#------------------------------------------------------------------------------
#$Date: 2025-07-06 18:43:06 +0200 (Sun 06 de Jul de 2025) $
#$Revision: 300921 $
#$URL: svn://www.crystallography.net/cod/cif/7/71/83/7718392.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_7718392
loop_
_publ_author_name
'Knott, Jackson P.'
'Hsiang, Shou-Jen'
'Hayes, Paul G.'
_publ_section_title
;
 Alkylamido lutetium complexes as prospective lutetium imido precursors:
 synthesis, characterization and ligand design.
;
_journal_issue                   15
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              6261
_journal_page_last               6273
_journal_paper_doi               10.1039/d5dt00338e
_journal_volume                  54
_journal_year                    2025
_chemical_formula_moiety         'C50 H81 Lu N4 P2 Si'
_chemical_formula_sum            'C50 H81 Lu N4 P2 Si'
_chemical_formula_weight         1003.18
_space_group_crystal_system      monoclinic
_space_group_IT_number           4
_space_group_name_Hall           'P 2yb'
_space_group_name_H-M_alt        'P 1 21 1'
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     dual
_audit_creation_date             2018-06-06
_audit_creation_method
;
Olex2 1.2
(compiled 2018.04.26 svn.r3504 for OlexSys, GUI svn.r5492)
;
_audit_update_record
;
2025-01-16 deposited with the CCDC.	2025-03-19 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 113.2891(9)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   11.59705(9)
_cell_length_b                   20.55239(15)
_cell_length_c                   11.79321(10)
_cell_measurement_reflns_used    22617
_cell_measurement_temperature    107.75(15)
_cell_measurement_theta_max      79.8870
_cell_measurement_theta_min      4.0630
_cell_volume                     2581.85(4)
_computing_cell_refinement       'CrysAlisPro 1.171.38.46 (Rigaku OD, 2015)'
_computing_data_collection       'CrysAlisPro 1.171.38.46 (Rigaku OD, 2015)'
_computing_data_reduction        'CrysAlisPro 1.171.38.46 (Rigaku OD, 2015)'
_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      107.75(15)
_diffrn_detector                 'CCD plate'
_diffrn_detector_type            'Pilatus 200/300K'
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measurement_details
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  tₑₓₚ   ω     θ     κ     φ   Frames
#--------------------------------------------------------------------------
  1  ω    -44.00  31.00   0.50    0.50    --  -38.50  19.00 150.00  150
  2  ω    -50.00  25.00   0.50    0.50    --  -38.50  57.00  30.00  150
  3  ω   -105.00 -35.00   0.50    0.50    --  -38.50 -37.00-150.00  140
  4  ω     42.00 117.00   0.50    0.50    --   47.56  19.00 -30.00  150
  5  ω    -16.00  59.00   0.50    0.50    --   47.56 -57.00 -30.00  150
  6  ω    -22.00  54.00   0.50    0.50    --   47.56 -19.00 -30.00  152
  7  ω     41.00 143.00   0.50    1.31    --  111.00 -91.00 -90.00  204
  8  ω    105.00 175.00   0.50    1.31    --  111.00  50.00  90.00  140
  9  ω     47.00 117.00   0.50    1.31    --  111.00 -50.00 120.00  140
 10  ω     47.00 117.00   0.50    1.31    --  111.00 -50.00-150.00  140
 11  ω     46.00 134.00   0.50    1.31    --  111.00 -77.00-180.00  176
 12  ω     57.00  90.00   0.50    1.31    --  111.00 -50.00 -30.00   66
 13  ω     43.00 100.00   0.50    1.31    --  111.00 -25.00 120.00  114
 14  ω     96.00 173.00   0.50    1.31    --  111.00  63.00 120.00  154
 15  ω    118.00 154.00   0.50    1.31    --  111.00 111.00  90.00   72
 16  ω    140.00 174.00   0.50    1.31    --  111.00  50.00  60.00   68
 17  ω     52.00 116.00   0.50    1.31    --  111.00-111.00  60.00  128
 18  ω     43.00 105.00   0.50    1.31    --  111.00-111.00 -60.00  124
 19  ω     55.00 100.00   0.50    1.31    --  111.00 -12.00 120.00   90
 20  ω     61.00 114.00   0.50    1.31    --  111.00 -50.00   0.00  106
 21  ω     55.00  81.00   0.50    1.31    --  111.00 -37.00   0.00   52
 22  ω     71.00 101.00   0.50    1.31    --  111.00 -63.00 -60.00   60
 23  ω     47.00  90.00   0.50    1.31    --  111.00 -50.00  90.00   86
 24  ω     91.00 117.00   0.50    1.31    --  111.00 -91.00 -30.00   52
 25  ω     71.00 133.00   0.50    1.31    --  111.00 -77.00   0.00  124
 26  ω     73.00 125.00   0.50    1.31    --  111.00 -63.00 -90.00  104
 27  ω     44.00 115.00   0.50    1.31    --  111.00 -25.00 -60.00  142
 28  ω    140.00 166.00   0.50    1.31    --  111.00  50.00 150.00   52
 29  ω    108.00 135.00   0.50    1.31    --  111.00  50.00   0.00   54
 30  ω    119.00 149.00   0.50    1.31    --  111.00 178.00-150.00   60
 31  ω     80.00 105.00   0.50    1.31    --  111.00-111.00   0.00   50
 32  ω     62.00 113.00   0.50    1.31    --  111.00 178.00-150.00  102
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at zero, Pilatus 200/300K'
_diffrn_measurement_method       'ω scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      0.0399646000
_diffrn_orient_matrix_UB_12      0.0720435000
_diffrn_orient_matrix_UB_13      0.0169823000
