#------------------------------------------------------------------------------
#$Date: 2024-07-05 19:25:06 +0300 (Fri, 05 Jul 2024) $
#$Revision: 293068 $
#$URL: file:///home/coder/svn-repositories/cod/cif/7/71/62/7716224.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_7716224
loop_
_publ_author_name
'You, Shuhao'
'Shi, Wenyu'
'Ouyang, Ruoxue'
'Wang, Yang'
'Shi, Xiaochao'
_publ_section_title
;
 Synthesis of bis(oxazoline)-based rare-earth metal complexes and their
 catalytic performance in the polymerization of isoprene and polar
 ortho-methoxystyrene.
;
_journal_issue                   25
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              10563
_journal_page_last               10570
_journal_paper_doi               10.1039/d4dt01036a
_journal_volume                  53
_journal_year                    2024
_chemical_formula_moiety         'C29 H49 Lu N2 O3 Si2'
_chemical_formula_sum            'C29 H52 Lu N2 O3 Si2'
_chemical_formula_weight         707.87
_chemical_name_systematic        Ph-Box-Lu
_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   geom
_atom_sites_solution_primary     iterative
_audit_creation_date             2023-07-12
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_audit_update_record
;
2024-04-07 deposited with the CCDC.	2024-05-29 downloaded from the CCDC.
;
_cell_angle_alpha                92.6780(10)
_cell_angle_beta                 100.7490(10)
_cell_angle_gamma                112.1510(10)
_cell_formula_units_Z            2
_cell_length_a                   10.3467(4)
_cell_length_b                   11.7319(4)
_cell_length_c                   14.9386(5)
_cell_measurement_reflns_used    9284
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      27.48
_cell_measurement_theta_min      2.25
_cell_volume                     1636.33(10)
_computing_cell_refinement       'SAINT V8.40B (?, 2016)'
_computing_data_reduction        'SAINT V8.40B (?, 2016)'
_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_temperature      150.0
_diffrn_measured_fraction_theta_full 0.985
_diffrn_measured_fraction_theta_max 0.986
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       'φ and ω scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0483
_diffrn_reflns_av_unetI/netI     0.0359
_diffrn_reflns_Laue_measured_fraction_full 0.985
_diffrn_reflns_Laue_measured_fraction_max 0.986
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            47958
_diffrn_reflns_point_group_measured_fraction_full 0.985
_diffrn_reflns_point_group_measured_fraction_max 0.986
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.504
_diffrn_reflns_theta_min         2.202
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    3.119
_exptl_absorpt_correction_T_max  0.7456
_exptl_absorpt_correction_T_min  0.5446
_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    1.437
_exptl_crystal_description       block
_exptl_crystal_F_000             726
_exptl_crystal_size_max          0.3
_exptl_crystal_size_mid          0.1
_exptl_crystal_size_min          0.1
_refine_diff_density_max         0.856
_refine_diff_density_min         -0.822
_refine_diff_density_rms         0.082
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.963
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     344
_refine_ls_number_reflns         7444
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.963
_refine_ls_R_factor_all          0.0181
_refine_ls_R_factor_gt           0.0176
_refine_ls_shift/su_max          0.004
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[σ²(Fo²)+(0.0359P)²+0.4621P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0521
_refine_ls_wR_factor_ref         0.0524
_reflns_Friedel_coverage         0.000
_reflns_number_gt                7298
_reflns_number_total             7444
_reflns_threshold_expression     'I > 2σ(I)'
_cod_data_source_file            d4dt01036a2.cif
_cod_data_source_block           ph-box-lu-20230711
_cod_depositor_comments
'Adding full bibliography for 7716223--7716225.cif.'
