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_7060743
_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 Eu0.99 N2 O4, 2(C4 H8 O)'
_chemical_formula_sum            'C55 H69 Cl2 Eu0.97 N2 O6'
_chemical_formula_weight         1072.80
_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   mixed
_atom_sites_solution_primary     iterative
_audit_creation_date             2021-04-05
_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                   12.9908(4)
_cell_length_b                   12.9908(4)
_cell_length_c                   30.0245(16)
_cell_measurement_reflns_used    9871
_cell_measurement_temperature    296.15
_cell_measurement_theta_max      25.48
_cell_measurement_theta_min      2.31
_cell_volume                     5067.0(3)
_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    'olex2.solve (Bourhis et al., 2015)'
_diffrn_ambient_temperature      296.15
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.992
_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_unetI/netI     0.0535
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.992
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       37
_diffrn_reflns_limit_l_min       -32
_diffrn_reflns_number            5853
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.991
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.646
_diffrn_reflns_theta_min         2.217
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    1.361
_exptl_absorpt_correction_T_max  0.7456
_exptl_absorpt_correction_T_min  0.6279
_exptl_absorpt_correction_type   none
_exptl_absorpt_process_details
;
SADABS-2014/5 (Bruker,2014/5) was used for absorption correction.
wR2(int) was 0.1715 before and 0.0996 after correction.
The Ratio of minimum to maximum transmission is 0.8421.
The \l/2 correction factor is Not present.
;
_exptl_crystal_colour            'clear light brown'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   light
_exptl_crystal_colour_primary    brown
_exptl_crystal_density_diffrn    1.406
_exptl_crystal_description       block
_exptl_crystal_F_000             2225
_exptl_crystal_size_max          0.3
_exptl_crystal_size_mid          0.2
_exptl_crystal_size_min          0.2
_refine_diff_density_max         5.210
_refine_diff_density_min         -3.561
_refine_diff_density_rms         0.206
_refine_ls_abs_structure_details
;
 Flack x determined using 1626 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   0.079(9)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.078
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     274
_refine_ls_number_reflns         5853
_refine_ls_number_restraints     550
_refine_ls_restrained_S_all      1.241
_refine_ls_R_factor_all          0.1423
_refine_ls_R_factor_gt           0.1259
_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^)+(0.0662P)^2^+109.4203P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2777
_refine_ls_wR_factor_ref         0.2870
_reflns_Friedel_coverage         0.720
_reflns_Friedel_fraction_full    1.000
_reflns_Friedel_fraction_max     0.990
_reflns_number_gt                4954
_reflns_number_total             5853
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d1nj02460d2.cif
_cod_data_source_block           h
_cod_depositor_comments
'Adding full bibliography for 7060742--7060746.cif.'
_cod_original_cell_volume        5067.0(4)
_cod_database_code               7060743
_shelx_shelxl_version_number     2016/4
_shelx_estimated_absorpt_t_max   0.772
_shelx_estimated_absorpt_t_min   0.686
_olex2_refinement_description
;
1. Twinned data refinement
 Scales: 0.980(5)
 0.020(5)
2. 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
3. Restrained distances
 H4-H15
 2 with sigma of 0.02
 O4-H4
 0.5 with sigma of 0.02
 H4-O4
 1 with sigma of 0.02
 C1BA-C0BA
 2 with sigma of 0.02
4. Uiso/Uaniso restraints and constraints
C2 \\sim C6 \\sim C1 \\sim C10 \\sim C4 \\sim C5 \\sim C9 \\sim C8 \\sim C3
\\sim C0AA \\sim C1AA \\sim C3AA \\sim C4AA \\sim C2AA \\sim C11 \\sim C15
\\sim C7AA \\sim C8AA \\sim C36 \\sim C14 \\sim C5AA \\sim C20 \\sim C6AA:
within 3.8A with sigma of 0.01 and sigma for terminal atoms of 0.02
C9AA \\sim C4BA: within 2A with sigma of 0.01 and sigma for terminal atoms of
0.02
C0BA \\sim C1BA \\sim C2BA \\sim C3BA \\sim O4BA: within 2A with sigma of 0.01
and sigma for terminal atoms of 0.02
Uanis(C15) \\sim Ueq: with sigma of 0.001 and sigma for terminal atoms of 0.002
Uanis(Eu1) \\sim Ueq: with sigma of 0.001 and sigma for terminal atoms of 0.002
5. Others
 Fixed Sof: H0AA(0.5) H0AB(0.5) H0AC(0.5)
6.a Riding coordinates:
 C0AA(H0AA,H0AB,H0AC)
6.b Ternary CH refined with riding coordinates:
 C1AA(H1AA)
6.c Secondary CH2 refined with riding coordinates:
 C6(H6A,H6B), C5(H5A,H5B), C9(H9A,H9B), C8(H8A,H8B), C0BA(H0BA,H0BB),
 C3BA(H3BA,H3BB), C2BA(H2BA,H2BB), C1BA(H1BA,H1BB), C4BA(H4BA,H4BB), C9AA(H9AA,
 H9AB)
6.d Aromatic/amide H refined with riding coordinates:
 C3(H3), C4AA(H4AA), C3AA(H3AA), C6AA(H6AA), C20(H20), C11(H11), C15(H15),
 C7AA(H7AA), C8AA(H8AA), C36(H36), C14(H14)
6.e Fitted pentagon refined as free rotating group:
 C0BA(O4BA,C3BA,C2BA,C1BA)
6.f Fitted hexagon refined as free rotating group:
 C2AA(C4AA,C3AA,C6AA,C20,C11), C15(C7AA,C8AA,C36,C14,C5AA)
;
_shelx_res_checksum              64532
_olex2_submission_special_instructions 'No special instructions were received'