0.995
_diffrn_reflns_Laue_measured_fraction_max 0.989
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -4
_diffrn_reflns_limit_k_max       22
_diffrn_reflns_limit_k_min       -21
_diffrn_reflns_limit_l_max       27
_diffrn_reflns_limit_l_min       -27
_diffrn_reflns_number            36536
_diffrn_reflns_point_group_measured_fraction_full 0.995
_diffrn_reflns_point_group_measured_fraction_max 0.989
_diffrn_reflns_theta_full        53.597
_diffrn_reflns_theta_max         62.582
_diffrn_reflns_theta_min         2.968
_diffrn_source                   'Metaljet D2'
_diffrn_source_current           2.860
_diffrn_source_power             0.200
_diffrn_source_target            Ga
_diffrn_source_type              'Metaljet D2'
_diffrn_source_voltage           70
_exptl_absorpt_coefficient_mu    3.831
_exptl_absorpt_correction_T_max  0.2117
_exptl_absorpt_correction_T_min  0.0733
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
STOE LANA, absorption correction by scaling of reflection intensities.
J. Koziskova, F. Hahn, J. Richter, J. Kozisek, "Comparison of different
absorption corrections on the model structure of tetrakis(μ₂-acetato)-
diaqua-di-copper(II)", Acta Chimica Slovaca, vol. 9, no. 2, 2016, pp. 136 - 140.
Afterwards a spherical absorption correction was performed within STOE LANA.
;
_exptl_crystal_colour            yellow
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    1.234
_exptl_crystal_description       block
_exptl_crystal_F_000             1248
_exptl_crystal_size_max          0.36
_exptl_crystal_size_mid          0.34
_exptl_crystal_size_min          0.33
_refine_diff_density_max         0.811
_refine_diff_density_min         -0.278
_refine_diff_density_rms         0.048
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.026
_refine_ls_hydrogen_treatment    refall
_refine_ls_matrix_type           full
_refine_ls_number_parameters     504
_refine_ls_number_reflns         7553
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.026
_refine_ls_R_factor_all          0.0290
_refine_ls_R_factor_gt           0.0270
_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/[σ²(Fo²)+(0.0437P)²+1.2875P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0741
_refine_ls_wR_factor_ref         0.0754
_reflns_Friedel_coverage         0.000
_reflns_number_gt                7100
_reflns_number_total             7553
_reflns_threshold_expression     'I > 2σ(I)'
_cod_data_source_file            d1dt02832d2.cif
_cod_data_source_block           sun35
_cod_database_code               7708678
_shelx_shelxl_version_number     2018/3
_shelx_space_group_comment
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;
_shelx_estimated_absorpt_t_max   0.365
_shelx_estimated_absorpt_t_min   0.339
_olex2_refinement_description
;
;
_olex2_submission_special_instructions 'No special instructions were received'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x+1/2, y+1/2, -z+1/2'
'-x, -y, -z'
'x-1/2, -y-1/2, z-1/2'
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
Fe1 Fe 0.66984(2) 0.81532(2) 0.39325(2) 0.01963(6) Uani 1 1 d . . . . .
H1 H 0.712(2) 0.8872(12) 0.4380(9) 0.040(5) Uiso 1 1 d . . . . .
P1 P 0.78353(4) 0.75740(2) 0.48329(2) 0.02108(7) Uani 1 1 d . . . . .
P2 P 0.44036(4) 0.82735(2) 0.40923(2) 0.02623(8) Uani 1 1 d . . . . .
P3 P 0.67620(4) 0.91873(2) 0.33073(2) 0.02699(8) Uani 1 1 d . . . . .
Si1 Si 0.73536(4) 0.70178(2) 0.34509(2) 0.02146(8) Uani 1 1 d . . . . .
C1 C 0.80947(15) 0.71562(8) 0.26745(6) 0.0248(3) Uani 1 1 d . . . . .
C2 C 0.72305(17) 0.70497(9) 0.20546(7) 0.0288(3) Uani 1 1 d . . . . .
H2 H 0.624(3) 0.6893(12) 0.1999(11) 0.048(6) Uiso 1 1 d . . . . .
C3 C 0.77956(18) 0.71875(10) 0.14999(7) 0.0328(3) Uani 1 1 d . . . . .
H3 H 0.715(2) 0.7125(13) 0.1090(11) 0.050(6) Uiso 1 1 d . . . . .
C4 C 0.92576(19) 0.74183(10) 0.15511(7) 0.0358(3) Uani 1 1 d . . . . .
H4 H 0.965(2) 0.7524(13) 0.1157(10) 0.047(6) Uiso 1 1 d . . . . .