_diffrn_orient_matrix_UB_21      -0.0359834000
_diffrn_orient_matrix_UB_22      0.0045039000
_diffrn_orient_matrix_UB_23      0.1123242000
_diffrn_orient_matrix_UB_31      0.1341829000
_diffrn_orient_matrix_UB_32      -0.0202349000
_diffrn_orient_matrix_UB_33      0.0856189000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0398
_diffrn_reflns_av_unetI/netI     0.0430
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.997
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       25
_diffrn_reflns_limit_k_min       -26
_diffrn_reflns_limit_l_max       14
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_number            30369
_diffrn_reflns_point_group_measured_fraction_full 0.950
_diffrn_reflns_point_group_measured_fraction_max 0.924
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         80.149
_diffrn_reflns_theta_min         4.081
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    4.723
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.87929
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.38.46 (Rigaku Oxford Diffraction, 2015)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            'clear yellowish white'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   yellowish
_exptl_crystal_colour_primary    white
_exptl_crystal_density_diffrn    1.290
_exptl_crystal_description       block
_exptl_crystal_F_000             1048
_exptl_crystal_size_max          0.3
_exptl_crystal_size_mid          0.2
_exptl_crystal_size_min          0.1
_refine_diff_density_max         0.630
_refine_diff_density_min         -0.701
_refine_diff_density_rms         0.080
_refine_ls_abs_structure_details
;
 Flack x determined using 4338 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   -0.022(6)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.089
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     553
_refine_ls_number_reflns         10423
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.089
_refine_ls_R_factor_all          0.0308
_refine_ls_R_factor_gt           0.0298
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[σ²(Fo²)+(0.0258P)²+3.2072P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0755
_refine_ls_wR_factor_ref         0.0760
_reflns_Friedel_coverage         0.801
_reflns_Friedel_fraction_full    0.898
_reflns_Friedel_fraction_max     0.846
_reflns_number_gt                10128
_reflns_number_total             10423
_reflns_threshold_expression     'I > 2σ(I)'
_cod_data_source_file            d5dt00338e2.cif
_cod_data_source_block           ph18052
_cod_depositor_comments
'Adding full bibliography for 7718388--7718395.cif.'
_cod_database_code               7718392
_shelx_shelxl_version_number     2016/6
_chemical_oxdiff_formula         'C50 H79 Lu N4 P2 Si'
_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   0.650
_shelx_estimated_absorpt_t_min   0.332
_reflns_odcompleteness_completeness 98.86
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     80.95
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All N(H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2.a Ternary CH refined with riding coordinates:
 C5(H5), C23(H23), C14(H14), C45(H45), C8(H8), C32(H32), C11(H11), C48(H48)
2.b Aromatic/amide H refined with riding coordinates:
 C27(H27), C3(H3), C30(H30), C21(H21), C28(H28), C29(H29), C19(H19), C18(H18),
 C44(H44), C43(H43), C42(H42), C20(H20), C2(H2)
2.c Idealised Me refined as rotating group:
 C47(H47A,H47B,H47C), C25(H25A,H25B,H25C), C6(H6A,H6B,H6C), C13(H13A,H13B,
 H13C), C16(H16A,H16B,H16C), C12(H12A,H12B,H12C), C7(H7A,H7B,H7C), C46(H46A,
 H46B,H46C), C33(H33A,H33B,H33C), C50(H50A,H50B,H50C), C24(H24A,H24B,H24C),
 C38(H38A,H38B,H38C), C10(H10A,H10B,H10C), C15(H15A,H15B,H15C), C9(H9A,H9B,H9C),
  C49(H49A,H49B,H49C), C36(H36A,H36B,H36C), C34(H34A,H34B,H34C), C37(H37A,H37B,
 H37C)
;
_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 1.226
_oxdiff_exptl_absorpt_empirical_full_min 0.845
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, y+1/2, -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
Lu1 Lu 0.67049(2) 0.52684(2) 0.41760(2) 0.01725(7) Uani 1 1 d . . . . .
Si1 Si 0.84523(13) 0.59928(8) 0.73802(13) 0.0237(3) Uani 1 1 d . . . . .
P2 P 0.84543(11) 0.46005(7) 0.26493(11) 0.0183(2) Uani 1 1 d . . . . .
P1 P 0.52583(12) 0.65270(7) 0.21248(12) 0.0203(2) Uani 1 1 d . . . . .
N4 N 0.5643(4) 0.4625(2) 0.4898(4) 0.0228(9) Uani 1 1 d . . . . .
H4 H 0.601(7) 0.480(4) 0.566(7) 0.027 Uiso 1 1 d R . . . .
C26 C 0.4722(5) 0.6419(3) 0.4105(5) 0.0213(10) Uani 1 1 d . . . . .
N1 N 0.6766(4) 0.5528(2) 0.2318(4) 0.0197(8) Uani 1 1 d . . . . .
C17 C 0.8744(5) 0.4156(3) 0.4904(5) 0.0205(10) Uani 1 1 d . . . . .
C27 C 0.3976(5) 0.5999(3) 0.4466(5) 0.0212(10) Uani 1 1 d . . . . .
H27 H 0.387764 0.555903 0.419774 0.025 Uiso 1 1 calc R . . . .
C39 C 0.4623(5) 0.4242(3) 0.4806(5) 0.0238(11) Uani 1 1 d . . . . .
C5 C 1.0055(5) 0.4891(3) 0.3003(5) 0.0252(12) Uani 1 1 d . . . . .
H5 H 1.065335 0.459597 0.363849 0.030 Uiso 1 1 calc R . . . .
