An insight into the molecular structures, theoretical calculation and catalytic activities of novel heterotrinuclear [CuII2CeIII] and heterohexanuclear [CuII4YIII2] bis(salamo)-based complexes
Chen, Zhuang-Zhuang; Zhang, Wen-Ze; Zhang, Ting; Zhang, Yang; Dong, Wen-Kui; New Journal of Chemistry 44 (2020) 19836–19849; doi:10.1039/D0NJ04126B

data_7060129
_publ_section_title
;
 An insight into the molecular structures, theoretical calculation and
 catalytic activities of novel heterotrinuclear [CuII2CeIII] and
 heterohexanuclear [CuII4YIII2] bis(salamo)-based complexes
;
_journal_issue                   45
_journal_name_full               'New Journal of Chemistry'
_journal_page_first              19836
_journal_page_last               19849
_journal_paper_doi               10.1039/D0NJ04126B
_journal_volume                  44
_journal_year                    2020
_chemical_formula_moiety
'C40 H45 Cu2 N8 O16 Y, C39 H46 Cu2 N9 O18 Y, 4(C H4 O)'
_chemical_formula_sum            'C83 H107 Cu4 N17 O38 Y2'
_chemical_formula_weight         2382.83
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     dual
_audit_creation_date             2020-08-02
_audit_creation_method
;
Olex2 1.3
(compiled 2020.06.28 svn.raecde09e for OlexSys, GUI svn.r6132)
;
_audit_update_record
;
2020-08-12 deposited with the CCDC.	2020-10-22 downloaded from the CCDC.
;
_cell_angle_alpha                106.755(2)
_cell_angle_beta                 101.128(2)
_cell_angle_gamma                93.311(2)
_cell_formula_units_Z            2
_cell_length_a                   12.8639(7)
_cell_length_b                   17.7598(9)
_cell_length_c                   23.1688(13)
_cell_measurement_reflns_used    9967
_cell_measurement_temperature    173.15
_cell_measurement_theta_max      27.19
_cell_measurement_theta_min      2.31
_cell_volume                     4936.8(5)
_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      173.15
_diffrn_measured_fraction_theta_full 0.994
_diffrn_measured_fraction_theta_max 0.994
_diffrn_measurement_device_type  CCD
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0387
_diffrn_reflns_av_unetI/netI     0.0652
_diffrn_reflns_Laue_measured_fraction_full 0.994
_diffrn_reflns_Laue_measured_fraction_max 0.994
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       21
_diffrn_reflns_limit_k_min       -21
_diffrn_reflns_limit_l_max       27
_diffrn_reflns_limit_l_min       -27
_diffrn_reflns_number            35519
_diffrn_reflns_point_group_measured_fraction_full 0.994
_diffrn_reflns_point_group_measured_fraction_max 0.994
_diffrn_reflns_theta_full        25.010
_diffrn_reflns_theta_max         25.010
_diffrn_reflns_theta_min         2.049
_exptl_absorpt_coefficient_mu    2.103
_exptl_absorpt_correction_T_max  1.0000
_exptl_absorpt_correction_T_min  0.7924
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   SADABS
_exptl_crystal_colour            colourless
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.603
_exptl_crystal_description       block
_exptl_crystal_F_000             2444
_exptl_crystal_size_max          0.22
_exptl_crystal_size_mid          0.17
_exptl_crystal_size_min          0.16
_refine_diff_density_max         1.037
_refine_diff_density_min         -0.650
_refine_diff_density_rms         0.092
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.021
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1374
_refine_ls_number_reflns         17298
_refine_ls_number_restraints     166
_refine_ls_restrained_S_all      1.034
_refine_ls_R_factor_all          0.0784
_refine_ls_R_factor_gt           0.0482
_refine_ls_shift/su_max          0.006
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0614P)^2^+10.1097P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1225
_refine_ls_wR_factor_ref         0.1371
_reflns_Friedel_coverage         0.000
_reflns_number_gt                12430
