Cycloaddition of carbon dioxide and epoxides catalyzed by rare earth metal complexes bearing a Trost ligand
Cheng, Jun; Lu, Chengrong; Zhao, Bei; New Journal of Chemistry 45 (2021) 13096–13103; doi:10.1039/D1NJ02460D

data_7060744
_publ_section_title
;
 Cycloaddition of carbon dioxide and epoxides catalyzed by rare earth
 metal complexes bearing a Trost ligand
;
_journal_issue                   29
_journal_name_full               'New Journal of Chemistry'
_journal_page_first              13096
_journal_page_last               13103
_journal_paper_doi               10.1039/D1NJ02460D
_journal_volume                  45
_journal_year                    2021
_chemical_absolute_configuration rmad
_chemical_formula_moiety         'C47 H53 Cl2 Lu N2 O4, 2(C4 H8 O)'
_chemical_formula_sum            'C55 H69 Cl2 Lu N2 O6'
_chemical_formula_weight         1099.99
_space_group_crystal_system      tetragonal
_space_group_IT_number           96
_space_group_name_Hall           'P 4nw 2abw'
_space_group_name_H-M_alt        'P 43 21 2'
_atom_sites_solution_hydrogens   geom
_audit_creation_date             2021-01-23
_audit_creation_method
;
Olex2 1.3
(compiled 2020.07.31 svn.rc2a77460 for OlexSys, GUI svn.r6145)
;
_audit_update_record
;
2021-04-05 deposited with the CCDC.	2021-06-14 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   12.8865(5)
_cell_length_b                   12.8865(5)
_cell_length_c                   29.8955(17)
_cell_measurement_reflns_used    9834
_cell_measurement_temperature    296.15
_cell_measurement_theta_max      23.686
_cell_measurement_theta_min      2.34
_cell_volume                     4964.5(4)
_computing_cell_refinement       'SAINT v8.37A (Bruker, 2015)'
_computing_data_reduction        'SAINT v8.37A (Bruker, 2015)'
_computing_molecular_graphics    'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2018/3 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT 2014/5 (Sheldrick, 2014)'
_diffrn_ambient_temperature      296.15
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0933
_diffrn_reflns_av_unetI/netI     0.0512
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       38
_diffrn_reflns_limit_l_min       -38
_diffrn_reflns_number            97816
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.997
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.573
_diffrn_reflns_theta_min         2.235
_diffrn_source_current           1.0
_diffrn_source_power             0.05
_diffrn_source_voltage           50.0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    2.149
_exptl_absorpt_correction_T_max  0.7456
_exptl_absorpt_correction_T_min  0.6566
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2014/5 (Bruker,2014/5) was used for absorption correction.
wR2(int) was 0.1417 before and 0.0724 after correction.
The Ratio of minimum to maximum transmission is 0.8806.
The \l/2 correction factor is Not present.
;
_exptl_crystal_colour            'clear light colourless'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   light
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.472
_exptl_crystal_description       block
_exptl_crystal_F_000             2264
_exptl_crystal_size_max          0.2
_exptl_crystal_size_mid          0.1
_exptl_crystal_size_min          0.1
_refine_diff_density_max         2.138
_refine_diff_density_min         -1.694
_refine_diff_density_rms         0.121
_refine_ls_abs_structure_details
;
 Flack x determined using 1360 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   0.019(5)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.093
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     343
_refine_ls_number_reflns         5742
_refine_ls_number_restraints     240
_refine_ls_restrained_S_all      1.106
_refine_ls_R_factor_all          0.1098
_refine_ls_R_factor_gt           0.0700
_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/[\s^2^(Fo^2^)+(0.0546P)^2^+28.9195P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1538
_refine_ls_wR_factor_ref         0.1728
_reflns_Friedel_coverage         0.717
_reflns_Friedel_fraction_full    1.000
_reflns_Friedel_fraction_max     0.995
_reflns_number_gt                4134
_reflns_number_total             5742
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d1nj02460d2.cif
_cod_data_source_block           b201113f_0m
_cod_depositor_comments
'Adding full bibliography for 7060742--7060746.cif.'
