#------------------------------------------------------------------------------
#$Date: 2024-09-24 11:55:37 +0300 (Tue, 24 Sep 2024) $
#$Revision: 294865 $
#$URL: file:///home/coder/svn-repositories/cod/cif/7/70/86/7708673.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_7708673
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         '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  tₑₓₚ   ω     θ     κ     φ   Frames
#--------------------------------------------------------------------------
  1  ω    -83.00 -55.00   1.00    0.10    --  -48.45 106.00  85.00   28
  2  ω     16.00  71.00   1.00    0.10    --   48.45-106.00 -13.00   55
  3  ω    -85.00 -13.00   1.00    0.45    --  -86.25 106.00  85.00   72
  4  ω   -136.00 -80.00   1.00    0.45    --  -86.25-106.00 -13.00   56
  5  ω    102.00 160.00   1.00    0.45    --  106.49 106.00  85.00   58
  6  ω     39.00 111.00   1.00    0.45    --  106.49-106.00 -13.00   72
  7  ω    -47.00   1.00   1.00    0.10    --  -48.45 106.00  85.00   48
  8  ω    -60.00  23.00   1.00    0.10    --  -48.45  38.00 120.00   83
  9  ω   -120.00 -74.00   1.00    0.10    --  -48.45-125.00 120.00   46
 10  ω    -60.00  27.00   1.00    0.10    --  -48.45  19.00  30.00   87
 11  ω   -156.00 -71.00   1.00    0.45    --  -86.25 -57.00   0.00   85
 12  ω   -158.00 -83.00   1.00    0.45    --  -86.25 -99.00  90.00   75
 13  ω     93.00 168.00   1.00    0.45    --  106.49 125.00  30.00   75
 14  ω     93.00 178.00   1.00    0.45    --  106.49  38.00-180.00   85
 15  ω     34.00 117.00   1.00    0.45    --  106.49-125.00 -30.00   83
 16  ω     34.00 120.00   1.00    0.45    --  106.49 -38.00 -30.00   86
 17  ω     37.00 115.00   1.00    0.45    --  106.49-125.00-150.00   78
 18  ω     35.00 117.00   1.00    0.45    --  106.49-125.00 150.00   82
 19  ω     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       'ω 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/[σ²(Fo²)+(0.0191P)²+4.8982P] where P=(Fo²+2Fc²)/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 > 2σ(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
_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.
;
_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)
;
_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
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, -y, -z'
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
Fe2 Fe 0.55765(4) 0.81296(4) 0.88204(2) 0.01500(9) Uani 1 1 d . . . . .
Fe1 Fe 0.96638(4) 0.26571(4) 0.61451(2) 0.01524(9) Uani 1 1 d . . . . .
P2 P 0.91260(7) 0.22003(6) 0.67171(2) 0.01615(13) Uani 1 1 d . . . . .
P62 P 0.60774(7) 0.85168(6) 0.82418(2) 0.01645(13) Uani 1 1 d . . . . .
P1 P 0.86056(7) 0.26203(7) 0.55927(2) 0.01921(14) Uani 1 1 d . . . . .
P55 P 0.65329(7) 0.80980(7) 0.93760(2) 0.01882(14) Uani 1 1 d . . . . .
Si2 Si 0.58831(8) 0.60702(7) 0.86468(2) 0.01685(14) Uani 1 1 d . . . . .
Si1 Si 0.92713(8) 0.46446(7) 0.63259(2) 0.01635(14) Uani 1 1 d . . . . .
P3 P 1.21596(7) 0.40447(7) 0.61471(2) 0.02053(14) Uani 1 1 d . . . . .
P74 P 0.30489(7) 0.71645(7) 0.88151(2) 0.02222(14) Uani 1 1 d . . . . .
N78 N 0.5565(3) 0.9869(2) 0.89603(6) 0.0225(5) Uani 1 1 d . . . . .
N1 N 0.9825(3) 0.0984(2) 0.60002(6) 0.0233(5) Uani 1 1 d . . . . .
N2 N 0.9969(3) 0.0003(3) 0.59082(8) 0.0362(6) Uani 1 1 d . . . . .
N77 N 0.5478(3) 1.0893(3) 0.90434(7) 0.0340(6) Uani 1 1 d . . . . .
C18 C 0.7859(3) 0.2972(3) 0.68771(7) 0.0190(5) Uani 1 1 d . . . . .
