Design and synthesis of copper(ii) malonates with N,N′-containing linkers
Zorina-Tikhonova, Ekaterina N.; Chistyakov, Aleksandr S.; Novikova, Veronika A.; Knyazev, Daniil A.; Gogoleva, Natalia V.; Blinou, Daniil O.; Efimov, Nikolay N.; Dorovatovskii, Pavel V.; Kiskin, Mikhail A.; Eremenko, Igor L.; Vologzhanina, Anna V.; CrystEngComm 25 (2023) 2859–2870; doi:10.1039/D3CE00081H

data_7246583
_publ_section_title
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 Design and synthesis of copper(ii) malonates with N,N&#x2032;-containing
 linkers
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_journal_issue                   19
_journal_name_full               CrystEngComm
_journal_page_first              2859
_journal_page_last               2870
_journal_paper_doi               10.1039/D3CE00081H
_journal_volume                  25
_journal_year                    2023
_chemical_formula_moiety         'C64 H76 Cu4 N6 O16, 5.5(H2 O)'
_chemical_formula_sum            'C64 H87 Cu4 N6 O21.5'
_chemical_formula_weight         1538.55
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2yn'
_space_group_name_H-M_alt        'P 1 21/n 1'
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     dual
_audit_creation_date             2023-02-15
_audit_creation_method
;
Olex2 1.5
(compiled 2022.04.07 svn.rca3783a0 for OlexSys, GUI svn.r6498)
;
_audit_update_record
;
2023-03-28 deposited with the CCDC.	2023-04-06 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 117.980(2)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   16.7676(6)
_cell_length_b                   13.2787(5)
_cell_length_c                   17.0342(6)
_cell_measurement_reflns_used    9000
_cell_measurement_temperature    100
_cell_measurement_theta_max      30.58
_cell_measurement_theta_min      2.34
_cell_volume                     3349.4(2)
_computing_molecular_graphics    'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2018/3 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT 2018/2 (Sheldrick, 2018)'
_diffrn_ambient_temperature      100
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device_type  'Bruker Quest'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0281
_diffrn_reflns_av_unetI/netI     0.0249
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -23
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_limit_l_min       -24
_diffrn_reflns_number            45830
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         30.581
_diffrn_reflns_theta_min         2.046
_diffrn_source_current           1.4
_diffrn_source_power             0.07
_diffrn_source_voltage           50.0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    1.333
_exptl_absorpt_correction_T_max  0.7461
_exptl_absorpt_correction_T_min  0.6376
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2016/2 (Bruker,2016/2) was used for absorption correction.
wR2(int) was 0.1358 before and 0.0488 after correction.
The Ratio of minimum to maximum transmission is 0.8546.
The \l/2 correction factor is Not present.
;
_exptl_crystal_colour            blue
_exptl_crystal_colour_primary    blue
_exptl_crystal_density_diffrn    1.526
_exptl_crystal_description       plate
_exptl_crystal_F_000             1602
_exptl_crystal_size_max          0.31
_exptl_crystal_size_mid          0.27
_exptl_crystal_size_min          0.06
_refine_diff_density_max         0.871
_refine_diff_density_min         -0.503
_refine_diff_density_rms         0.082
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.067
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     440
_refine_ls_number_reflns         10278
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.067
_refine_ls_R_factor_all          0.0404
_refine_ls_R_factor_gt           0.0331
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0393P)^2^+2.6948P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0890
_refine_ls_wR_factor_ref         0.0934
_reflns_Friedel_coverage         0.000
_reflns_number_gt                8792
_reflns_number_total             10278
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d3ce00081h2.cif
_cod_data_source_block           7
_cod_depositor_comments
'Adding full bibliography for 7246576--7246583.cif.'
_cod_original_formula_sum        'C64 H87 Cu4 N6 O21.50'
_cod_database_code               7246583
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   0.924
_shelx_estimated_absorpt_t_min   0.683
_olex2_refinement_description
;
1. Others
 Fixed Sof: O10(0.75) H10A(0.75) H10B(0.75)
2.a Riding coordinates:
 O9(H9A,H9B), O10(H10A,H10B), O11(H11A,H11B)
2.b Secondary CH2 refined with riding coordinates:
 C6(H6A,H6B), C12(H12A,H12B), C13(H13A,H13B), C22(H22A,H22B), C24(H24A,H24B),
 C29(H29A,H29B), C31(H31A,H31B)
2.c Aromatic/amide H refined with riding coordinates:
 C1(H1), C2(H2), C4(H4), C5(H5), C7(H7), C8(H8), C10(H10), C11(H11), C14(H14),
 C15(H15), C17(H17), C18(H18)
2.d Idealised Me refined as rotating group:
 C23(H23A,H23B,H23C), C25(H25A,H25B,H25C), C30(H30A,H30B,H30C), C32(H32A,H32B,
 H32C)
;
_shelx_res_checksum              59318
_olex2_submission_special_instructions 'No special instructions were received'