Syntheses, characterizations and catalytic properties of three zinc complexes and one lithium compound chelated by β-diketiminate ligands
Lu, Yanhua; Li, Yafei; She, Yeye; Jia, Chaohong; Li, Yahong; New Journal of Chemistry 47 (2023) 8933–8941; doi:10.1039/D3NJ00713H

data_7062439
_publ_section_title
;
 Syntheses, characterizations and catalytic properties of three zinc
 complexes and one lithium compound chelated by \b-diketiminate ligands
;
_journal_issue                   18
_journal_name_full               'New Journal of Chemistry'
_journal_page_first              8933
_journal_page_last               8941
_journal_paper_doi               10.1039/D3NJ00713H
_journal_volume                  47
_journal_year                    2023
_chemical_formula_moiety         'C36 H53 Cl3 N4 Zn2, C7 H8'
_chemical_formula_sum            'C43 H61 Cl3 N4 Zn2'
_chemical_formula_weight         871.04
_space_group_crystal_system      monoclinic
_space_group_IT_number           15
_space_group_name_Hall           '-C 2yc'
_space_group_name_H-M_alt        'C 1 2/c 1'
_atom_sites_solution_hydrogens   geom
_audit_creation_date             2023-03-08
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_audit_update_record
;
2023-03-10 deposited with the CCDC.	2023-04-18 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 110.407(3)
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   32.1803(15)
_cell_length_b                   12.7041(5)
_cell_length_c                   23.3535(9)
_cell_measurement_reflns_used    9850
_cell_measurement_temperature    120.00
_cell_measurement_theta_max      48.40
_cell_measurement_theta_min      2.55
_cell_volume                     8948.2(7)
_computing_cell_refinement       'SAINT V8.40B (?, 2016)'
_computing_data_reduction        'SAINT V8.40B (?, 2016)'
_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 2018/2 (Sheldrick, 2018)'
_diffrn_ambient_temperature      120.0
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.998
_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  0.0996
_diffrn_reflns_av_unetI/netI     0.0588
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_limit_h_max       38
_diffrn_reflns_limit_h_min       -38
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       28
_diffrn_reflns_limit_l_min       -28
_diffrn_reflns_number            84405
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_theta_full        53.594
_diffrn_reflns_theta_max         54.185
_diffrn_reflns_theta_min         2.549
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    2.041
_exptl_absorpt_correction_T_max  0.7506
_exptl_absorpt_correction_T_min  0.6357
_exptl_absorpt_correction_type   none
_exptl_absorpt_process_details
;
SADABS-2016/2 (Bruker,2016/2) was used for absorption correction.
wR2(int) was 0.1271 before and 0.0765 after correction.
The Ratio of minimum to maximum transmission is 0.8469.
The \l/2 correction factor is Not present.
;
_exptl_crystal_colour            'metallic light colourless'
_exptl_crystal_colour_lustre     metallic
_exptl_crystal_colour_modifier   light
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.293
_exptl_crystal_description       block
_exptl_crystal_F_000             3664
_exptl_crystal_size_max          0.02
_exptl_crystal_size_mid          0.02
_exptl_crystal_size_min          0.01
_refine_diff_density_max         0.812
_refine_diff_density_min         -0.490
_refine_diff_density_rms         0.080
_refine_ls_extinction_coef       0.00056(5)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     'SHELXL-2018/3 (Sheldrick 2018)'
_refine_ls_goodness_of_fit_ref   1.070
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     546
_refine_ls_number_reflns         8265
_refine_ls_number_restraints     393
_refine_ls_restrained_S_all      1.089
_refine_ls_R_factor_all          0.1120
_refine_ls_R_factor_gt           0.0617
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.1014P)^2^+6.3412P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1646
_refine_ls_wR_factor_ref         0.1956
_reflns_Friedel_coverage         0.000
_reflns_number_gt                4893
_reflns_number_total             8265
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d3nj00713h2.cif
_cod_data_source_block           t
_cod_depositor_comments
'Adding full bibliography for 7062437--7062439.cif.'
