Rare-earth/zinc heterometallic complexes containing both alkoxy-amino-bis(phenolato) and chiral salen ligands: synthesis and catalytic application for copolymerization of CO<sub>2</sub> with cyclohexene oxide.
Xu, Ruoyu; Hua, Linyan; Li, Xiang; Yao, Yingming; Leng, Xuebing; Chen, Yaofeng; Dalton transactions (Cambridge, England : 2003) 48 (2019) 10565–10573; doi:10.1039/c9dt00064j

data_7700211
_publ_section_title
;
 Rare-earth/zinc heterometallic complexes containing both
 alkoxy-amino-bis(phenolato) and chiral salen ligands: synthesis and
 catalytic application for copolymerization of CO<sub>2</sub> with
 cyclohexene oxide.
;
_journal_issue                   28
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              10565
_journal_page_last               10573
_journal_paper_doi               10.1039/c9dt00064j
_journal_volume                  48
_journal_year                    2019
_chemical_absolute_configuration rmad
_chemical_formula_moiety         'C59 H89 N4 O5 Si2 Sm Zn, C7 H8'
_chemical_formula_sum            'C66 H97 N4 O5 Si2 Sm Zn'
_chemical_formula_weight         1298.37
_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'
_symmetry_space_group_name_Hall  'P 2yb'
_symmetry_space_group_name_H-M   'P 1 21 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_audit_creation_date             2018-04-24
_audit_creation_method
;
Olex2 1.2
(compiled 2018.04.18 svn.r3501 for OlexSys, GUI svn.r5488)
;
_audit_update_record
;
2018-09-27 deposited with the CCDC.    2019-06-05 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 108.7512(9)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   10.3825(2)
_cell_length_b                   26.0638(5)
_cell_length_c                   15.2519(3)
_cell_measurement_reflns_used    9592
_cell_measurement_temperature    173(2)
_cell_measurement_theta_max      55.036
_cell_measurement_theta_min      5.170
_cell_volume                     3908.22(13)
_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 (Sheldrick, 2015)'
_diffrn_ambient_temperature      173.0
_diffrn_measured_fraction_theta_full 0.987
_diffrn_measured_fraction_theta_max 0.986
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_type           GaK\a
_diffrn_radiation_wavelength     1.34139
_diffrn_reflns_av_R_equivalents  0.0377
_diffrn_reflns_av_unetI/netI     0.0489
_diffrn_reflns_Laue_measured_fraction_full 0.987
_diffrn_reflns_Laue_measured_fraction_max 0.986
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       31
_diffrn_reflns_limit_k_min       -29
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            39799
_diffrn_reflns_point_group_measured_fraction_full 0.987
_diffrn_reflns_point_group_measured_fraction_max 0.986
_diffrn_reflns_theta_full        53.594
_diffrn_reflns_theta_max         55.011
_diffrn_reflns_theta_min         3.962
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    4.483
_exptl_absorpt_correction_T_max  0.7508
_exptl_absorpt_correction_T_min  0.5052
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
'SADABS-2016/2 (Bruker,2016/2) was used for absorption correction. wR2(int) was 0.1333 before and 0.0933 after correction. The Ratio of minimum to maximum transmission is 0.6729. The \l/2 correction factor is Not present.'
_exptl_crystal_colour            colourless
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.103
_exptl_crystal_description       block
_exptl_crystal_F_000             1362
_exptl_crystal_size_max          0.25
_exptl_crystal_size_mid          0.2
_exptl_crystal_size_min          0.12
_refine_diff_density_max         0.969
_refine_diff_density_min         -0.461
_refine_diff_density_rms         0.075
_refine_ls_abs_structure_details
;
 Refined as an inversion twin.
;
_refine_ls_abs_structure_Flack   0.199(4)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.030
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     721
_refine_ls_number_reflns         12221
_refine_ls_number_restraints     7
_refine_ls_restrained_S_all      1.031
_refine_ls_R_factor_all          0.0362
_refine_ls_R_factor_gt           0.0356
_refine_ls_shift/su_max          0.005
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0496P)^2^+4.3931P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0959
_refine_ls_wR_factor_ref         0.0966
_reflns_Friedel_coverage         0.955
_reflns_Friedel_fraction_full    0.988
_reflns_Friedel_fraction_max     0.986
_reflns_number_gt                11980
_reflns_number_total             12221
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c9dt00064j2.cif
_cod_data_source_block           mjl18157_0m
_cod_depositor_comments
'Adding full bibliography for 7700208--7700212.cif.'
_cod_original_cell_volume        3908.21(13)
_cod_database_code               7700211
_shelx_shelxl_version_number     2017/1
_shelx_estimated_absorpt_t_max   0.615
_shelx_estimated_absorpt_t_min   0.400
_olex2_refinement_description
;
1. Twinned data refinement
 Scales: 0.801(4)
 0.199(4)
2. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups, All Si(H) groups
 At 1.5 times of:
  All C(H,H,H) groups
3. Uiso/Uaniso restraints and constraints
Uanis(C53) \\sim Ueq: with sigma of 0.005 and sigma for terminal atoms of 0.01
4.a Ternary CH refined with riding coordinates:
 Si1(H1), Si2(H2), C9(H9), C14(H14)
4.b Secondary CH2 refined with riding coordinates:
 C10(H10A,H10B), C11(H11A,H11B), C12(H12A,H12B), C13(H13A,H13B), C29(H29A,
 H29B), C38(H38A,H38B), C39(H39A,H39B), C41(H41A,H41B)
4.c Aromatic/amide H refined with riding coordinates:
 C3(H3), C4(H4), C5(H5), C7(H7), C15(H15), C17(H17), C18(H18), C19(H19),
 C25(H25), C27(H27), C43(H43), C45(H45), C61(H61), C62(H62), C63(H63), C64(H64),
  C65(H65)
4.d Fitted hexagon refined as free rotating group:
 C60(C61,C62,C63,C64,C65)
4.e Idealised Me refined as rotating group:
 C8(H8A,H8B,H8C), C22(H22A,H22B,H22C), C31(H31A,H31B,H31C), C32(H32A,H32B,
 H32C), C33(H33A,H33B,H33C), C35(H35A,H35B,H35C), C36(H36A,H36B,H36C), C37(H37A,
 H37B,H37C), C40(H40A,H40B,H40C), C49(H49A,H49B,H49C), C50(H50A,H50B,H50C),
 C51(H51A,H51B,H51C), C53(H53A,H53B,H53C), C54(H54A,H54B,H54C), C55(H55A,H55B,
 H55C), C56(H56A,H56B,H56C), C57(H57A,H57B,H57C), C58(H58A,H58B,H58C), C59(H59A,
 H59B,H59C), C66(H66A,H66B,H66C)
;
_shelx_res_checksum              83553
_shelx_fab_checksum              67488
_olex2_submission_special_instructions 'No special instructions were received'