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_7700210
_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 Dy N4 O5 Si2 Zn, C7 H8'
_chemical_formula_sum            'C66 H97 Dy N4 O5 Si2 Zn'
_chemical_formula_weight         1310.52
_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     direct
_audit_creation_date             2018-04-26
_audit_creation_method
;
Olex2 1.2
(compiled 2018.04.03 svn.r3497 for OlexSys, GUI svn.r5486)
;
_audit_update_record
;
2018-09-27 deposited with the CCDC.    2019-06-05 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 108.6460(8)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   10.4278(2)
_cell_length_b                   25.8777(4)
_cell_length_c                   15.2743(2)
_cell_measurement_reflns_used    9099
_cell_measurement_temperature    170(2)
_cell_measurement_theta_max      54.97
_cell_measurement_theta_min      5.32
_cell_volume                     3905.39(11)
_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    'ShelXS (Sheldrick, 2008)'
_diffrn_ambient_temperature      170.01
_diffrn_measured_fraction_theta_full 0.984
_diffrn_measured_fraction_theta_max 0.984
_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  0.0362
_diffrn_reflns_av_unetI/netI     0.0786
_diffrn_reflns_Laue_measured_fraction_full 0.984
_diffrn_reflns_Laue_measured_fraction_max 0.984
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       28
_diffrn_reflns_limit_k_min       -31
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            38609
_diffrn_reflns_point_group_measured_fraction_full 0.985
_diffrn_reflns_point_group_measured_fraction_max 0.985
_diffrn_reflns_theta_full        53.594
_diffrn_reflns_theta_max         54.948
_diffrn_reflns_theta_min         5.318
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    5.631
_exptl_absorpt_correction_T_max  0.7508
_exptl_absorpt_correction_T_min  0.4988
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
'SADABS-2016/2 (Bruker,2016/2) was used for absorption correction. wR2(int) was 0.1353 before and 0.0902 after correction. The Ratio of minimum to maximum transmission is 0.6644. The \l/2 correction factor is Not present.'
_exptl_crystal_colour            colourless
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.114
_exptl_crystal_description       block
_exptl_crystal_F_000             1370
_exptl_crystal_size_max          0.2
_exptl_crystal_size_mid          0.15
_exptl_crystal_size_min          0.1
_refine_diff_density_max         1.163
_refine_diff_density_min         -0.840
_refine_diff_density_rms         0.137
_refine_ls_abs_structure_details
;
 Refined as an inversion twin.
;
_refine_ls_abs_structure_Flack   0.099(6)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.055
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     721
_refine_ls_number_reflns         13053
_refine_ls_number_restraints     68
_refine_ls_restrained_S_all      1.059
_refine_ls_R_factor_all          0.0647
_refine_ls_R_factor_gt           0.0620
_refine_ls_shift/su_max          0.043
_refine_ls_shift/su_mean         0.001
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.1101P)^2^+9.1048P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1772
_refine_ls_wR_factor_ref         0.1797
_reflns_Friedel_coverage         0.956
_reflns_Friedel_fraction_full    0.986
_reflns_Friedel_fraction_max     0.986
_reflns_number_gt                12128
_reflns_number_total             13053
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c9dt00064j2.cif
_cod_data_source_block           mjl18162_0m
_cod_depositor_comments
'Adding full bibliography for 7700208--7700212.cif.'
_cod_database_code               7700210
_shelx_shelxl_version_number     2016/6
_shelx_estimated_absorpt_t_max   0.603
_shelx_estimated_absorpt_t_min   0.399
_olex2_refinement_description
;
1. Twinned data refinement
 Scales: 0.901(6)
 0.099(6)
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. Restrained distances
 H3-H33A
 2 with sigma of 0.02
4. Uiso/Uaniso restraints and constraints
C2S \\sim C7S \\sim C6S \\sim C5S \\sim C4S \\sim C3S \\sim C1S: within 2A with
sigma of 0.01 and sigma for terminal atoms of 0.02
Uanis(C28) \\sim Ueq, Uanis(C27) \\sim Ueq, Uanis(C26) \\sim Ueq, Uanis(C4)
\\sim Ueq: with sigma of 0.005 and sigma for terminal atoms of 0.01
5.a Ternary CH refined with riding coordinates:
 Si1(H1), Si2(H2), C41(H41), C46(H46)
5.b Secondary CH2 refined with riding coordinates:
 C7(H7A,H7B), C8(H8A,H8B), C9(H9A,H9B), C11(H11A,H11B), C42(H42A,H42B),
 C43(H43A,H43B), C44(H44A,H44B), C45(H45A,H45B)
5.c Aromatic/amide H refined with riding coordinates:
 C3(H3), C5(H5), C15(H15), C17(H17), C36(H36), C37(H37), C38(H38), C40(H40),
 C47(H47), C49(H49), C50(H50), C51(H51), C3S(H3S), C4S(H4S), C5S(H5S), C6S(H6S),
  C7S(H7S)
5.d Fitted hexagon refined as free rotating group:
 C2S(C3S,C4S,C5S,C6S,C7S)
5.e Idealised Me refined as rotating group:
 C10(H10A,H10B,H10C), C19(H19A,H19B,H19C), C20(H20A,H20B,H20C), C21(H21A,H21B,
 H21C), C23(H23A,H23B,H23C), C24(H24A,H24B,H24C), C25(H25A,H25B,H25C), C27(H27A,
 H27B,H27C), C28(H28A,H28B,H28C), C29(H29A,H29B,H29C), C31(H31A,H31B,H31C),
 C32(H32A,H32B,H32C), C33(H33A,H33B,H33C), C54(H54A,H54B,H54C), C55(H55A,H55B,
 H55C), C56(H56A,H56B,H56C), C57(H57A,H57B,H57C), C58(H58A,H58B,H58C), C59(H59A,
 H59B,H59C), C1S(H1SA,H1SB,H1SC)
;
_shelx_res_checksum              87058
_shelx_fab_checksum              59174
_olex2_submission_special_instructions 'No special instructions were received'