N3 N 0.8085(4) 0.4538(2) 0.3831(4) 0.0195(8) Uani 1 1 d . . . . .
C31 C 0.3441(6) 0.6863(3) 0.5575(6) 0.0221(12) Uani 1 1 d . . . . .
C47 C 0.4021(6) 0.3314(3) 0.1770(6) 0.0325(13) Uani 1 1 d . . . . .
H47A H 0.431048 0.291245 0.224724 0.049 Uiso 1 1 calc GR . . . .
H47B H 0.439614 0.334833 0.115875 0.049 Uiso 1 1 calc GR . . . .
H47C H 0.310457 0.330488 0.134560 0.049 Uiso 1 1 calc GR . . . .
C3 C 0.7092(5) 0.5450(3) 0.0549(5) 0.0236(11) Uani 1 1 d . . . . .
H3 H 0.740709 0.530614 -0.003889 0.028 Uiso 1 1 calc R . . . .
C23 C 1.0460(5) 0.3118(3) 0.8416(6) 0.0312(13) Uani 1 1 d . . . . .
H23 H 1.138436 0.320287 0.874508 0.037 Uiso 1 1 calc R . . . .
C30 C 0.3381(5) 0.6216(3) 0.5209(5) 0.0227(10) Uani 1 1 d . . . . .
H30 H 0.291847 0.591465 0.547500 0.027 Uiso 1 1 calc R . . . .
N2 N 0.5352(4) 0.6159(2) 0.3378(4) 0.0193(8) Uani 1 1 d . . . . .
C25 C 0.9969(7) 0.3407(4) 0.9337(6) 0.0401(15) Uani 1 1 d . . . . .
H25A H 0.905687 0.334898 0.902259 0.060 Uiso 1 1 calc GR . . . .
H25B H 1.017071 0.387148 0.944591 0.060 Uiso 1 1 calc GR . . . .
H25C H 1.036522 0.318365 1.013283 0.060 Uiso 1 1 calc GR . . . .
C35 C 0.8231(5) 0.5827(3) 0.5769(5) 0.0242(11) Uani 1 1 d . . . . .
C40 C 0.4197(5) 0.4194(3) 0.5774(5) 0.0242(11) Uani 1 1 d . . . . .
C6 C 1.0190(6) 0.5573(4) 0.3555(7) 0.0333(14) Uani 1 1 d . . . . .
H6A H 0.962239 0.587161 0.293847 0.050 Uiso 1 1 calc GR . . . .
H6B H 1.105798 0.572192 0.379990 0.050 Uiso 1 1 calc GR . . . .
H6C H 0.997688 0.556260 0.428000 0.050 Uiso 1 1 calc GR . . . .
C14 C 0.3673(5) 0.6658(3) 0.0964(5) 0.0275(11) Uani 1 1 d . . . . .
H14 H 0.376051 0.678390 0.018299 0.033 Uiso 1 1 calc R . . . .
C13 C 0.7420(5) 0.7237(3) 0.3300(6) 0.0297(12) Uani 1 1 d . . . . .
H13A H 0.740838 0.713541 0.410755 0.044 Uiso 1 1 calc GR . . . .
H13B H 0.788081 0.764403 0.335651 0.044 Uiso 1 1 calc GR . . . .
H13C H 0.783469 0.688378 0.304820 0.044 Uiso 1 1 calc GR . . . .
C21 C 1.0541(5) 0.3917(3) 0.6804(5) 0.0265(11) Uani 1 1 d . . . . .
H21 H 1.139476 0.399663 0.732266 0.032 Uiso 1 1 calc R . . . .
C41 C 0.3981(5) 0.3883(3) 0.3697(5) 0.0250(11) Uani 1 1 d . . . . .
C4 C 0.7392(4) 0.5202(4) 0.1739(4) 0.0205(10) Uani 1 1 d . . . . .
C16 C 0.2972(6) 0.7213(4) 0.1280(6) 0.0367(14) Uani 1 1 d . . . . .
H16A H 0.281391 0.709536 0.201177 0.055 Uiso 1 1 calc GR . . . .
H16B H 0.217032 0.728880 0.058262 0.055 Uiso 1 1 calc GR . . . .
H16C H 0.348109 0.760946 0.144921 0.055 Uiso 1 1 calc GR . . . .
C12 C 0.6048(6) 0.7596(3) 0.1133(6) 0.0333(13) Uani 1 1 d . . . . .
H12A H 0.651937 0.730947 0.080557 0.050 Uiso 1 1 calc GR . . . .
H12B H 0.643272 0.802880 0.128550 0.050 Uiso 1 1 calc GR . . . .
H12C H 0.517729 0.762907 0.053224 0.050 Uiso 1 1 calc GR . . . .
C28 C 0.4841(5) 0.7066(3) 0.4533(5) 0.0229(10) Uani 1 1 d . . . . .
H28 H 0.537093 0.735858 0.433968 0.027 Uiso 1 1 calc R . . . .
C29 C 0.4196(5) 0.7281(3) 0.5232(5) 0.0218(10) Uani 1 1 d . . . . .
H29 H 0.426898 0.772359 0.548361 0.026 Uiso 1 1 calc R . . . .
C7 C 1.0400(6) 0.4898(4) 0.1877(6) 0.0354(14) Uani 1 1 d . . . . .
H7A H 1.029200 0.446076 0.151855 0.053 Uiso 1 1 calc GR . . . .
H7B H 1.127648 0.503399 0.213102 0.053 Uiso 1 1 calc GR . . . .
H7C H 0.985248 0.520373 0.126183 0.053 Uiso 1 1 calc GR . . . .