C5 C 1.0150(2) 0.75188(12) 0.21572(8) 0.0422(4) Uani 1 1 d . . . . .
H5 H 1.114(2) 0.7660(13) 0.2197(10) 0.050(6) Uiso 1 1 d . . . . .
C6 C 0.95684(18) 0.73941(11) 0.27093(7) 0.0352(3) Uani 1 1 d . . . . .
H6 H 1.019(2) 0.7450(13) 0.3129(11) 0.049(6) Uiso 1 1 d . . . . .
C7 C 0.59381(16) 0.61649(8) 0.32420(7) 0.0282(3) Uani 1 1 d . . . . .
C8 C 0.44986(19) 0.63199(11) 0.28930(8) 0.0376(3) Uani 1 1 d . . . . .
H8 H 0.421(2) 0.6842(13) 0.2758(11) 0.046(6) Uiso 1 1 d . . . . .
C9 C 0.3424(2) 0.57187(13) 0.27500(9) 0.0500(5) Uani 1 1 d . . . . .
H9 H 0.244(3) 0.5847(15) 0.2489(12) 0.068(7) Uiso 1 1 d . . . . .
C10 C 0.3775(3) 0.49451(13) 0.29581(9) 0.0542(5) Uani 1 1 d . . . . .
H10 H 0.307(3) 0.4531(15) 0.2876(11) 0.062(7) Uiso 1 1 d . . . . .
C11 C 0.5184(3) 0.47688(11) 0.32990(9) 0.0495(5) Uani 1 1 d . . . . .
H11 H 0.544(3) 0.4232(15) 0.3458(12) 0.062(7) Uiso 1 1 d . . . . .
C12 C 0.6254(2) 0.53725(9) 0.34369(8) 0.0353(3) Uani 1 1 d . . . . .
H12 H 0.715(2) 0.5256(12) 0.3675(10) 0.036(5) Uiso 1 1 d . . . . .
C13 C 0.89858(15) 0.65576(8) 0.40427(6) 0.0239(2) Uani 1 1 d . . . . .
C14 C 0.92204(15) 0.68344(8) 0.46821(7) 0.0234(2) Uani 1 1 d . . . . .
C15 C 1.03992(16) 0.65301(9) 0.51486(7) 0.0296(3) Uani 1 1 d . . . . .
H15 H 1.058(2) 0.6716(11) 0.5578(10) 0.032(5) Uiso 1 1 d . . . . .
C16 C 1.13424(17) 0.59522(10) 0.49751(8) 0.0349(3) Uani 1 1 d . . . . .
H16 H 1.218(2) 0.5757(13) 0.5313(10) 0.047(6) Uiso 1 1 d . . . . .
C17 C 1.11287(18) 0.56791(9) 0.43445(8) 0.0362(3) Uani 1 1 d . . . . .
H17 H 1.183(2) 0.5292(13) 0.4226(10) 0.047(5) Uiso 1 1 d . . . . .
C18 C 0.99610(17) 0.59781(9) 0.38820(8) 0.0313(3) Uani 1 1 d . . . . .
H18 H 0.983(2) 0.5790(12) 0.3448(10) 0.038(5) Uiso 1 1 d . . . . .
C19 C 0.89715(16) 0.82569(9) 0.54404(7) 0.0284(3) Uani 1 1 d . . . . .
H19 H 0.9505(19) 0.7897(11) 0.5774(9) 0.030(4) Uiso 1 1 d . . . . .
C20 C 1.00998(18) 0.87244(10) 0.51424(8) 0.0356(3) Uani 1 1 d . . . . .
H20A H 0.964(2) 0.9102(13) 0.4819(10) 0.044(5) Uiso 1 1 d . . . . .
H20B H 1.078(2) 0.9037(13) 0.5480(11) 0.052(6) Uiso 1 1 d . . . . .
H20C H 1.069(2) 0.8380(13) 0.4911(11) 0.048(6) Uiso 1 1 d . . . . .
C21 C 0.8011(2) 0.88283(11) 0.57505(9) 0.0402(4) Uani 1 1 d . . . . .
H21A H 0.726(2) 0.8554(14) 0.5965(10) 0.050(6) Uiso 1 1 d . . . . .
H21B H 0.862(2) 0.9135(14) 0.6101(11) 0.051(6) Uiso 1 1 d . . . . .
H21C H 0.750(2) 0.9201(13) 0.5432(11) 0.047(6) Uiso 1 1 d . . . . .
C22 C 0.68182(17) 0.69709(9) 0.53582(7) 0.0287(3) Uani 1 1 d . . . . .