_reflns_number_total             17298
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d0nj04126b2.cif
_cod_data_source_block           cu-y
_cod_database_code               7060129
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   0.730
_shelx_estimated_absorpt_t_min   0.655
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups, All C(H,H,H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups, All O(H) groups
2. Restrained distances
 C83-O38
 1.4 with sigma of 0.02
 O34-H34
 0.87 with sigma of 0.01
 O37-C81
 1.4 with sigma of 0.01
 O38-C83
 1.4 with sigma of 0.01
 C84-O39
 1.4 with sigma of 0.02
 C79-H34
 1.861966 with sigma of 0.02
 Cu4-H34
 2.889268 with sigma of 0.02
3. Uiso/Uaniso restraints and constraints
Uanis(C79) \\sim Ueq, Uanis(C79A) \\sim Ueq: with sigma of 0.005 and sigma for
terminal atoms of 0.01
Uanis(C83) \\sim Ueq, Uanis(O38) \\sim Ueq: with sigma of 0.01 and sigma for
terminal atoms of 0.02
Uanis(N9) \\sim Ueq, Uanis(C41) \\sim Ueq, Uanis(C42) \\sim Ueq, Uanis(C43)
\\sim Ueq, Uanis(C44) \\sim Ueq, Uanis(C44A) \\sim Ueq, Uanis(C41A) \\sim Ueq:
with sigma of 0.01 and sigma for terminal atoms of 0.02
Uanis(O39) \\sim Ueq, Uanis(C84) \\sim Ueq: with sigma of 0.01 and sigma for
terminal atoms of 0.02
Uanis(O30) \\sim Ueq: with sigma of 0.005 and sigma for terminal atoms of 0.01
4. Rigid body (RIGU) restrains
 O34, C79
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 C79A, O34
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 C83, O38
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 N9, C41, C42, C43, C44, C44A, C41A
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 O39, C84
 with sigma for 1-2 distances of 0.001 and sigma for 1-3 distances of 0.001
 O30, N17, O28
 with sigma for 1-2 distances of 0.001 and sigma for 1-3 distances of 0.001
 C78, N14, C76, C75, C77
 with sigma for 1-2 distances of 0.001 and sigma for 1-3 distances of 0.001
5. Others
 Sof(H43C)=Sof(H43D)=Sof(C44A)=Sof(H44D)=Sof(H44E)=Sof(H44F)=1-FVAR(1)
 Sof(H43A)=Sof(H43B)=Sof(C44)=Sof(H44A)=Sof(H44B)=Sof(H44C)=FVAR(1)
 Sof(H42C)=Sof(H42D)=Sof(C41A)=Sof(H41D)=Sof(H41E)=Sof(H41F)=1-FVAR(2)
 Sof(C41)=Sof(H41A)=Sof(H41B)=Sof(H41C)=Sof(H42A)=Sof(H42B)=FVAR(2)
 Fixed Sof: C40(0.5) H40A(0.5) H40B(0.5) H40C(0.5) C40A(0.5) H40D(0.5)
 H40E(0.5) H40F(0.5) C79(0.5) H79A(0.5) H79B(0.5) H79C(0.5) O38(0.5) H38(0.5)
 C83(0.5) H83A(0.5) H83B(0.5) H83C(0.5) O39(0.5) H39(0.5) C84(0.5) H84A(0.5)
 H84B(0.5) H84C(0.5) C79A(0.5) H79D(0.5) H79E(0.5) H79F(0.5)
6.a Riding coordinates:
 O37(H37), O35(H35), C81(H81A,H81B,H81C), C82(H82A,H82B,H82C), O38(H38),
 C83(H83A,H83B,H83C)
6.b Secondary CH2 refined with riding coordinates:
 C2(H2A,H2B), C4(H4A,H4B), C12(H12A,H12B), C13(H13A,H13B), C26(H26A,H26B),
 C27(H27A,H27B), C35(H35A,H35B), C37(H37A,H37B), C42(H42A,H42B), C42(H42C,H42D),
  C43(H43A,H43B), C43(H43C,H43D), C52(H52A,H52B), C53(H53A,H53B), C66(H66A,
 H66B), C67(H67A,H67B), C76(H76A,H76B), C78(H78A,H78B)
6.c Aromatic/amide H refined with riding coordinates:
 C6(H6), C7(H7), C10(H10), C11(H11), C14(H14), C17(H17), C18(H18), C19(H19),
 C20(H20), C25(H25), C28(H28), C31(H31), C33(H33), C34(H34A), C46(H46),
 C47(H47), C50(H50), C51(H51), C54(H54), C57(H57), C58(H58), C59(H59), C60(H60),
  C65(H65), C68(H68), C70(H70), C71(H71), C73(H73)
6.d Idealised Me refined as rotating group:
 C1(H1A,H1B,H1C), C3(H3A,H3B,H3C), C36(H36A,H36B,H36C), C38(H38A,H38B,H38C),
 C40(H40A,H40B,H40C), C40A(H40D,H40E,H40F), C41(H41A,H41B,H41C), C44(H44A,H44B,
 H44C), C75(H75A,H75B,H75C), C77(H77A,H77B,H77C), C79(H79A,H79B,H79C),
 C44A(H44D,H44E,H44F), C41A(H41D,H41E,H41F), C80(H80A,H80B,H80C), C84(H84A,H84B,
 H84C), C79A(H79D,H79E,H79F)
6.e Idealised tetrahedral OH refined as rotating group:
 O36(H36), O39(H39)
;
_shelx_res_checksum              73054
_olex2_submission_special_instructions 'No special instructions were received'