C19 C 1.0000(5) 0.4262(3) 0.5697(5) 0.0256(11) Uani 1 1 d . . . . .
H19 H 1.048712 0.457123 0.548061 0.031 Uiso 1 1 calc R . . . .
C18 C 0.8091(5) 0.3691(3) 0.5281(5) 0.0226(10) Uani 1 1 d . . . . .
H18 H 0.724356 0.360048 0.475552 0.027 Uiso 1 1 calc R . . . .
C44 C 0.2523(5) 0.3466(3) 0.4539(6) 0.0306(13) Uani 1 1 d . . . . .
H44 H 0.180522 0.321318 0.444375 0.037 Uiso 1 1 calc R . . . .
C43 C 0.2943(5) 0.3501(3) 0.3595(5) 0.0283(12) Uani 1 1 d . . . . .
H43 H 0.251777 0.326094 0.285880 0.034 Uiso 1 1 calc R . . . .
C42 C 0.3160(6) 0.3803(4) 0.5625(7) 0.0288(15) Uani 1 1 d . . . . .
H42 H 0.288686 0.376785 0.628319 0.035 Uiso 1 1 calc R . . . .
C45 C 0.4419(5) 0.3904(3) 0.2645(5) 0.0254(11) Uani 1 1 d . . . . .
H45 H 0.535745 0.391156 0.302158 0.030 Uiso 1 1 calc R . . . .
C46 C 0.3985(6) 0.4525(4) 0.1887(6) 0.0333(13) Uani 1 1 d . . . . .
H46A H 0.439508 0.456046 0.130542 0.050 Uiso 1 1 calc GR . . . .
H46B H 0.420903 0.490237 0.244062 0.050 Uiso 1 1 calc GR . . . .
H46C H 0.307259 0.451165 0.142945 0.050 Uiso 1 1 calc GR . . . .
C33 C 0.3294(7) 0.6830(4) 0.7649(6) 0.0363(14) Uani 1 1 d . . . . .
H33A H 0.324227 0.635432 0.762269 0.054 Uiso 1 1 calc GR . . . .
H33B H 0.282664 0.700055 0.811851 0.054 Uiso 1 1 calc GR . . . .
H33C H 0.417546 0.696347 0.804882 0.054 Uiso 1 1 calc GR . . . .
C50 C 0.4106(7) 0.4690(4) 0.7741(6) 0.0381(15) Uani 1 1 d . . . . .
H50A H 0.333270 0.491128 0.720748 0.057 Uiso 1 1 calc GR . . . .
H50B H 0.458253 0.497270 0.843877 0.057 Uiso 1 1 calc GR . . . .
H50C H 0.389288 0.428433 0.805109 0.057 Uiso 1 1 calc GR . . . .
C24 C 1.0275(6) 0.2385(3) 0.8315(6) 0.0361(14) Uani 1 1 d . . . . .
H24A H 1.072774 0.218530 0.912570 0.054 Uiso 1 1 calc GR . . . .
H24B H 1.059899 0.221134 0.772440 0.054 Uiso 1 1 calc GR . . . .
H24C H 0.937815 0.228431 0.803031 0.054 Uiso 1 1 calc GR . . . .
C38 C 0.9057(6) 0.5228(6) 0.8308(5) 0.0456(16) Uani 1 1 d . . . . .
H38A H 0.846348 0.487212 0.794477 0.068 Uiso 1 1 calc GR . . . .
H38B H 0.914768 0.530076 0.916026 0.068 Uiso 1 1 calc GR . . . .
H38C H 0.987504 0.511470 0.830084 0.068 Uiso 1 1 calc GR . . . .
C1 C 0.6052(5) 0.5983(3) 0.1504(5) 0.0227(10) Uani 1 1 d . . . . .
C8 C 0.8227(5) 0.3878(3) 0.1703(5) 0.0225(10) Uani 1 1 d . . . . .
H8 H 0.834644 0.400342 0.093748 0.027 Uiso 1 1 calc R . . . .
C32 C 0.2731(5) 0.7099(3) 0.6337(5) 0.0264(11) Uani 1 1 d . . . . .
H32 H 0.281198 0.758395 0.639427 0.032 Uiso 1 1 calc R . . . .
C10 C 0.9185(6) 0.3345(3) 0.2358(6) 0.0336(13) Uani 1 1 d . . . . .
H10A H 1.003379 0.350338 0.252499 0.050 Uiso 1 1 calc GR . . . .
H10B H 0.901287 0.295870 0.182796 0.050 Uiso 1 1 calc GR . . . .
H10C H 0.912066 0.323106 0.313741 0.050 Uiso 1 1 calc GR . . . .
C15 C 0.2924(6) 0.6028(4) 0.0702(7) 0.0438(16) Uani 1 1 d . . . . .
H15A H 0.339272 0.568569 0.048965 0.066 Uiso 1 1 calc GR . . . .
H15B H 0.211385 0.609419 0.001007 0.066 Uiso 1 1 calc GR . . . .
H15C H 0.278278 0.589804 0.143614 0.066 Uiso 1 1 calc GR . . . .
C11 C 0.6071(5) 0.7313(3) 0.2345(5) 0.0245(11) Uani 1 1 d . . . . .
H11 H 0.562892 0.762663 0.268496 0.029 Uiso 1 1 calc R . . . .
C9 C 0.6879(5) 0.3627(3) 0.1316(6) 0.0290(12) Uani 1 1 d . . . . .
H9A H 0.674999 0.348154 0.204887 0.043 Uiso 1 1 calc GR . . . .
