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_7062437
_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         'C64 H84 N6 Zn'
_chemical_formula_sum            'C64 H84 N6 Zn'
_chemical_formula_weight         1002.74
_chemical_properties_physical    Air-sensitive,Moisture-sensitive
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2ybc'
_space_group_name_H-M_alt        'P 1 21/c 1'
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     iterative
_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
;
2023-03-08 deposited with the CCDC.	2023-04-18 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 97.174(2)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   22.4873(12)
_cell_length_b                   10.3091(5)
_cell_length_c                   23.5539(13)
_cell_measurement_reflns_used    9631
_cell_measurement_temperature    120(2)
_cell_measurement_theta_max      53.850
_cell_measurement_theta_min      3.447
_cell_volume                     5417.6(5)
_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    'olex2.solve (Bourhis et al., 2015)'
_diffrn_ambient_temperature      120.0
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.995
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_type           GaK\a
_diffrn_radiation_wavelength     1.34138
_diffrn_reflns_av_R_equivalents  0.0559
_diffrn_reflns_av_unetI/netI     0.0425
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.995
_diffrn_reflns_limit_h_max       26
_diffrn_reflns_limit_h_min       -27
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       28
_diffrn_reflns_limit_l_min       -28
_diffrn_reflns_number            54230
_diffrn_reflns_point_group_measured_fraction_full 0.997
_diffrn_reflns_point_group_measured_fraction_max 0.995
_diffrn_reflns_theta_full        53.594
_diffrn_reflns_theta_max         53.955
_diffrn_reflns_theta_min         3.447
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.606
_exptl_absorpt_correction_T_max  0.7506
_exptl_absorpt_correction_T_min  0.5984
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
'SADABS-2016/2 (Bruker,2016/2) was used for absorption correction. wR2(int) was 0.0919 before and 0.0602 after correction. The Ratio of minimum to maximum transmission is 0.7972. The \l/2 correction factor is Not present.'
_exptl_crystal_colour            yellow
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    1.229
_exptl_crystal_description       BLOCK
_exptl_crystal_F_000             2160
_exptl_crystal_size_max          0.04
_exptl_crystal_size_mid          0.03
_exptl_crystal_size_min          0.02
_refine_diff_density_max         0.407
_refine_diff_density_min         -0.748
_refine_diff_density_rms         0.104
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.036
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     654
_refine_ls_number_reflns         9897
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.036
_refine_ls_R_factor_all          0.0527
_refine_ls_R_factor_gt           0.0400
_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^)+(0.0470P)^2^+3.7802P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0983
_refine_ls_wR_factor_ref         0.1052
_reflns_Friedel_coverage         0.000
_reflns_number_gt                8399
_reflns_number_total             9897
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d3nj00713h2.cif
_cod_data_source_block           b211221lyh6_0m
_cod_depositor_comments
'Adding full bibliography for 7062437--7062439.cif.'
_cod_database_code               7062437
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   0.988
_shelx_estimated_absorpt_t_min   0.976
_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.a Ternary CH refined with riding coordinates:
 C00U(H00U), C5(H5), C34(H34), C44(H44), C12(H12), C49(H49)
2.b Secondary CH2 refined with riding coordinates:
 C37(H37A,H37B), C4(H4A,H4B), C46(H46A,H46B), C45(H45A,H45B), C13(H13A,H13B),
 C35(H35A,H35B), C50(H50A,H50B), C36(H36A,H36B), C47(H47A,H47B), C48(H48A,H48B),
  C01K(H01A,H01B), C01L(H01C,H01D), C33(H33A,H33B), C3(H3A,H3B), C01O(H01E,
 H01F), C15(H15A,H15B), C2(H2A,H2B), C51(H51A,H51B), C14(H14A,H14B), C1(H1A,
 H1B), C52(H52A,H52B), C16(H16A,H16B), C01X(H01G,H01H), C53(H53A,H53B)
2.c Aromatic/amide H refined with riding coordinates:
 C40(H40), C7(H7), C8(H8), C42(H42), C21(H21), C58(H58), C57(H57), C55(H55),
 C19(H19), C20(H20)
2.d Idealised Me refined as rotating group:
 C27(H27A,H27B,H27C), C28(H28A,H28B,H28C), C23(H23A,H23B,H23C), C32(H32A,H32B,
 H32C), C17(H17A,H17B,H17C), C54(H54A,H54B,H54C)
;
_shelx_res_checksum              13307
_olex2_submission_special_instructions 'No special instructions were received'