H22 H 0.602(2) 0.7302(11) 0.5398(9) 0.032(4) Uiso 1 1 d . . . . .
C23 C 0.6221(2) 0.61961(10) 0.50085(8) 0.0357(3) Uani 1 1 d . . . . .
H23A H 0.570(2) 0.6300(12) 0.4559(10) 0.038(5) Uiso 1 1 d . . . . .
H23B H 0.702(2) 0.5850(13) 0.5018(10) 0.046(6) Uiso 1 1 d . . . . .
H23C H 0.552(2) 0.5925(12) 0.5248(10) 0.042(5) Uiso 1 1 d . . . . .
C24 C 0.7662(2) 0.67669(12) 0.60428(8) 0.0409(4) Uani 1 1 d . . . . .
H24A H 0.801(2) 0.7241(14) 0.6278(11) 0.049(6) Uiso 1 1 d . . . . .
H24B H 0.855(2) 0.6464(14) 0.6059(10) 0.049(6) Uiso 1 1 d . . . . .
H24C H 0.700(2) 0.6474(13) 0.6280(11) 0.052(6) Uiso 1 1 d . . . . .
C25 C 0.4075(2) 0.89654(12) 0.47235(11) 0.0452(4) Uani 1 1 d . . . . .
H25A H 0.461(3) 0.8762(16) 0.5134(13) 0.069(8) Uiso 1 1 d . . . . .
H25B H 0.302(3) 0.9008(15) 0.4716(12) 0.065(7) Uiso 1 1 d . . . . .
H25C H 0.444(2) 0.9484(14) 0.4641(11) 0.053(6) Uiso 1 1 d . . . . .
C26 C 0.30218(19) 0.86437(13) 0.34021(11) 0.0462(4) Uani 1 1 d . . . . .
H26A H 0.299(3) 0.8264(15) 0.3049(13) 0.061(7) Uiso 1 1 d . . . . .
H26B H 0.332(3) 0.9161(16) 0.3270(12) 0.067(7) Uiso 1 1 d . . . . .
H26C H 0.205(3) 0.8673(15) 0.3503(12) 0.066(7) Uiso 1 1 d . . . . .
C27 C 0.33438(18) 0.74023(10) 0.42783(9) 0.0369(3) Uani 1 1 d . . . . .
H27A H 0.342(3) 0.6996(14) 0.3970(12) 0.056(6) Uiso 1 1 d . . . . .
H27B H 0.376(2) 0.7194(14) 0.4711(11) 0.051(6) Uiso 1 1 d . . . . .
H27C H 0.233(2) 0.7559(12) 0.4262(10) 0.041(5) Uiso 1 1 d . . . . .
C28 C 0.5971(3) 0.90984(12) 0.24387(8) 0.0457(4) Uani 1 1 d . . . . .
H28A H 0.609(3) 0.9588(16) 0.2207(13) 0.068(7) Uiso 1 1 d . . . . .
H28B H 0.645(3) 0.8656(17) 0.2270(12) 0.070(7) Uiso 1 1 d . . . . .
H28C H 0.497(3) 0.8972(14) 0.2388(11) 0.053(6) Uiso 1 1 d . . . . .
C29 C 0.8632(2) 0.95413(11) 0.32720(10) 0.0409(4) Uani 1 1 d . . . . .
H29A H 0.859(3) 0.9991(15) 0.3032(11) 0.058(6) Uiso 1 1 d . . . . .
H29B H 0.921(3) 0.9617(15) 0.3691(13) 0.067(7) Uiso 1 1 d . . . . .
H29C H 0.917(2) 0.9144(13) 0.3089(10) 0.046(6) Uiso 1 1 d . . . . .
C30 C 0.5950(2) 1.01410(10) 0.34954(11) 0.0438(4) Uani 1 1 d . . . . .
H30A H 0.604(3) 1.0532(16) 0.3178(12) 0.066(7) Uiso 1 1 d . . . . .
H30B H 0.645(3) 1.0287(14) 0.3917(12) 0.055(6) Uiso 1 1 d . . . . .
H30C H 0.487(3) 1.0111(16) 0.3527(12) 0.070(7) Uiso 1 1 d . . . . .
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0148 0.0070 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Fe Fe -0.2786 2.5796 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
P P 0.2596 0.3354 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Si Si 0.2148 0.2489 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
P1 Fe1 P2 102.230(15) . . ?
P1 Fe1 Si1 84.069(14) . . ?
P2 Fe1 Si1 119.123(15) . . ?
P3 Fe1 P1 143.562(16) . . ?
P3 Fe1 P2 99.308(15) . . ?