C41 C 0.7305(3) 0.7708(3) 0.80879(7) 0.0188(5) Uani 1 1 d . . . . .
C7 C 0.8282(3) 0.4971(3) 0.59248(7) 0.0192(5) Uani 1 1 d . . . . .
C13 C 0.7946(3) 0.4134(3) 0.67043(7) 0.0184(5) Uani 1 1 d . . . . .
C43 C 0.4399(3) 0.4088(3) 0.85111(7) 0.0196(5) Uani 1 1 d . . . . .
C1 C 1.0713(3) 0.6585(3) 0.65225(7) 0.0208(5) Uani 1 1 d . . . . .
C63 C 0.4639(3) 0.7835(3) 0.78300(7) 0.0220(5) Uani 1 1 d . . . . .
H63 H 0.3969 0.8283 0.7876 0.026 Uiso 1 1 calc R . . . .
C36 C 0.7123(3) 0.6486(3) 0.82459(7) 0.0197(5) Uani 1 1 d . . . . .
C65 C 0.7132(3) 1.0448(3) 0.81630(8) 0.0240(6) Uani 1 1 d . . . . .
H65 H 0.7516 1.0422 0.7920 0.029 Uiso 1 1 calc R . . . .
C15 C 0.6099(3) 0.4333(3) 0.70927(8) 0.0277(6) Uani 1 1 d . . . . .
H15 H 0.5516 0.4794 0.7164 0.033 Uiso 1 1 calc R . . . .
C8 C 0.7821(3) 0.6071(3) 0.59400(8) 0.0259(6) Uani 1 1 d . . . . .
H8 H 0.8039 0.6718 0.6157 0.031 Uiso 1 1 calc R . . . .
C44 C 0.3708(3) 0.3248(3) 0.87852(8) 0.0282(6) Uani 1 1 d . . . . .
H44 H 0.3990 0.3659 0.9033 0.034 Uiso 1 1 calc R . . . .
C25 C 0.8010(3) 0.0264(3) 0.67919(8) 0.0238(6) Uani 1 1 d . . . . .
H25 H 0.7677 0.0301 0.7041 0.029 Uiso 1 1 calc R . . . .
C49 C 0.7023(3) 0.5858(3) 0.90389(7) 0.0208(5) Uani 1 1 d . . . . .
C12 C 0.7970(3) 0.4031(3) 0.55917(7) 0.0224(5) Uani 1 1 d . . . . .
C17 C 0.6879(3) 0.2490(3) 0.71521(8) 0.0239(6) Uani 1 1 d . . . . .
H17 H 0.6814 0.1712 0.7264 0.029 Uiso 1 1 calc R . . . .
C6 C 1.1099(3) 0.7039(3) 0.69028(8) 0.0257(6) Uani 1 1 d . . . . .
H6 H 1.0645 0.6382 0.7066 0.031 Uiso 1 1 calc R . . . .
C37 C 0.7917(3) 0.5742(3) 0.81154(8) 0.0254(6) Uani 1 1 d . . . . .
H37 H 0.7784 0.4909 0.8211 0.030 Uiso 1 1 calc R . . . .
C50 C 0.7381(3) 0.6846(3) 0.93655(7) 0.0212(5) Uani 1 1 d . . . . .
C28 C 1.0610(3) 0.2973(3) 0.71188(7) 0.0216(5) Uani 1 1 d . . . . .
H28 H 1.1092 0.4025 0.7121 0.026 Uiso 1 1 calc R . . . .
C40 C 0.8310(3) 0.8186(3) 0.78149(8) 0.0260(6) Uani 1 1 d . . . . .
H40 H 0.8437 0.9004 0.7712 0.031 Uiso 1 1 calc R . . . .
C38 C 0.8900(3) 0.6212(3) 0.78453(8) 0.0301(6) Uani 1 1 d . . . . .
H38 H 0.9421 0.5699 0.7763 0.036 Uiso 1 1 calc R . . . .
C31 C 1.3301(3) 0.5352(3) 0.65522(8) 0.0283(6) Uani 1 1 d . . . . .
H31A H 1.3060 0.6151 0.6583 0.042 Uiso 1 1 calc GR . . . .
H31B H 1.4347 0.5701 0.6516 0.042 Uiso 1 1 calc GR . . . .
H31C H 1.3093 0.4885 0.6769 0.042 Uiso 1 1 calc GR . . . .