_cod_database_code               7716224
_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   0.746
_shelx_estimated_absorpt_t_min   0.455
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2.a Secondary CH2 refined with riding coordinates:
 C9(H9A,H9B), C14(H14A,H14B), C22(H22A,H22B), C26(H26A,H26B), C27(H27A,H27B),
 C28(H28A,H28B), C29(H29A,H29B)
2.b Aromatic/amide H refined with riding coordinates:
 C1(H1), C2(H2), C4(H4), C5(H5), C6(H6)
2.c Idealised Me refined as rotating group:
 C11(H11A,H11B,H11C), C12(H12A,H12B,H12C), C16(H16A,H16B,H16C), C17(H17A,H17B,
 H17C), C19(H19A,H19B,H19C), C20(H20A,H20B,H20C), C21(H21A,H21B,H21C), C23(H23A,
 H23B,H23C), C24(H24A,H24B,H24C), C25(H25A,H25B,H25C)
;
_olex2_submission_special_instructions 'No special instructions were received'
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
Lu1 Lu 0.51996(2) 0.80453(2) 0.73923(2) 0.01702(4) Uani 1 1 d . . . . .
Si1 Si 0.31936(6) 0.59905(5) 0.88644(4) 0.02465(10) Uani 1 1 d . . . . .
Si2 Si 0.84629(6) 1.09590(5) 0.83095(4) 0.02710(11) Uani 1 1 d . . . . .
O1 O 0.58611(16) 0.45801(13) 0.69148(10) 0.0262(3) Uani 1 1 d . . . . .
O2 O 0.20614(15) 0.51922(12) 0.51336(10) 0.0255(3) Uani 1 1 d . . . . .
O3 O 0.41479(17) 0.95026(14) 0.75618(11) 0.0293(3) Uani 1 1 d . . . . .
N1 N 0.60956(17) 0.65695(15) 0.71633(11) 0.0196(3) Uani 1 1 d . . . . .
N2 N 0.36195(15) 0.69672(13) 0.60354(10) 0.0183(3) Uani 1 1 d . . . . .
C1 C 0.1233(2) 0.16601(19) 0.60160(16) 0.0339(4) Uani 1 1 d . . . . .
H1 H 0.041336 0.121475 0.624700 0.041 Uiso 1 1 calc R . . . .
C2 C 0.1921(2) 0.29315(18) 0.62483(14) 0.0278(4) Uani 1 1 d . . . . .
H2 H 0.156948 0.335289 0.663746 0.033 Uiso 1 1 calc R . . . .
C3 C 0.31256(19) 0.36019(15) 0.59178(12) 0.0208(3) Uani 1 1 d . . . . .
C4 C 0.3611(2) 0.29639(18) 0.53418(13) 0.0270(4) Uani 1 1 d . . . . .
H4 H 0.442635 0.340676 0.510673 0.032 Uiso 1 1 calc R . . . .
C5 C 0.2917(2) 0.16901(19) 0.51073(15) 0.0313(4) Uani 1 1 d . . . . .
H5 H 0.325649 0.126674 0.471091 0.038 Uiso 1 1 calc R . . . .
C6 C 0.1731(2) 0.10315(18) 0.54483(16) 0.0331(5) Uani 1 1 d . . . . .
H6 H 0.126263 0.015665 0.529431 0.040 Uiso 1 1 calc R . . . .
C7 C 0.38857(19) 0.49712(15) 0.61954(12) 0.0198(3) Uani 1 1 d . . . . .
C8 C 0.52707(19) 0.54311(16) 0.67644(12) 0.0194(3) Uani 1 1 d . . . . .
C9 C 0.7160(2) 0.51850(18) 0.76043(14) 0.0293(4) Uani 1 1 d . . . . .
H9A H 0.793043 0.494644 0.746687 0.035 Uiso 1 1 calc R . . . .
H9B H 0.700772 0.497063 0.822014 0.035 Uiso 1 1 calc R . . . .
C10 C 0.75312(19) 0.65691(17) 0.75562(13) 0.0230(3) Uani 1 1 d . . . . .
C11 C 0.8188(2) 0.7315(2) 0.85039(14) 0.0314(4) Uani 1 1 d . . . . .
H11A H 0.831121 0.817960 0.846370 0.047 Uiso 1 1 calc GR . . . .