P3 Fe1 Si1 110.305(15) . . ?
C14 P1 Fe1 111.76(4) . . ?
C14 P1 C19 102.46(6) . . ?
C14 P1 C22 100.63(6) . . ?
C19 P1 Fe1 115.28(5) . . ?
C19 P1 C22 101.47(7) . . ?
C22 P1 Fe1 122.53(5) . . ?
C25 P2 Fe1 117.94(6) . . ?
C25 P2 C26 100.07(11) . . ?
C25 P2 C27 99.97(9) . . ?
C26 P2 Fe1 116.09(7) . . ?
C27 P2 Fe1 121.58(6) . . ?
C27 P2 C26 97.08(9) . . ?
C28 P3 Fe1 119.06(7) . . ?
C29 P3 Fe1 114.74(6) . . ?
C29 P3 C28 100.00(10) . . ?
C29 P3 C30 98.85(9) . . ?
C30 P3 Fe1 119.71(7) . . ?
C30 P3 C28 100.85(10) . . ?
C1 Si1 Fe1 116.80(4) . . ?
C1 Si1 C7 103.57(6) . . ?
C1 Si1 C13 103.92(6) . . ?
C7 Si1 Fe1 119.36(5) . . ?
C13 Si1 Fe1 106.59(4) . . ?
C13 Si1 C7 105.03(6) . . ?
C2 C1 Si1 123.54(11) . . ?
C2 C1 C6 116.65(13) . . ?
C6 C1 Si1 119.80(10) . . ?
C3 C2 C1 121.80(14) . . ?
C4 C3 C2 120.09(14) . . ?
C3 C4 C5 119.61(14) . . ?
C4 C5 C6 119.92(15) . . ?
C5 C6 C1 121.91(14) . . ?
C8 C7 Si1 120.54(11) . . ?
C12 C7 Si1 122.88(12) . . ?
C12 C7 C8 116.55(14) . . ?
C9 C8 C7 122.14(17) . . ?
C10 C9 C8 119.52(19) . . ?
C9 C10 C11 119.97(16) . . ?
C10 C11 C12 120.14(18) . . ?
C11 C12 C7 121.67(18) . . ?
C14 C13 Si1 116.47(10) . . ?
C14 C13 C18 118.43(13) . . ?
C18 C13 Si1 125.09(11) . . ?
C13 C14 P1 114.05(10) . . ?
C13 C14 C15 120.22(13) . . ?
C15 C14 P1 125.69(11) . . ?
C16 C15 C14 120.00(14) . . ?
C17 C16 C15 120.29(14) . . ?
C16 C17 C18 119.83(14) . . ?
C17 C18 C13 121.22(14) . . ?
C20 C19 P1 111.21(10) . . ?
C20 C19 C21 110.67(14) . . ?
C21 C19 P1 112.42(11) . . ?
C23 C22 P1 109.95(10) . . ?
C24 C22 P1 117.12(11) . . ?
C24 C22 C23 109.26(14) . . ?
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Fe1 P1 2.1943(4) . ?
Fe1 P2 2.2051(4) . ?
Fe1 P3 2.1745(4) . ?
Fe1 Si1 2.2816(4) . ?
P1 C14 1.8415(14) . ?
P1 C19 1.8654(14) . ?
P1 C22 1.8734(14) . ?
P2 C25 1.8275(18) . ?
P2 C26 1.8325(18) . ?
P2 C27 1.8315(16) . ?
P3 C28 1.8319(18) . ?
P3 C29 1.8284(18) . ?
P3 C30 1.8308(18) . ?
Si1 C1 1.9036(14) . ?
Si1 C7 1.9152(14) . ?
Si1 C13 1.9059(14) . ?
C1 C2 1.3950(19) . ?
C1 C6 1.396(2) . ?
C2 C3 1.387(2) . ?
C3 C4 1.378(2) . ?
C4 C5 1.380(2) . ?
C5 C6 1.386(2) . ?
C7 C8 1.400(2) . ?
C7 C12 1.395(2) . ?
C8 C9 1.395(2) . ?
C9 C10 1.378(3) . ?
C10 C11 1.378(3) . ?
C11 C12 1.394(2) . ?
C13 C14 1.3968(19) . ?
C13 C18 1.4021(19) . ?
C14 C15 1.4014(19) . ?
C15 C16 1.391(2) . ?
C16 C17 1.378(2) . ?
C17 C18 1.387(2) . ?
C19 C20 1.526(2) . ?
C19 C21 1.528(2) . ?
C22 C23 1.531(2) . ?
C22 C24 1.531(2) . ?