H9B H 0.673968 0.326203 0.074293 0.043 Uiso 1 1 calc GR . . . .
H9C H 0.628647 0.397775 0.091036 0.043 Uiso 1 1 calc GR . . . .
C20 C 0.8621(5) 0.3357(3) 0.6377(5) 0.0272(11) Uani 1 1 d . . . . .
H20 H 0.812723 0.305305 0.659664 0.033 Uiso 1 1 calc R . . . .
C49 C 0.6045(6) 0.4127(4) 0.7790(6) 0.0370(14) Uani 1 1 d . . . . .
H49A H 0.576107 0.372086 0.803168 0.055 Uiso 1 1 calc GR . . . .
H49B H 0.655726 0.437208 0.853162 0.055 Uiso 1 1 calc GR . . . .
H49C H 0.654656 0.402719 0.731088 0.055 Uiso 1 1 calc GR . . . .
C36 C 0.9623(6) 0.6665(4) 0.8126(7) 0.0436(17) Uani 1 1 d . . . . .
H36A H 1.042288 0.656124 0.806835 0.065 Uiso 1 1 calc GR . . . .
H36B H 0.975256 0.670582 0.899574 0.065 Uiso 1 1 calc GR . . . .
H36C H 0.929966 0.707691 0.769901 0.065 Uiso 1 1 calc GR . . . .
C34 C 0.1340(6) 0.6939(4) 0.5718(6) 0.0354(14) Uani 1 1 d . . . . .
H34A H 0.100093 0.711124 0.487421 0.053 Uiso 1 1 calc GR . . . .
H34B H 0.089696 0.713715 0.618678 0.053 Uiso 1 1 calc GR . . . .
H34C H 0.122712 0.646622 0.569436 0.053 Uiso 1 1 calc GR . . . .
C22 C 0.9871(5) 0.3459(3) 0.7175(5) 0.0249(11) Uani 1 1 d . . . . .
C37 C 0.6965(6) 0.6265(4) 0.7534(6) 0.0350(14) Uani 1 1 d . . . . .
H37A H 0.665564 0.666471 0.705596 0.053 Uiso 1 1 calc GR . . . .
H37B H 0.714106 0.634934 0.840535 0.053 Uiso 1 1 calc GR . . . .
H37C H 0.632731 0.592383 0.722220 0.053 Uiso 1 1 calc GR . . . .
C2 C 0.6234(5) 0.5954(3) 0.0405(5) 0.0254(11) Uani 1 1 d . . . . .
H2 H 0.585157 0.622240 -0.030101 0.031 Uiso 1 1 calc R . . . .
C48 C 0.4900(6) 0.4536(3) 0.7001(6) 0.0304(12) Uani 1 1 d . . . . .
H48 H 0.521978 0.495834 0.681890 0.036 Uiso 1 1 calc R . . . .
H35A H 0.838(9) 0.629(5) 0.548(9) 0.06(3) Uiso 1 1 d . . . . .
H35B H 0.897(11) 0.570(6) 0.588(10) 0.07(3) 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'
Lu Lu -6.6179 4.6937 '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
N4 Lu1 H4 22.2(18) . . ?
N4 Lu1 N1 138.41(17) . . ?
N4 Lu1 N3 102.01(17) . . ?
N4 Lu1 N2 103.65(17) . . ?
N4 Lu1 C35 110.51(19) . . ?
N1 Lu1 H4 160.2(18) . . ?
N1 Lu1 N3 72.58(16) . . ?
N1 Lu1 N2 72.72(16) . . ?
N1 Lu1 C35 111.06(18) . . ?
N3 Lu1 H4 108.7(18) . . ?
N3 Lu1 N2 145.30(15) . . ?
N2 Lu1 H4 103.9(17) . . ?
C35 Lu1 H4 88.6(18) . . ?
C35 Lu1 N3 95.92(18) . . ?
C35 Lu1 N2 96.54(18) . . ?
C35 Si1 C38 108.2(3) . . ?
C35 Si1 C36 113.3(3) . . ?
C35 Si1 C37 113.2(3) . . ?
C38 Si1 C36 107.8(4) . . ?
C38 Si1 C37 109.6(3) . . ?
C37 Si1 C36 104.7(3) . . ?
N3 P2 C5 114.8(2) . . ?
N3 P2 C4 102.7(2) . . ?
N3 P2 C8 116.2(3) . . ?
C4 P2 C5 108.0(3) . . ?
C4 P2 C8 107.5(3) . . ?
C8 P2 C5 107.1(3) . . ?
N2 P1 C14 115.8(2) . . ?
N2 P1 C1 102.8(2) . . ?
N2 P1 C11 115.8(2) . . ?
C14 P1 C11 106.5(3) . . ?
C1 P1 C14 108.4(3) . . ?
C1 P1 C11 106.9(3) . . ?
Lu1 N4 H4 92(5) . . ?
C39 N4 Lu1 154.4(4) . . ?
C39 N4 H4 111(5) . . ?
C27 C26 N2 118.3(5) . . ?
C27 C26 C28 117.1(5) . . ?
C28 C26 N2 124.5(5) . . ?
C4 N1 Lu1 126.4(4) . . ?
C4 N1 C1 106.4(4) . . ?
C1 N1 Lu1 126.6(3) . . ?
C19 C17 N3 123.8(5) . . ?
C18 C17 N3 119.4(4) . . ?
C18 C17 C19 116.5(5) . . ?
C26 C27 H27 119.5 . . ?
C30 C27 C26 121.0(5) . . ?
C30 C27 H27 119.5 . . ?
N4 C39 C40 122.3(5) . . ?
N4 C39 C41 119.0(5) . . ?