C2 C 1.1411(3) 0.7627(3) 0.62909(9) 0.0274(6) Uani 1 1 d . . . . .
H2 H 1.1160 0.7371 0.6037 0.033 Uiso 1 1 calc R . . . .
C48 C 0.3972(3) 0.3401(3) 0.81450(8) 0.0245(6) Uani 1 1 d . . . . .
H48 H 0.4430 0.3913 0.7955 0.029 Uiso 1 1 calc R . . . .
C14 C 0.7066(3) 0.4812(3) 0.68207(8) 0.0247(6) Uani 1 1 d . . . . .
H14 H 0.7131 0.5600 0.6713 0.030 Uiso 1 1 calc R . . . .
C30 C 1.1858(3) 0.2512(3) 0.70661(8) 0.0298(6) Uani 1 1 d . . . . .
H30A H 1.1575 0.1602 0.7154 0.045 Uiso 1 1 calc GR . . . .
H30B H 1.2771 0.3235 0.7203 0.045 Uiso 1 1 calc GR . . . .
H30C H 1.2009 0.2411 0.6808 0.045 Uiso 1 1 calc GR . . . .
C47 C 0.2879(4) 0.1970(3) 0.80570(9) 0.0331(7) Uani 1 1 d . . . . .
H47 H 0.2611 0.1541 0.7811 0.040 Uiso 1 1 calc R . . . .
C16 C 0.6001(3) 0.3176(3) 0.72575(8) 0.0260(6) Uani 1 1 d . . . . .
H16 H 0.5347 0.2852 0.7439 0.031 Uiso 1 1 calc R . . . .
C11 C 0.7168(4) 0.4168(3) 0.52907(9) 0.0336(7) Uani 1 1 d . . . . .
H11 H 0.6937 0.3523 0.5072 0.040 Uiso 1 1 calc R . . . .
C29 C 1.0078(3) 0.2741(3) 0.75051(8) 0.0288(6) Uani 1 1 d . . . . .
H29A H 0.9356 0.3106 0.7546 0.043 Uiso 1 1 calc GR . . . .
H29B H 1.0921 0.3249 0.7688 0.043 Uiso 1 1 calc GR . . . .
H29C H 0.9622 0.1725 0.7523 0.043 Uiso 1 1 calc GR . . . .
C51 C 0.8269(3) 0.6793(3) 0.96615(8) 0.0281(6) Uani 1 1 d . . . . .
H51 H 0.8527 0.7470 0.9875 0.034 Uiso 1 1 calc R . . . .
C56 C 0.8153(3) 0.9808(3) 0.96098(8) 0.0306(6) Uani 1 1 d . . . . .
H56 H 0.8479 0.9575 0.9838 0.037 Uiso 1 1 calc R . . . .
C53 C 0.8376(3) 0.4724(3) 0.93238(8) 0.0294(6) Uani 1 1 d . . . . .
H53 H 0.8690 0.4004 0.9312 0.035 Uiso 1 1 calc R . . . .
C67 C 0.8504(3) 1.1329(3) 0.84430(9) 0.0328(7) Uani 1 1 d . . . . .
H67A H 0.8179 1.1487 0.8681 0.049 Uiso 1 1 calc GR . . . .
H67B H 0.9110 1.2246 0.8364 0.049 Uiso 1 1 calc GR . . . .
H67C H 0.9083 1.0805 0.8459 0.049 Uiso 1 1 calc GR . . . .
C46 C 0.2190(3) 0.1186(3) 0.83336(10) 0.0350(7) Uani 1 1 d . . . . .
H46 H 0.1445 0.0235 0.8275 0.042 Uiso 1 1 calc R . . . .
C54 C 0.7521(3) 0.4784(3) 0.90277(8) 0.0274(6) Uani 1 1 d . . . . .
H54 H 0.7269 0.4100 0.8816 0.033 Uiso 1 1 calc R . . . .
C68 C 0.3670(3) 0.6194(3) 0.77928(8) 0.0299(6) Uani 1 1 d . . . . .
H68A H 0.4241 0.5708 0.7700 0.045 Uiso 1 1 calc GR . . . .
H68B H 0.2798 0.5910 0.7625 0.045 Uiso 1 1 calc GR . . . .
H68C H 0.3365 0.5932 0.8031 0.045 Uiso 1 1 calc GR . . . .
C52 C 0.8761(3) 0.5746(3) 0.96388(8) 0.0300(6) Uani 1 1 d . . . . .