_cod_database_code               7062439
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   0.980
_shelx_estimated_absorpt_t_min   0.960
_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
2. Restrained distances
 C1A-C1B
 1.51 with sigma of 0.02
 C1B-C1C = C1B-C1G = C1D-C1E
 1.39 with sigma of 0.02
 C1C-C1D = C1E-C1F = C1F-C1G
 1.38 with sigma of 0.02
 C1H-C1I
 1.51 with sigma of 0.02
 C1I-C1J = C1I-C1N = C1K-C1L
 1.39 with sigma of 0.02
 C1J-C1K = C1L-C1M = C1M-C1N
 1.38 with sigma of 0.02
 C35-C34
 1.54 with sigma of 0.001
 C1I-C1H
 1.5 with sigma of 0.01
 C1A-C1C = C1A-C1G
 2.52 with sigma of 0.04
 C1B-C1D
 2.42 with sigma of 0.04
 C1B-C1F
 2.41 with sigma of 0.04
 C1C-C1E
 2.39 with sigma of 0.04
 C1D-C1F = C1E-C1G
 2.4 with sigma of 0.04
 C1H-C1J = C1H-C1N
 2.52 with sigma of 0.04
 C1I-C1K
 2.42 with sigma of 0.04
 C1I-C1M
 2.41 with sigma of 0.04
 C1J-C1L
 2.39 with sigma of 0.04
 C1K-C1M = C1L-C1N
 2.4 with sigma of 0.04
 C1B-C1C \\sim C1C-C1D \\sim C1D-C1E \\sim C1E-C1F \\sim C1F-C1G \\sim C1G-C1B
 with sigma of 0.02
 C1B-C1F \\sim C1B-C1D \\sim C1G-C1E \\sim C1C-C1G \\sim C1D-C1F \\sim C1C-C1E
 with sigma of 0.04
 C1A-C1G \\sim C1A-C1C
 with sigma of 0.04
 C1I-C1J \\sim C1J-C1K \\sim C1K-C1L \\sim C1L-C1M \\sim C1M-C1N \\sim C1N-C1I
 with sigma of 0.02
 C1I-C1M \\sim C1I-C1K \\sim C1N-C1L \\sim C1J-C1N \\sim C1K-C1M \\sim C1J-C1L
 with sigma of 0.04
 C1H-C1N \\sim C1H-C1J
 with sigma of 0.04
 C35A-C34 \\sim C35-C34
 with sigma of 0.02
 C35-C34 \\sim C35A-C34
 with sigma of 0.02
3. Restrained planarity
 C1A, C1B, C1C, C1D, C1E, C1F, C1G
 with sigma of 0.1
 C1H, C1I, C1J, C1K, C1L, C1M, C1N
 with sigma of 0.1
 C1K, C1H, C1I, C1J, C1N, C1M, C1L
 with sigma of 0.1
4. Uiso/Uaniso restraints and constraints
C1A \\sim C1B \\sim C1C \\sim C1D \\sim C1E \\sim C1F \\sim C1G: within 2A with
sigma of 0.04 and sigma for terminal atoms of 0.08
C1H \\sim C1I \\sim C1J \\sim C1K \\sim C1L \\sim C1M \\sim C1N: within 2A with
sigma of 0.04 and sigma for terminal atoms of 0.08
Uanis(C1I) \\sim Ueq, Uanis(C1H) \\sim Ueq, Uanis(C1N) \\sim Ueq, Uanis(C1M)
\\sim Ueq, Uanis(C1L) \\sim Ueq, Uanis(C1K) \\sim Ueq, Uanis(C1J) \\sim Ueq:
with sigma of 0.01 and sigma for terminal atoms of 0.02
Uanis(C1A) \\sim Ueq, Uanis(C1B) \\sim Ueq, Uanis(C1C) \\sim Ueq, Uanis(C1G)
\\sim Ueq, Uanis(C1D) \\sim Ueq, Uanis(C1F) \\sim Ueq, Uanis(C1E) \\sim Ueq:
with sigma of 0.01 and sigma for terminal atoms of 0.02
Uanis(C34) \\sim Ueq, Uanis(C35) \\sim Ueq, Uanis(C35A) \\sim Ueq, Uanis(C36)
\\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
Uanis(C35) \\sim Ueq, Uanis(C35A) \\sim Ueq: with sigma of 0.01 and sigma for
terminal atoms of 0.02
5. Rigid body (RIGU) restrains
 C1A, C1B, C1C, C1D, C1E, C1F, C1G
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 C1H, C1I, C1J, C1K, C1L, C1M, C1N
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 C34, C35, C35A
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.02
6. Others
 Sof(H34A)=Sof(C35A)=Sof(H35D)=Sof(H35E)=Sof(H35F)=1-FVAR(1)
 Sof(H34)=Sof(C35)=Sof(H35A)=Sof(H35B)=Sof(H35C)=FVAR(1)
 Fixed Sof: C1A(0.5) H1AA(0.5) H1AB(0.5) H1AC(0.5) C1B(0.5) C1C(0.5) H1CA(0.5)
 C1D(0.5) H1D(0.5) C1E(0.5) H1E(0.5) C1F(0.5) H1F(0.5) C1G(0.5) H1G(0.5)
 C1H(0.5) H1HA(0.5) H1HB(0.5) H1HC(0.5) C1J(0.5) H1J(0.5) C1K(0.5) H1K(0.5)
 C1L(0.5) H1L(0.5) C1M(0.5) H1M(0.5) C1N(0.5) H1N(0.5) C1I(0.5)
7.a Ternary CH refined with riding coordinates:
 C3(H3), C11(H11), C27(H27), C34(H34), C34(H34A)
7.b Secondary CH2 refined with riding coordinates:
 C15(H15A,H15B), C18(H18A,H18B), C19(H19A,H19B)
7.c Aromatic/amide H refined with riding coordinates:
 C5(H5), C6(H6), C7(H7), C22(H22), C30(H30), C31(H31), C32(H32), C1C(H1CA),
 C1D(H1D), C1E(H1E), C1F(H1F), C1G(H1G), C1J(H1J), C1K(H1K), C1L(H1L), C1M(H1M),
  C1N(H1N)
7.d Fitted hexagon refined as free rotating group:
 C1J(C1K,C1L,C1M,C1N,C1I)
7.e Idealised Me refined as rotating group:
 C1(H1A,H1B,H1C), C2(H2A,H2B,H2C), C10(H10A,H10B,H10C), C12(H12A,H12B,H12C),
 C13(H13A,H13B,H13C), C17(H17A,H17B,H17C), C20(H20A,H20B,H20C), C24(H24A,H24B,
 H24C), C28(H28A,H28B,H28C), C29(H29A,H29B,H29C), C35(H35A,H35B,H35C), C36(H36A,
 H36B,H36C), C1A(H1AA,H1AB,H1AC), C1H(H1HA,H1HB,H1HC), C35A(H35D,H35E,H35F)
;
_shelx_res_checksum              56607
_olex2_submission_special_instructions 'No special instructions were received'