C40 C39 C41 118.7(5) . . ?
P2 C5 H5 108.3 . . ?
C6 C5 P2 108.7(4) . . ?
C6 C5 H5 108.3 . . ?
C6 C5 C7 110.1(5) . . ?
C7 C5 P2 113.2(4) . . ?
C7 C5 H5 108.3 . . ?
P2 N3 Lu1 122.1(2) . . ?
C17 N3 Lu1 111.2(3) . . ?
C17 N3 P2 125.2(4) . . ?
C30 C31 C29 117.3(6) . . ?
C30 C31 C32 121.1(6) . . ?
C29 C31 C32 121.5(6) . . ?
H47A C47 H47B 109.5 . . ?
H47A C47 H47C 109.5 . . ?
H47B C47 H47C 109.5 . . ?
C45 C47 H47A 109.5 . . ?
C45 C47 H47B 109.5 . . ?
C45 C47 H47C 109.5 . . ?
C4 C3 H3 127.0 . . ?
C2 C3 H3 127.0 . . ?
C2 C3 C4 105.9(5) . . ?
C25 C23 H23 107.4 . . ?
C24 C23 H23 107.4 . . ?
C24 C23 C25 111.0(5) . . ?
C22 C23 H23 107.4 . . ?
C22 C23 C25 110.7(5) . . ?
C22 C23 C24 112.7(5) . . ?
C27 C30 C31 121.8(5) . . ?
C27 C30 H30 119.1 . . ?
C31 C30 H30 119.1 . . ?
P1 N2 Lu1 121.3(2) . . ?
C26 N2 Lu1 118.0(3) . . ?
C26 N2 P1 120.3(4) . . ?
C23 C25 H25A 109.5 . . ?
C23 C25 H25B 109.5 . . ?
C23 C25 H25C 109.5 . . ?
H25A C25 H25B 109.5 . . ?
H25A C25 H25C 109.5 . . ?
H25B C25 H25C 109.5 . . ?
Lu1 C35 H35A 111(5) . . ?
Lu1 C35 H35B 112(7) . . ?
Si1 C35 Lu1 132.7(3) . . ?
Si1 C35 H35A 101(5) . . ?
Si1 C35 H35B 100(7) . . ?
H35A C35 H35B 93(9) . . ?
C39 C40 C48 120.5(5) . . ?
C42 C40 C39 119.7(6) . . ?
C42 C40 C48 119.7(5) . . ?
C5 C6 H6A 109.5 . . ?
C5 C6 H6B 109.5 . . ?
C5 C6 H6C 109.5 . . ?
H6A C6 H6B 109.5 . . ?
H6A C6 H6C 109.5 . . ?
H6B C6 H6C 109.5 . . ?
P1 C14 H14 106.8 . . ?
C16 C14 P1 113.7(4) . . ?
C16 C14 H14 106.8 . . ?
C15 C14 P1 110.6(4) . . ?
C15 C14 H14 106.8 . . ?
C15 C14 C16 111.6(5) . . ?
H13A C13 H13B 109.5 . . ?
H13A C13 H13C 109.5 . . ?
H13B C13 H13C 109.5 . . ?
C11 C13 H13A 109.5 . . ?
C11 C13 H13B 109.5 . . ?
C11 C13 H13C 109.5 . . ?
C19 C21 H21 118.8 . . ?
C22 C21 H21 118.8 . . ?
C22 C21 C19 122.3(5) . . ?
C39 C41 C45 120.8(5) . . ?
C43 C41 C39 119.2(5) . . ?
C43 C41 C45 120.0(5) . . ?
N1 C4 P2 114.9(4) . . ?
N1 C4 C3 110.7(5) . . ?
C3 C4 P2 134.2(4) . . ?
C14 C16 H16A 109.5 . . ?
C14 C16 H16B 109.5 . . ?
C14 C16 H16C 109.5 . . ?
H16A C16 H16B 109.5 . . ?
H16A C16 H16C 109.5 . . ?
H16B C16 H16C 109.5 . . ?
H12A C12 H12B 109.5 . . ?
H12A C12 H12C 109.5 . . ?
H12B C12 H12C 109.5 . . ?
C11 C12 H12A 109.5 . . ?
C11 C12 H12B 109.5 . . ?
C11 C12 H12C 109.5 . . ?
C26 C28 H28 119.5 . . ?
C29 C28 C26 121.0(5) . . ?
C29 C28 H28 119.5 . . ?
C31 C29 H29 119.2 . . ?
C28 C29 C31 121.5(5) . . ?
C28 C29 H29 119.2 . . ?
C5 C7 H7A 109.5 . . ?
C5 C7 H7B 109.5 . . ?
C5 C7 H7C 109.5 . . ?
H7A C7 H7B 109.5 . . ?
H7A C7 H7C 109.5 . . ?
H7B C7 H7C 109.5 . . ?
C17 C19 H19 119.7 . . ?
C21 C19 C17 120.5(5) . . ?
C21 C19 H19 119.7 . . ?
C17 C18 H18 118.6 . . ?
C20 C18 C17 122.9(5) . . ?
C20 C18 H18 118.6 . . ?
C43 C44 H44 120.3 . . ?
C43 C44 C42 119.3(5) . . ?
C42 C44 H44 120.3 . . ?
C41 C43 H43 119.2 . . ?
C44 C43 C41 121.6(5) . . ?
C44 C43 H43 119.2 . . ?
C40 C42 H42 119.3 . . ?
C44 C42 C40 121.4(6) . . ?
C44 C42 H42 119.3 . . ?
C47 C45 H45 107.2 . . ?