H52 H 0.9356 0.5724 0.9836 0.036 Uiso 1 1 calc R . . . .
C5 C 1.2146(3) 0.8446(3) 0.70433(10) 0.0353(7) Uani 1 1 d . . . . .
H5 H 1.2383 0.8720 0.7298 0.042 Uiso 1 1 calc R . . . .
C32 C 1.2853(3) 0.5283(3) 0.58013(9) 0.0318(7) Uani 1 1 d . . . . .
H32A H 1.2642 0.4729 0.5559 0.048 Uiso 1 1 calc GR . . . .
H32B H 1.3917 0.5872 0.5853 0.048 Uiso 1 1 calc GR . . . .
H32C H 1.2361 0.5895 0.5812 0.048 Uiso 1 1 calc GR . . . .
C9 C 0.7053(3) 0.6209(3) 0.56392(9) 0.0314(7) Uani 1 1 d . . . . .
H9 H 0.6761 0.6945 0.5654 0.038 Uiso 1 1 calc R . . . .
C19 C 0.9717(3) 0.2835(3) 0.51761(8) 0.0279(6) Uani 1 1 d . . . . .
H19 H 1.0447 0.3863 0.5207 0.033 Uiso 1 1 calc R . . . .
C45 C 0.2618(3) 0.1824(3) 0.86988(10) 0.0354(7) Uani 1 1 d . . . . .
H45 H 0.2171 0.1296 0.8887 0.043 Uiso 1 1 calc R . . . .
C60 C 0.4178(4) 0.5967(3) 0.96714(9) 0.0365(7) Uani 1 1 d . . . . .
H60A H 0.3751 0.5760 0.9420 0.055 Uiso 1 1 calc GR . . . .
H60B H 0.3392 0.5738 0.9834 0.055 Uiso 1 1 calc GR . . . .
H60C H 0.4693 0.5394 0.9703 0.055 Uiso 1 1 calc GR . . . .
C64 C 0.5249(4) 0.8198(3) 0.74550(8) 0.0311(6) Uani 1 1 d . . . . .
H64A H 0.5740 0.9231 0.7462 0.047 Uiso 1 1 calc GR . . . .
H64B H 0.4433 0.7769 0.7263 0.047 Uiso 1 1 calc GR . . . .
H64C H 0.5954 0.7819 0.7406 0.047 Uiso 1 1 calc GR . . . .
C58 C 0.5288(3) 0.7578(3) 0.97628(8) 0.0274(6) Uani 1 1 d . . . . .
H58 H 0.4690 0.8111 0.9759 0.033 Uiso 1 1 calc R . . . .
C21 C 1.0644(4) 0.2007(3) 0.51813(9) 0.0334(7) Uani 1 1 d . . . . .
H21A H 1.1226 0.2275 0.5416 0.050 Uiso 1 1 calc GR . . . .
H21B H 1.1304 0.2239 0.4987 0.050 Uiso 1 1 calc GR . . . .
H21C H 0.9986 0.0984 0.5144 0.050 Uiso 1 1 calc GR . . . .
C10 C 0.6718(4) 0.5244(3) 0.53135(9) 0.0351(7) Uani 1 1 d . . . . .
H10 H 0.6190 0.5326 0.5111 0.042 Uiso 1 1 calc R . . . .
C39 C 0.9103(3) 0.7441(3) 0.77002(8) 0.0310(7) Uani 1 1 d . . . . .
H39 H 0.9781 0.7770 0.7523 0.037 Uiso 1 1 calc R . . . .
C73 C 0.1713(3) 0.5225(3) 0.87206(9) 0.0317(7) Uani 1 1 d . . . . .
H73A H 0.1872 0.4808 0.8487 0.047 Uiso 1 1 calc GR . . . .
H73B H 0.0705 0.5115 0.8711 0.047 Uiso 1 1 calc GR . . . .
H73C H 0.1864 0.4740 0.8914 0.047 Uiso 1 1 calc GR . . . .
C22 C 0.6767(3) 0.1019(3) 0.54187(8) 0.0281(6) Uani 1 1 d . . . . .
H22 H 0.6483 0.1166 0.5174 0.034 Uiso 1 1 calc R . . . .
C26 C 0.6590(3) -0.0511(3) 0.65271(9) 0.0364(7) Uani 1 1 d . . . . .
