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_7060746
_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 unk
_chemical_formula_moiety         'C47 H53 Cl2 N2 O4 Sm'
_chemical_formula_sum            'C47 H51 Cl2 N2 O4 Sm'
_chemical_formula_weight         929.15
_space_group_crystal_system      orthorhombic
_space_group_IT_number           19
_space_group_name_Hall           'P 2ac 2ab'
_space_group_name_H-M_alt        'P 21 21 21'
_atom_sites_solution_hydrogens   mixed
_audit_creation_date             2021-01-30
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_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                   12.9665(12)
_cell_length_b                   12.9771(12)
_cell_length_c                   30.056(3)
_cell_measurement_reflns_used    9991
_cell_measurement_temperature    296.15
_cell_measurement_theta_max      20.54
_cell_measurement_theta_min      2.32
_cell_volume                     5057.4(8)
_computing_cell_refinement       'SAINT v8.37A (Bruker, 2015)'
_computing_data_reduction        'SAINT v8.37A (Bruker, 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 2014/5 (Sheldrick, 2014)'
_diffrn_ambient_temperature      296.15
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_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  0.1725
_diffrn_reflns_av_unetI/netI     0.0858
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       36
_diffrn_reflns_limit_l_min       -36
_diffrn_reflns_number            139369
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         25.677
_diffrn_reflns_theta_min         2.220
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    1.305
_exptl_absorpt_correction_T_max  0.7456
_exptl_absorpt_correction_T_min  0.6814
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2014/5 (Bruker,2014/5) was used for absorption correction.
wR2(int) was 0.1812 before and 0.0765 after correction.
The Ratio of minimum to maximum transmission is 0.9139.
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    1.220
_exptl_crystal_description       block
_exptl_crystal_F_000             1900
_exptl_crystal_size_max          0.3
_exptl_crystal_size_mid          0.2
_exptl_crystal_size_min          0.2
_refine_diff_density_max         2.734
_refine_diff_density_min         -2.492
_refine_diff_density_rms         0.162
_refine_ls_abs_structure_details
;
 Flack x determined using 2119 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   0.122(9)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.037
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     443
_refine_ls_number_reflns         9582
_refine_ls_number_restraints     1082
_refine_ls_restrained_S_all      1.135
_refine_ls_R_factor_all          0.1485
_refine_ls_R_factor_gt           0.1025
_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^)+(0.0981P)^2^+66.4616P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2417
_refine_ls_wR_factor_ref         0.2686
_reflns_Friedel_coverage         0.800
_reflns_Friedel_fraction_full    1.000
_reflns_Friedel_fraction_max     1.000
_reflns_number_gt                6446
_reflns_number_total             9582
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d1nj02460d2.cif
_cod_data_source_block           b201101d_0ma_a
_cod_depositor_comments
'Adding full bibliography for 7060742--7060746.cif.'
_cod_database_code               7060746
_shelx_estimated_absorpt_t_max   0.780
_shelx_estimated_absorpt_t_min   0.696
_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, All O(H) groups
2. Restrained distances
 C31-C38
 1.5 with sigma of 0.02
 O2-H2
 0.85 with sigma of 0.01
 O3-H3A
 0.85 with sigma of 0.01
 Sm1-H2 = Sm1-H3A
 1.5 with sigma of 0.02
 N2-C26 = N1-C8
 2 with sigma of 0.02
 N1-C8 = N2-C26
 1.2 with sigma of 0.02
 H2-H25
 2.4 with sigma of 0.02
 C13-H2
 1.930344 with sigma of 0.02
 Sm1-H2
 2.222452 with sigma of 0.02
 C31-H3A
 1.874601 with sigma of 0.02
 Sm1-H3A
 2.102827 with sigma of 0.02
3. Uiso/Uaniso restraints and constraints
C27 \\sim C4 \\sim C6 \\sim C7 \\sim C5 \\sim C30 \\sim C29 \\sim C10 \\sim C13
\\sim C8 \\sim C12 \\sim C26 \\sim C28 \\sim C3 \\sim C11 \\sim C9 \\sim C20
\\sim C25 \\sim C24 \\sim C23 \\sim C22 \\sim C21 \\sim C2 \\sim C1 \\sim C15
\\sim C16 \\sim C17 \\sim C18 \\sim C19 \\sim C14 \\sim C39 \\sim C38 \\sim C43
\\sim C42 \\sim C41 \\sim C40 \\sim C31 \\sim C36 \\sim C35 \\sim C34 \\sim C33
\\sim C32 \\sim C37 \\sim C44 \\sim C47 \\sim C45 \\sim C46: within 3.8A with
sigma of 0.01 and sigma for terminal atoms of 0.02
4.a Ternary CH refined with riding coordinates:
 C30(H30), C12(H12)
4.b Secondary CH2 refined with riding coordinates:
 C29(H29A,H29B), C27(H27A,H27B), C28(H28A,H28B), C8(H8A,H8B), C11(H11A,H11B),
 C10(H10A,H10B), C9(H9A,H9B), C26(H26A,H26B), C46(H46A,H46B), C45(H45A,H45B),
 C44(H44A,H44B), C47(H47A,H47B)
4.c Aromatic/amide H refined with riding coordinates:
 C7(H7), C3(H3), C25(H25), C24(H24), C23(H23), C22(H22), C21(H21), C15(H15),
 C16(H16), C17(H17), C18(H18), C19(H19), C39(H39), C43(H43), C42(H42), C41(H41),
  C40(H40), C36(H36), C35(H35), C34(H34), C33(H33), C37(H37)
4.d Fitted pentagon refined as free rotating group:
 C46(C45,C44,O4,C47)
4.e Fitted hexagon refined as free rotating group:
 C7(C6,C5,C4,C3,C2), C20(C25,C24,C23,C22,C21), C15(C16,C17,C18,C19,C14),
 C39(C38,C43,C42,C41,C40), C36(C35,C34,C33,C32,C37)
4.f Idealised Me refined as rotating group:
 C1(H1A,H1B,H1C)
;
_shelx_res_checksum              12994
_shelx_fab_checksum              36223
_shelx_shelxl_version_number     2016/4
_olex2_submission_special_instructions 'No special instructions were received'