C41 C45 C47 114.7(5) . . ?
C41 C45 H45 107.2 . . ?
C41 C45 C46 111.3(5) . . ?
C46 C45 C47 108.9(5) . . ?
C46 C45 H45 107.2 . . ?
C45 C46 H46A 109.5 . . ?
C45 C46 H46B 109.5 . . ?
C45 C46 H46C 109.5 . . ?
H46A C46 H46B 109.5 . . ?
H46A C46 H46C 109.5 . . ?
H46B C46 H46C 109.5 . . ?
H33A C33 H33B 109.5 . . ?
H33A C33 H33C 109.5 . . ?
H33B C33 H33C 109.5 . . ?
C32 C33 H33A 109.5 . . ?
C32 C33 H33B 109.5 . . ?
C32 C33 H33C 109.5 . . ?
H50A C50 H50B 109.5 . . ?
H50A C50 H50C 109.5 . . ?
H50B C50 H50C 109.5 . . ?
C48 C50 H50A 109.5 . . ?
C48 C50 H50B 109.5 . . ?
C48 C50 H50C 109.5 . . ?
C23 C24 H24A 109.5 . . ?
C23 C24 H24B 109.5 . . ?
C23 C24 H24C 109.5 . . ?
H24A C24 H24B 109.5 . . ?
H24A C24 H24C 109.5 . . ?
H24B C24 H24C 109.5 . . ?
Si1 C38 H38A 109.5 . . ?
Si1 C38 H38B 109.5 . . ?
Si1 C38 H38C 109.5 . . ?
H38A C38 H38B 109.5 . . ?
H38A C38 H38C 109.5 . . ?
H38B C38 H38C 109.5 . . ?
N1 C1 P1 114.3(4) . . ?
N1 C1 C2 110.7(5) . . ?
C2 C1 P1 134.6(4) . . ?
P2 C8 H8 107.9 . . ?
C10 C8 P2 112.1(4) . . ?
C10 C8 H8 107.9 . . ?
C9 C8 P2 110.0(4) . . ?
C9 C8 H8 107.9 . . ?
C9 C8 C10 111.1(5) . . ?
C31 C32 C33 111.7(5) . . ?
C31 C32 H32 107.5 . . ?
C31 C32 C34 111.5(5) . . ?
C33 C32 H32 107.5 . . ?
C34 C32 C33 110.8(5) . . ?
C34 C32 H32 107.5 . . ?
C8 C10 H10A 109.5 . . ?
C8 C10 H10B 109.5 . . ?
C8 C10 H10C 109.5 . . ?
H10A C10 H10B 109.5 . . ?
H10A C10 H10C 109.5 . . ?
H10B C10 H10C 109.5 . . ?
C14 C15 H15A 109.5 . . ?
C14 C15 H15B 109.5 . . ?
C14 C15 H15C 109.5 . . ?
H15A C15 H15B 109.5 . . ?
H15A C15 H15C 109.5 . . ?
H15B C15 H15C 109.5 . . ?
P1 C11 H11 107.9 . . ?
C13 C11 P1 109.4(4) . . ?
C13 C11 C12 111.1(5) . . ?
C13 C11 H11 107.9 . . ?
C12 C11 P1 112.5(4) . . ?
C12 C11 H11 107.9 . . ?
C8 C9 H9A 109.5 . . ?
C8 C9 H9B 109.5 . . ?
C8 C9 H9C 109.5 . . ?
H9A C9 H9B 109.5 . . ?
H9A C9 H9C 109.5 . . ?
H9B C9 H9C 109.5 . . ?
C18 C20 H20 119.4 . . ?
C18 C20 C22 121.2(5) . . ?
C22 C20 H20 119.4 . . ?
H49A C49 H49B 109.5 . . ?
H49A C49 H49C 109.5 . . ?
H49B C49 H49C 109.5 . . ?
C48 C49 H49A 109.5 . . ?
C48 C49 H49B 109.5 . . ?
C48 C49 H49C 109.5 . . ?
Si1 C36 H36A 109.5 . . ?
Si1 C36 H36B 109.5 . . ?
Si1 C36 H36C 109.5 . . ?
H36A C36 H36B 109.5 . . ?
H36A C36 H36C 109.5 . . ?
H36B C36 H36C 109.5 . . ?
C32 C34 H34A 109.5 . . ?
C32 C34 H34B 109.5 . . ?
C32 C34 H34C 109.5 . . ?
H34A C34 H34B 109.5 . . ?
H34A C34 H34C 109.5 . . ?
H34B C34 H34C 109.5 . . ?
C21 C22 C23 121.2(5) . . ?
C20 C22 C23 122.2(5) . . ?
C20 C22 C21 116.6(5) . . ?
Si1 C37 H37A 109.5 . . ?
Si1 C37 H37B 109.5 . . ?
Si1 C37 H37C 109.5 . . ?
H37A C37 H37B 109.5 . . ?
H37A C37 H37C 109.5 . . ?
H37B C37 H37C 109.5 . . ?
C3 C2 H2 126.9 . . ?
C1 C2 C3 106.3(5) . . ?
C1 C2 H2 126.9 . . ?
C40 C48 C50 114.8(5) . . ?
C40 C48 C49 109.5(5) . . ?
C40 C48 H48 107.5 . . ?
C50 C48 C49 109.8(5) . . ?
C50 C48 H48 107.5 . . ?
C49 C48 H48 107.5 . . ?
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
Lu1 N4 2.195(4) . ?
Lu1 H4 2.40(7) . ?
Lu1 N1 2.283(4) . ?
Lu1 N3 2.344(4) . ?