H26A H 0.6066 0.0071 0.6533 0.055 Uiso 1 1 calc GR . . . .
H26B H 0.5956 -0.1430 0.6601 0.055 Uiso 1 1 calc GR . . . .
H26C H 0.6853 -0.0663 0.6281 0.055 Uiso 1 1 calc GR . . . .
C33 C 1.3302(3) 0.3072(3) 0.60692(9) 0.0321(7) Uani 1 1 d . . . . .
H33A H 1.3254 0.2547 0.6271 0.048 Uiso 1 1 calc GR . . . .
H33B H 1.4326 0.3756 0.6053 0.048 Uiso 1 1 calc GR . . . .
H33C H 1.2923 0.2405 0.5843 0.048 Uiso 1 1 calc GR . . . .
C3 C 1.2464(3) 0.9030(3) 0.64300(10) 0.0358(7) Uani 1 1 d . . . . .
H3 H 1.2920 0.9693 0.6269 0.043 Uiso 1 1 calc R . . . .
C66 C 0.6133(4) 1.1209(3) 0.81415(9) 0.0332(7) Uani 1 1 d . . . . .
H66A H 0.5357 1.0700 0.7942 0.050 Uiso 1 1 calc GR . . . .
H66B H 0.6729 1.2188 0.8099 0.050 Uiso 1 1 calc GR . . . .
H66C H 0.5687 1.1216 0.8370 0.050 Uiso 1 1 calc GR . . . .
C27 C 0.8872(4) -0.0636(3) 0.67863(10) 0.0359(7) Uani 1 1 d . . . . .
H27A H 0.9356 -0.0582 0.6562 0.054 Uiso 1 1 calc GR . . . .
H27B H 0.8186 -0.1628 0.6799 0.054 Uiso 1 1 calc GR . . . .
H27C H 0.9615 -0.0264 0.6995 0.054 Uiso 1 1 calc GR . . . .
C75 C 0.2332(4) 0.7689(4) 0.92337(9) 0.0362(7) Uani 1 1 d . . . . .
H75A H 0.2440 0.7187 0.9428 0.054 Uiso 1 1 calc GR . . . .
H75B H 0.1290 0.7439 0.9182 0.054 Uiso 1 1 calc GR . . . .
H75C H 0.2890 0.8717 0.9311 0.054 Uiso 1 1 calc GR . . . .
C4 C 1.2839(3) 0.9445(3) 0.68049(11) 0.0401(8) Uani 1 1 d . . . . .
H4 H 1.3550 1.0385 0.6898 0.048 Uiso 1 1 calc R . . . .
C76 C 0.2195(3) 0.7850(4) 0.84908(9) 0.0339(7) Uani 1 1 d . . . . .
H76A H 0.2769 0.8884 0.8512 0.051 Uiso 1 1 calc GR . . . .
H76B H 0.1186 0.7613 0.8547 0.051 Uiso 1 1 calc GR . . . .
H76C H 0.2181 0.7414 0.8243 0.051 Uiso 1 1 calc GR . . . .
C61 C 0.9491(4) 1.0308(4) 0.93795(9) 0.0460(9) Uani 1 1 d . . . . .
H61A H 0.9774 0.9542 0.9325 0.069 Uiso 1 1 calc GR . . . .
H61B H 1.0319 1.1144 0.9516 0.069 Uiso 1 1 calc GR . . . .
H61C H 0.9223 1.0552 0.9153 0.069 Uiso 1 1 calc GR . . . .
C59 C 0.6008(4) 0.7898(4) 1.01609(8) 0.0409(8) Uani 1 1 d . . . . .
H59A H 0.6564 0.7354 1.0182 0.061 Uiso 1 1 calc GR . . . .
H59B H 0.5238 0.7625 1.0328 0.061 Uiso 1 1 calc GR . . . .
H59C H 0.6675 0.8916 1.0222 0.061 Uiso 1 1 calc GR . . . .
C57 C 0.7709(4) 1.1021(3) 0.97277(10) 0.0462(9) Uani 1 1 d . . . . .
H57A H 0.7648 1.1468 0.9517 0.069 Uiso 1 1 calc GR . . . .
H57B H 0.8451 1.1734 0.9913 0.069 Uiso 1 1 calc GR . . . .
H57C H 0.6751 1.0619 0.9826 0.069 Uiso 1 1 calc GR . . . .