H11B H 0.912176 0.728097 0.873735 0.047 Uiso 1 1 calc GR . . . .
H11C H 0.755607 0.696487 0.892196 0.047 Uiso 1 1 calc GR . . . .
C12 C 0.8510(2) 0.7033(2) 0.68887(15) 0.0321(4) Uani 1 1 d . . . . .
H12A H 0.810340 0.647805 0.630692 0.048 Uiso 1 1 calc GR . . . .
H12B H 0.945737 0.704566 0.715307 0.048 Uiso 1 1 calc GR . . . .
H12C H 0.859912 0.787318 0.677747 0.048 Uiso 1 1 calc GR . . . .
C13 C 0.32517(18) 0.57553(16) 0.58312(12) 0.0191(3) Uani 1 1 d . . . . .
C14 C 0.1875(2) 0.61731(18) 0.46573(14) 0.0309(4) Uani 1 1 d . . . . .
H14A H 0.084630 0.599793 0.443834 0.037 Uiso 1 1 calc R . . . .
H14B H 0.233354 0.628219 0.412453 0.037 Uiso 1 1 calc R . . . .
C15 C 0.26017(19) 0.73242(16) 0.53736(12) 0.0211(3) Uani 1 1 d . . . . .
C16 C 0.3407(2) 0.84655(19) 0.49542(14) 0.0316(4) Uani 1 1 d . . . . .
H16A H 0.395076 0.916228 0.544211 0.047 Uiso 1 1 calc GR . . . .
H16B H 0.272413 0.867904 0.452028 0.047 Uiso 1 1 calc GR . . . .
H16C H 0.406611 0.829088 0.463006 0.047 Uiso 1 1 calc GR . . . .
C17 C 0.1500(2) 0.7522(2) 0.58389(15) 0.0303(4) Uani 1 1 d . . . . .
H17A H 0.095280 0.675092 0.606107 0.045 Uiso 1 1 calc GR . . . .
H17B H 0.084892 0.775920 0.539688 0.045 Uiso 1 1 calc GR . . . .
H17C H 0.198892 0.818208 0.635850 0.045 Uiso 1 1 calc GR . . . .
C18 C 0.7330(2) 0.97426(16) 0.73389(13) 0.0244(3) Uani 1 1 d . . . . .
C19 C 0.7764(3) 1.0717(2) 0.93890(17) 0.0410(5) Uani 1 1 d . . . . .
H19A H 0.681410 1.074605 0.928071 0.062 Uiso 1 1 calc GR . . . .
H19B H 0.841661 1.137260 0.988263 0.062 Uiso 1 1 calc GR . . . .
H19C H 0.769811 0.990696 0.956707 0.062 Uiso 1 1 calc GR . . . .
C20 C 1.0332(2) 1.1007(3) 0.8613(2) 0.0508(6) Uani 1 1 d . . . . .
H20A H 1.090561 1.166903 0.912035 0.076 Uiso 1 1 calc GR . . . .
H20B H 1.076375 1.116740 0.807698 0.076 Uiso 1 1 calc GR . . . .
H20C H 1.029922 1.020815 0.879936 0.076 Uiso 1 1 calc GR . . . .
C21 C 0.8639(3) 1.2545(2) 0.80236(19) 0.0464(6) Uani 1 1 d . . . . .
H21A H 0.769739 1.259093 0.791637 0.070 Uiso 1 1 calc GR . . . .
H21B H 0.902319 1.270216 0.746881 0.070 Uiso 1 1 calc GR . . . .
H21C H 0.928945 1.317025 0.853639 0.070 Uiso 1 1 calc GR . . . .
C22 C 0.4724(2) 0.74282(18) 0.88167(13) 0.0264(4) Uani 1 1 d . . . . .
H22A H 0.559387 0.735746 0.917064 0.032 Uiso 1 1 calc R . . . .
H22B H 0.460170 0.811629 0.915133 0.032 Uiso 1 1 calc R . . . .
C23 C 0.3634(3) 0.4596(2) 0.87087(16) 0.0366(5) Uani 1 1 d . . . . .