_cod_original_cell_volume        4964.5(5)
_cod_database_code               7060744
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   0.814
_shelx_estimated_absorpt_t_min   0.673
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups, All N(H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Restrained distances
 C18A-C11 = C18-C11
 1.5 with sigma of 0.01
 O3-C28 = O3-C31
 1.44 with sigma of 0.01
 O4-C24 = O4-C27
 1.44 with sigma of 0.01
 C24-C25 = C26-C27
 1.53 with sigma of 0.01
 C28-C29 = C30-C31
 1.53 with sigma of 0.02
 C25-C26
 1.54 with sigma of 0.02
 C29-C30
 1.54 with sigma of 0.02
 O4-C25 = O4-C26 = C24-C26 = C25-C27
 2.38 with sigma of 0.04
 O3-C29 = O3-C30 = C28-C30 = C29-C31
 2.38 with sigma of 0.04
 O4-C24 \\sim O4-C27
 with sigma of 0.02
 C25-C27 \\sim C24-C26
 with sigma of 0.04
 C28-C29 \\sim C29-C30 \\sim C30-C31
 with sigma of 0.02
 C24-C25 \\sim C25-C26 \\sim C26-C27
 with sigma of 0.02
 C29-C31 \\sim C28-C30
 with sigma of 0.04
 O4-C25 \\sim O4-C26
 with sigma of 0.04
3. Rigid bond restraints
 C12, C17, C16, C15, C14, C13
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.02
4. Uiso/Uaniso restraints and constraints
O3 \\sim C31 \\sim C30 \\sim C29 \\sim C28: within 2A with sigma of 0.01 and
sigma for terminal atoms of 0.02 within 2A
O4 \\sim C24 \\sim C25 \\sim C26 \\sim C27: within 2A with sigma of 0.01 and
sigma for terminal atoms of 0.02 within 2A
C12 \\sim C17 \\sim C16 \\sim C15 \\sim C14 \\sim C13: within 2A with sigma of
0.01 and sigma for terminal atoms of 0.02 within 2A
Uanis(O4) \\sim Ueq, Uanis(C24) \\sim Ueq, Uanis(C25) \\sim Ueq, Uanis(C26)
\\sim Ueq, Uanis(C27) \\sim Ueq: with sigma of 0.01 and sigma for terminal
atoms of 0.02
Uanis(C21) \\sim Ueq, Uanis(C22) \\sim Ueq, Uanis(C23) \\sim Ueq, Uanis(C18)
\\sim Ueq, Uanis(C19) \\sim Ueq, Uanis(C20) \\sim Ueq, Uanis(C22A) \\sim Ueq,
Uanis(C21A) \\sim Ueq, Uanis(C19A) \\sim Ueq, Uanis(C23A) \\sim Ueq,
Uanis(C18A) \\sim Ueq, Uanis(C20A) \\sim Ueq: with sigma of 0.01 and sigma for
terminal atoms of 0.02
5. Others
 Sof(C18A)=Sof(C19A)=Sof(H19A)=Sof(C20A)=Sof(H20A)=Sof(C21A)=Sof(H21A)=
 Sof(C22A)=Sof(H22A)=Sof(C23A)=Sof(H23A)=1-FVAR(1)
 Sof(C21)=Sof(H21)=Sof(C22)=Sof(H22)=Sof(C23)=Sof(H23)=Sof(C18)=Sof(C19)=
 Sof(H19)=Sof(C20)=Sof(H20)=FVAR(1)
 Fixed Sof: H1A(0.5) H1B(0.5) H1C(0.5) O4(0.5) C24(0.5) H24A(0.5) H24B(0.5)
 C25(0.5) H25A(0.5) H25B(0.5) C26(0.5) H26A(0.5) H26B(0.5) C27(0.5) H27A(0.5)
 H27B(0.5)
6.a Ternary CH refined with riding coordinates:
 N1(H1), C10(H10)
6.b Secondary CH2 refined with riding coordinates:
 C6(H6A,H6B), C7(H7A,H7B), C8(H8A,H8B), C9(H9A,H9B), C31(H31A,H31B), C30(H30A,
 H30B), C29(H29A,H29B), C28(H28A,H28B), C24(H24A,H24B), C25(H25A,H25B),
 C26(H26A,H26B), C27(H27A,H27B)
6.c Aromatic/amide H refined with riding coordinates:
 C3(H3), C13(H13), C14(H14), C15(H15), C16(H16), C17(H17), C21(H21), C22(H22),
 C23(H23), C19(H19), C20(H20), C19A(H19A), C20A(H20A), C21A(H21A), C22A(H22A),
 C23A(H23A)
6.d Fitted hexagon refined as free rotating group:
 C12(C13,C14,C15,C16,C17), C21(C22,C23,C18,C19,C20), C18A(C19A,C20A,C21A,C22A,
 C23A)
6.e Idealised Me refined as rotating group:
 C1(H1A,H1B,H1C)
;
_shelx_res_checksum              5892
_olex2_submission_special_instructions 'No special instructions were received'