C23 C 0.5515(4) 0.0920(4) 0.56601(10) 0.0395(8) Uani 1 1 d . . . . .
H23A H 0.5755 0.0785 0.5904 0.059 Uiso 1 1 calc GR . . . .
H23B H 0.4588 0.0113 0.5554 0.059 Uiso 1 1 calc GR . . . .
H23C H 0.5415 0.1799 0.5673 0.059 Uiso 1 1 calc GR . . . .
C24 C 0.6848(4) -0.0424(3) 0.53657(11) 0.0444(9) Uani 1 1 d . . . . .
H24A H 0.7622 -0.0358 0.5208 0.067 Uiso 1 1 calc GR . . . .
H24B H 0.5901 -0.1183 0.5254 0.067 Uiso 1 1 calc GR . . . .
H24C H 0.7074 -0.0636 0.5602 0.067 Uiso 1 1 calc GR . . . .
C20 C 0.8904(4) 0.2501(5) 0.47883(9) 0.0513(10) Uani 1 1 d . . . . .
H20A H 0.8202 0.1491 0.4738 0.077 Uiso 1 1 calc GR . . . .
H20B H 0.9625 0.2727 0.4608 0.077 Uiso 1 1 calc GR . . . .
H20C H 0.8378 0.3076 0.4777 0.077 Uiso 1 1 calc GR . . . .
H H 0.721(4) 0.871(4) 0.8797(10) 0.044(10) Uiso 1 1 d . . . . .
HA H 0.803(4) 0.199(4) 0.6163(10) 0.043(10) 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 0.0181 0.0091 '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 -1.1336 3.1974 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0311 0.0180 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
P P 0.2955 0.4335 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Si Si 0.2541 0.3302 '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
P62 Fe2 Si2 83.65(3) . . ?
P62 Fe2 P74 105.64(3) . . ?
P55 Fe2 P62 145.01(3) . . ?
P55 Fe2 Si2 84.36(3) . . ?
P55 Fe2 P74 108.89(3) . . ?
P74 Fe2 Si2 101.08(3) . . ?
N78 Fe2 P62 94.71(7) . . ?
N78 Fe2 P55 93.55(7) . . ?
N78 Fe2 Si2 173.55(8) . . ?
N78 Fe2 P74 85.37(8) . . ?
P2 Fe1 P1 142.18(3) . . ?
P2 Fe1 Si1 83.54(3) . . ?
P2 Fe1 P3 109.17(3) . . ?
P1 Fe1 Si1 84.81(3) . . ?
P1 Fe1 P3 107.10(3) . . ?
P3 Fe1 Si1 92.11(3) . . ?
N1 Fe1 P2 95.07(7) . . ?
N1 Fe1 P1 93.90(8) . . ?
N1 Fe1 Si1 175.71(8) . . ?
N1 Fe1 P3 92.18(8) . . ?
C18 P2 Fe1 109.32(9) . . ?
C18 P2 C25 100.65(12) . . ?
C18 P2 C28 100.21(12) . . ?
C25 P2 Fe1 118.58(9) . . ?
C28 P2 Fe1 121.91(9) . . ?
C28 P2 C25 102.77(12) . . ?
C41 P62 Fe2 108.95(9) . . ?
C41 P62 C63 100.60(12) . . ?
C41 P62 C65 103.59(12) . . ?
C63 P62 Fe2 125.22(9) . . ?
C65 P62 Fe2 117.10(9) . . ?
C65 P62 C63 98.42(12) . . ?
C12 P1 Fe1 113.10(9) . . ?
C12 P1 C19 103.21(13) . . ?
C12 P1 C22 97.54(13) . . ?
C19 P1 Fe1 119.52(10) . . ?
C22 P1 Fe1 117.53(10) . . ?
C22 P1 C19 102.82(13) . . ?
C50 P55 Fe2 113.05(9) . . ?
C50 P55 C56 99.91(14) . . ?
C50 P55 C58 102.34(13) . . ?
C56 P55 Fe2 117.69(10) . . ?
C56 P55 C58 101.03(13) . . ?
C58 P55 Fe2 119.88(10) . . ?
C43 Si2 Fe2 129.76(8) . . ?
C36 Si2 Fe2 105.71(8) . . ?
C36 Si2 C43 105.15(11) . . ?
C49 Si2 Fe2 108.39(8) . . ?
C49 Si2 C43 99.85(11) . . ?
C49 Si2 C36 106.01(12) . . ?