H23A H 0.285202 0.385990 0.881602 0.055 Uiso 1 1 calc GR . . . .
H23B H 0.452021 0.471669 0.914743 0.055 Uiso 1 1 calc GR . . . .
H23C H 0.375891 0.448200 0.808113 0.055 Uiso 1 1 calc GR . . . .
C24 C 0.1596(2) 0.5787(2) 0.79327(17) 0.0396(5) Uani 1 1 d . . . . .
H24A H 0.138977 0.653480 0.796889 0.059 Uiso 1 1 calc GR . . . .
H24B H 0.076628 0.507073 0.801229 0.059 Uiso 1 1 calc GR . . . .
H24C H 0.180049 0.564793 0.733168 0.059 Uiso 1 1 calc GR . . . .
C25 C 0.2588(3) 0.5952(3) 0.99723(18) 0.0462(6) Uani 1 1 d . . . . .
H25A H 0.220571 0.659267 1.003377 0.069 Uiso 1 1 calc GR . . . .
H25B H 0.340069 0.610909 1.048663 0.069 Uiso 1 1 calc GR . . . .
H25C H 0.184053 0.513515 0.997643 0.069 Uiso 1 1 calc GR . . . .
C26 C 0.4524(3) 1.0691(2) 0.72072(16) 0.0357(5) Uani 1 1 d . . . . .
H26A H 0.385926 1.061676 0.661704 0.043 Uiso 1 1 calc R . . . .
H26B H 0.551086 1.098617 0.710612 0.043 Uiso 1 1 calc R . . . .
C27 C 0.4411(4) 1.1577(3) 0.7926(3) 0.0556(8) Uani 1 1 d . . . . .
H27A H 0.376840 1.197662 0.765256 0.067 Uiso 1 1 calc R . . . .
H27B H 0.536367 1.223079 0.820454 0.067 Uiso 1 1 calc R . . . .
C28 C 0.3796(3) 1.0779(3) 0.86475(19) 0.0515(7) Uani 1 1 d . . . . .
H28A H 0.455634 1.086708 0.919001 0.062 Uiso 1 1 calc R . . . .
H28B H 0.305509 1.100537 0.884908 0.062 Uiso 1 1 calc R . . . .
C29 C 0.3170(3) 0.9508(2) 0.8154(2) 0.0449(6) Uani 1 1 d . . . . .
H29A H 0.311495 0.889015 0.859038 0.054 Uiso 1 1 calc R . . . .
H29B H 0.219745 0.931805 0.778365 0.054 Uiso 1 1 calc R . . . .
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 '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 -0.4720 5.8584 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Si Si 0.0817 0.0704 '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
N1 Lu1 O3 176.60(5) . . ?
N1 Lu1 N2 81.26(5) . . ?
N1 Lu1 C18 94.80(6) . . ?
N1 Lu1 C22 92.53(6) . . ?
N2 Lu1 O3 95.43(5) . . ?
N2 Lu1 C18 119.43(6) . . ?
N2 Lu1 C22 120.33(6) . . ?
C18 Lu1 O3 87.52(6) . . ?
C22 Lu1 O3 88.45(6) . . ?
C22 Lu1 C18 120.21(7) . . ?
C22 Si1 C23 111.20(10) . . ?
C22 Si1 C24 110.77(9) . . ?
C22 Si1 C25 113.71(11) . . ?
C23 Si1 C24 107.83(11) . . ?
C23 Si1 C25 106.87(11) . . ?
C25 Si1 C24 106.13(13) . . ?
C18 Si2 C19 112.96(10) . . ?
C18 Si2 C20 111.61(12) . . ?
C18 Si2 C21 111.55(11) . . ?
C19 Si2 C20 106.09(13) . . ?
C21 Si2 C19 107.84(13) . . ?
C21 Si2 C20 106.40(13) . . ?
C8 O1 C9 106.43(14) . . ?
C13 O2 C14 105.88(14) . . ?
C26 O3 Lu1 126.36(13) . . ?