Lu1 N2 2.351(4) . ?
Lu1 C35 2.314(5) . ?
Si1 C35 1.845(5) . ?
Si1 C38 1.884(10) . ?
Si1 C36 1.893(7) . ?
Si1 C37 1.889(6) . ?
P2 C5 1.834(6) . ?
P2 N3 1.617(4) . ?
P2 C4 1.775(7) . ?
P2 C8 1.813(6) . ?
P1 N2 1.626(5) . ?
P1 C14 1.826(6) . ?
P1 C1 1.779(6) . ?
P1 C11 1.837(6) . ?
N4 H4 0.91(8) . ?
N4 C39 1.389(7) . ?
C26 C27 1.402(8) . ?
C26 N2 1.431(7) . ?
C26 C28 1.410(8) . ?
N1 C4 1.355(7) . ?
N1 C1 1.361(7) . ?
C17 N3 1.429(7) . ?
C17 C19 1.402(7) . ?
C17 C18 1.396(8) . ?
C27 H27 0.9500 . ?
C27 C30 1.386(7) . ?
C39 C40 1.416(8) . ?
C39 C41 1.429(8) . ?
C5 H5 1.0000 . ?
C5 C6 1.527(8) . ?
C5 C7 1.531(8) . ?
C31 C30 1.391(9) . ?
C31 C29 1.395(9) . ?
C31 C32 1.519(8) . ?
C47 H47A 0.9800 . ?
C47 H47B 0.9800 . ?
C47 H47C 0.9800 . ?
C47 C45 1.540(8) . ?
C3 H3 0.9500 . ?
C3 C4 1.402(7) . ?
C3 C2 1.399(8) . ?
C23 H23 1.0000 . ?
C23 C25 1.532(9) . ?
C23 C24 1.521(10) . ?
C23 C22 1.519(8) . ?
C30 H30 0.9500 . ?
C25 H25A 0.9800 . ?
C25 H25B 0.9800 . ?
C25 H25C 0.9800 . ?
C35 H35A 1.06(11) . ?
C35 H35B 0.86(12) . ?
C40 C42 1.398(9) . ?
C40 C48 1.523(8) . ?
C6 H6A 0.9800 . ?
C6 H6B 0.9800 . ?
C6 H6C 0.9800 . ?
C14 H14 1.0000 . ?
C14 C16 1.529(9) . ?
C14 C15 1.522(10) . ?
C13 H13A 0.9800 . ?
C13 H13B 0.9800 . ?
C13 H13C 0.9800 . ?
C13 C11 1.532(8) . ?
C21 H21 0.9500 . ?
C21 C19 1.397(8) . ?
C21 C22 1.397(8) . ?
C41 C43 1.401(8) . ?
C41 C45 1.516(8) . ?
C16 H16A 0.9800 . ?
C16 H16B 0.9800 . ?
C16 H16C 0.9800 . ?
C12 H12A 0.9800 . ?
C12 H12B 0.9800 . ?
C12 H12C 0.9800 . ?
C12 C11 1.534(8) . ?
C28 H28 0.9500 . ?
C28 C29 1.387(7) . ?
C29 H29 0.9500 . ?
C7 H7A 0.9800 . ?
C7 H7B 0.9800 . ?
C7 H7C 0.9800 . ?
C19 H19 0.9500 . ?
C18 H18 0.9500 . ?
C18 C20 1.375(8) . ?
C44 H44 0.9500 . ?
C44 C43 1.382(9) . ?
C44 C42 1.385(10) . ?
C43 H43 0.9500 . ?
C42 H42 0.9500 . ?
C45 H45 1.0000 . ?
C45 C46 1.526(9) . ?
C46 H46A 0.9800 . ?
C46 H46B 0.9800 . ?
C46 H46C 0.9800 . ?
C33 H33A 0.9800 . ?
C33 H33B 0.9800 . ?
C33 H33C 0.9800 . ?
C33 C32 1.526(8) . ?
C50 H50A 0.9800 . ?
C50 H50B 0.9800 . ?
C50 H50C 0.9800 . ?
C50 C48 1.532(8) . ?
C24 H24A 0.9800 . ?
C24 H24B 0.9800 . ?
C24 H24C 0.9800 . ?
C38 H38A 0.9800 . ?
C38 H38B 0.9800 . ?
C38 H38C 0.9800 . ?
C1 C2 1.395(7) . ?
C8 H8 1.0000 . ?
C8 C10 1.534(8) . ?
C8 C9 1.534(7) . ?
C32 H32 1.0000 . ?
C32 C34 1.521(8) . ?
C10 H10A 0.9800 . ?
C10 H10B 0.9800 . ?
C10 H10C 0.9800 . ?
C15 H15A 0.9800 . ?
C15 H15B 0.9800 . ?
C15 H15C 0.9800 . ?
C11 H11 1.0000 . ?
C9 H9A 0.9800 . ?
C9 H9B 0.9800 . ?
C9 H9C 0.9800 . ?
C20 H20 0.9500 . ?
C20 C22 1.397(8) . ?
C49 H49A 0.9800 . ?
C49 H49B 0.9800 . ?
C49 H49C 0.9800 . ?
C49 C48 1.535(9) . ?
C36 H36A 0.9800 . ?
C36 H36B 0.9800 . ?
C36 H36C 0.9800 . ?
C34 H34A 0.9800 . ?
C34 H34B 0.9800 . ?
C34 H34C 0.9800 . ?
C37 H37A 0.9800 . ?
C37 H37B 0.9800 . ?
C37 H37C 0.9800 . ?
C2 H2 0.9500 . ?
C48 H48 1.0000 . ?