C7 Si1 Fe1 109.17(8) . . ?
C7 Si1 C13 107.88(12) . . ?
C7 Si1 C1 101.33(12) . . ?
C13 Si1 Fe1 105.97(8) . . ?
C13 Si1 C1 102.28(11) . . ?
C1 Si1 Fe1 128.81(8) . . ?
C31 P3 Fe1 122.18(10) . . ?
C31 P3 C32 96.99(14) . . ?
C31 P3 C33 98.34(14) . . ?
C32 P3 Fe1 119.00(11) . . ?
C32 P3 C33 99.51(15) . . ?
C33 P3 Fe1 116.29(11) . . ?
C73 P74 Fe2 126.34(10) . . ?
C75 P74 Fe2 116.02(11) . . ?
C75 P74 C73 99.40(15) . . ?
C76 P74 Fe2 113.57(11) . . ?
C76 P74 C73 99.39(16) . . ?
C76 P74 C75 97.18(16) . . ?
N77 N78 Fe2 176.4(2) . . ?
N2 N1 Fe1 177.6(3) . . ?
C13 C18 P2 114.93(19) . . ?
C13 C18 C17 120.2(2) . . ?
C17 C18 P2 124.9(2) . . ?
C36 C41 P62 115.26(19) . . ?
C36 C41 C40 120.2(2) . . ?
C40 C41 P62 124.4(2) . . ?
C8 C7 Si1 124.7(2) . . ?
C12 C7 Si1 117.18(19) . . ?
C12 C7 C8 118.1(3) . . ?
C18 C13 Si1 116.08(19) . . ?
C14 C13 Si1 125.6(2) . . ?
C14 C13 C18 118.3(2) . . ?
C44 C43 Si2 120.1(2) . . ?
C48 C43 Si2 123.3(2) . . ?
C48 C43 C44 116.6(2) . . ?
C6 C1 Si1 121.9(2) . . ?
C6 C1 C2 116.7(3) . . ?
C2 C1 Si1 121.4(2) . . ?
C68 C63 P62 111.22(19) . . ?
C68 C63 C64 108.2(2) . . ?
C64 C63 P62 116.2(2) . . ?
C41 C36 Si2 115.87(19) . . ?
C37 C36 Si2 125.9(2) . . ?
C37 C36 C41 118.1(2) . . ?
C67 C65 P62 112.6(2) . . ?
C67 C65 C66 111.3(2) . . ?
C66 C65 P62 113.2(2) . . ?
C16 C15 C14 120.0(3) . . ?
C9 C8 C7 121.4(3) . . ?
C45 C44 C43 121.9(3) . . ?
C26 C25 P2 111.4(2) . . ?
C26 C25 C27 110.5(3) . . ?
C27 C25 P2 115.8(2) . . ?
C50 C49 Si2 117.0(2) . . ?
C50 C49 C54 117.8(2) . . ?
C54 C49 Si2 125.2(2) . . ?
C7 C12 P1 115.7(2) . . ?
C7 C12 C11 119.8(3) . . ?
C11 C12 P1 124.4(2) . . ?
C16 C17 C18 120.1(3) . . ?
C5 C6 C1 121.6(3) . . ?
C38 C37 C36 121.6(3) . . ?
C49 C50 P55 115.2(2) . . ?
C51 C50 P55 124.4(2) . . ?
C51 C50 C49 120.3(3) . . ?
C30 C28 P2 112.61(19) . . ?
C30 C28 C29 109.4(2) . . ?
C29 C28 P2 117.0(2) . . ?
C39 C40 C41 119.9(3) . . ?
C39 C38 C37 119.7(3) . . ?
C3 C2 C1 121.8(3) . . ?
C47 C48 C43 121.7(3) . . ?
C15 C14 C13 121.4(3) . . ?
C46 C47 C48 120.2(3) . . ?
C15 C16 C17 120.1(3) . . ?
C10 C11 C12 120.9(3) . . ?
C52 C51 C50 120.4(3) . . ?
C61 C56 P55 112.0(2) . . ?
C61 C56 C57 112.0(3) . . ?
C57 C56 P55 112.7(2) . . ?
C54 C53 C52 119.5(3) . . ?
C47 C46 C45 119.5(3) . . ?
C53 C54 C49 121.5(3) . . ?
C51 C52 C53 120.5(3) . . ?
C6 C5 C4 120.2(3) . . ?