C26 O3 C29 104.85(17) . . ?
C29 O3 Lu1 128.14(14) . . ?
C8 N1 Lu1 122.24(12) . . ?
C8 N1 C10 106.93(14) . . ?
C10 N1 Lu1 129.80(11) . . ?
C13 N2 Lu1 121.17(11) . . ?
C13 N2 C15 107.15(14) . . ?
C15 N2 Lu1 130.14(11) . . ?
C2 C1 C6 120.4(2) . . ?
C1 C2 C3 120.72(19) . . ?
C2 C3 C7 120.22(16) . . ?
C4 C3 C2 118.49(17) . . ?
C4 C3 C7 121.28(17) . . ?
C5 C4 C3 120.73(19) . . ?
C6 C5 C4 120.3(2) . . ?
C5 C6 C1 119.41(18) . . ?
C8 C7 C3 118.60(15) . . ?
C13 C7 C3 119.15(15) . . ?
C13 C7 C8 122.08(15) . . ?
O1 C8 C7 115.32(15) . . ?
N1 C8 O1 114.84(16) . . ?
N1 C8 C7 129.83(16) . . ?
O1 C9 C10 104.15(14) . . ?
N1 C10 C9 101.33(14) . . ?
N1 C10 C11 112.29(15) . . ?
N1 C10 C12 109.63(15) . . ?
C11 C10 C9 111.19(16) . . ?
C11 C10 C12 111.68(17) . . ?
C12 C10 C9 110.25(16) . . ?
O2 C13 C7 114.95(15) . . ?
N2 C13 O2 114.21(15) . . ?
N2 C13 C7 130.83(16) . . ?
O2 C14 C15 104.39(15) . . ?
N2 C15 C14 102.03(14) . . ?
N2 C15 C16 110.75(15) . . ?
N2 C15 C17 110.69(14) . . ?
C16 C15 C14 111.60(16) . . ?
C16 C15 C17 111.57(16) . . ?
C17 C15 C14 109.82(17) . . ?
Si2 C18 Lu1 125.37(9) . . ?
Si1 C22 Lu1 120.60(9) . . ?
O3 C26 C27 106.1(2) . . ?
C26 C27 C28 105.3(2) . . ?
C29 C28 C27 103.1(2) . . ?
O3 C29 C28 104.6(2) . . ?
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 O3 2.3741(14) . ?
Lu1 N1 2.2907(16) . ?
Lu1 N2 2.3122(14) . ?
Lu1 C18 2.3669(18) . ?
Lu1 C22 2.3581(19) . ?
Si1 C22 1.843(2) . ?
Si1 C23 1.872(2) . ?
Si1 C24 1.881(2) . ?
Si1 C25 1.873(2) . ?
Si2 C18 1.8503(19) . ?
Si2 C19 1.878(3) . ?
Si2 C20 1.880(3) . ?
Si2 C21 1.878(2) . ?
O1 C8 1.360(2) . ?
O1 C9 1.438(2) . ?
O2 C13 1.372(2) . ?
O2 C14 1.436(2) . ?
O3 C26 1.453(3) . ?
O3 C29 1.464(3) . ?
N1 C8 1.320(2) . ?
N1 C10 1.492(2) . ?
N2 C13 1.329(2) . ?
N2 C15 1.498(2) . ?
C1 C2 1.382(3) . ?
C1 C6 1.386(3) . ?
C2 C3 1.394(3) . ?
C3 C4 1.392(3) . ?
C3 C7 1.495(2) . ?
C4 C5 1.385(3) . ?
C5 C6 1.385(3) . ?
C7 C8 1.410(2) . ?
C7 C13 1.393(2) . ?
C9 C10 1.530(3) . ?
C10 C11 1.519(3) . ?
C10 C12 1.526(3) . ?
C14 C15 1.527(3) . ?
C15 C16 1.520(3) . ?
C15 C17 1.522(3) . ?
C26 C27 1.512(4) . ?
C27 C28 1.531(5) . ?
C28 C29 1.476(4) . ?