C8 C9 C10 119.7(3) . . ?
C21 C19 P1 110.9(2) . . ?
C21 C19 C20 108.8(3) . . ?
C20 C19 P1 119.3(2) . . ?
C46 C45 C44 120.1(3) . . ?
C60 C58 P55 108.54(19) . . ?
C60 C58 C59 109.4(3) . . ?
C59 C58 P55 119.1(2) . . ?
C11 C10 C9 120.0(3) . . ?
C40 C39 C38 120.5(3) . . ?
C23 C22 P1 112.4(2) . . ?
C23 C22 C24 110.2(3) . . ?
C24 C22 P1 113.7(2) . . ?
C4 C3 C2 120.3(3) . . ?
C3 C4 C5 119.3(3) . . ?
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
Fe2 P62 2.2300(7) . ?
Fe2 P55 2.2290(8) . ?
Fe2 Si2 2.3161(8) . ?
Fe2 P74 2.2621(8) . ?
Fe2 N78 1.827(2) . ?
Fe1 P2 2.2282(7) . ?
Fe1 P1 2.2398(8) . ?
Fe1 Si1 2.2986(7) . ?
Fe1 P3 2.2564(8) . ?
Fe1 N1 1.838(2) . ?
P2 C18 1.851(3) . ?
P2 C25 1.879(3) . ?
P2 C28 1.879(3) . ?
P62 C41 1.838(3) . ?
P62 C63 1.883(3) . ?
P62 C65 1.872(3) . ?
P1 C12 1.842(3) . ?
P1 C19 1.887(3) . ?
P1 C22 1.873(3) . ?
P55 C50 1.842(3) . ?
P55 C56 1.874(3) . ?
P55 C58 1.878(3) . ?
Si2 C43 1.921(3) . ?
Si2 C36 1.910(3) . ?
Si2 C49 1.898(3) . ?
Si1 C7 1.891(3) . ?
Si1 C13 1.898(3) . ?
Si1 C1 1.917(3) . ?
P3 C31 1.839(3) . ?
P3 C32 1.840(3) . ?
P3 C33 1.841(3) . ?
P74 C73 1.840(3) . ?
P74 C75 1.835(3) . ?
P74 C76 1.824(3) . ?
N78 N77 1.115(3) . ?
N1 N2 1.107(3) . ?
C18 C13 1.400(4) . ?
C18 C17 1.401(4) . ?
C41 C36 1.400(4) . ?
C41 C40 1.408(4) . ?
C7 C8 1.408(4) . ?
C7 C12 1.399(4) . ?
C13 C14 1.399(4) . ?
C43 C44 1.399(4) . ?
C43 C48 1.397(4) . ?
C1 C6 1.398(4) . ?
C1 C2 1.400(4) . ?
C63 C68 1.529(4) . ?
C63 C64 1.537(4) . ?
C36 C37 1.392(4) . ?
C65 C67 1.530(4) . ?
C65 C66 1.530(4) . ?
C15 C14 1.384(4) . ?
C15 C16 1.377(4) . ?
C8 C9 1.380(4) . ?
C44 C45 1.383(4) . ?
C25 C26 1.521(4) . ?
C25 C27 1.528(4) . ?
C49 C50 1.402(4) . ?
C49 C54 1.409(4) . ?
C12 C11 1.400(4) . ?
C17 C16 1.392(4) . ?
C6 C5 1.389(4) . ?
C37 C38 1.387(4) . ?
C50 C51 1.400(4) . ?
C28 C30 1.531(4) . ?
C28 C29 1.532(4) . ?
C40 C39 1.376(4) . ?
C38 C39 1.378(4) . ?
C2 C3 1.386(4) . ?
C48 C47 1.389(4) . ?
C47 C46 1.379(5) . ?
C11 C10 1.375(4) . ?
C51 C52 1.377(4) . ?
C56 C61 1.522(5) . ?
C56 C57 1.535(5) . ?
C53 C54 1.384(4) . ?
C53 C52 1.387(4) . ?
C46 C45 1.382(5) . ?
C5 C4 1.390(5) . ?
C9 C10 1.390(5) . ?
C19 C21 1.521(4) . ?
C19 C20 1.534(4) . ?
C60 C58 1.531(4) . ?
C58 C59 1.535(4) . ?
C22 C23 1.524(4) . ?
C22 C24 1.529(4) . ?
C3 C4 1.375(5) . ?
