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_7246582
_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         'C60 H66 Cu4 N8 O21, 3(H2 O)'
_chemical_formula_sum            'C60 H72 Cu4 N8 O24'
_chemical_formula_weight         1543.41
_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     dual
_audit_creation_date             2023-02-17
_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                 95.6250(10)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   24.8208(14)
_cell_length_b                   19.2806(11)
_cell_length_c                   13.1952(8)
_cell_measurement_reflns_used    6579
_cell_measurement_temperature    120
_cell_measurement_theta_max      30.87
_cell_measurement_theta_min      2.47
_cell_volume                     6284.3(6)
_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 2014/4 (Sheldrick, 2014)'
_diffrn_ambient_temperature      120.00
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.921
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0469
_diffrn_reflns_av_unetI/netI     0.0590
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.921
_diffrn_reflns_limit_h_max       35
_diffrn_reflns_limit_h_min       -26
_diffrn_reflns_limit_k_max       26
_diffrn_reflns_limit_k_min       -27
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            57730
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.921
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         31.034
_diffrn_reflns_theta_min         0.824
_diffrn_source_current           30.0
_diffrn_source_power             1.5
_diffrn_source_voltage           50.0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    1.425
_exptl_absorpt_correction_T_max  0.3373
_exptl_absorpt_correction_T_min  0.2977
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2014/5 (Bruker,2014/5) was used for absorption correction.
wR2(int) was 0.0601 before and 0.0500 after correction.
The Ratio of minimum to maximum transmission is 0.8826.
The \l/2 correction factor is 0.00150.
;
_exptl_crystal_colour            blue
_exptl_crystal_colour_primary    blue
_exptl_crystal_density_diffrn    1.631
_exptl_crystal_description       prism
_exptl_crystal_F_000             3184
_exptl_crystal_size_max          0.23
_exptl_crystal_size_mid          0.21
_exptl_crystal_size_min          0.18
_refine_diff_density_max         5.477
_refine_diff_density_min         -1.589
_refine_diff_density_rms         0.125
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.016
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     887
_refine_ls_number_reflns         18491
_refine_ls_number_restraints     5
_refine_ls_restrained_S_all      1.016
_refine_ls_R_factor_all          0.1046
_refine_ls_R_factor_gt           0.0587
_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^)+(0.0620P)^2^+19.3718P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1471
_refine_ls_wR_factor_ref         0.1714
_reflns_Friedel_coverage         0.000
_reflns_number_gt                11155
_reflns_number_total             18491
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d3ce00081h2.cif
_cod_data_source_block           3
_cod_depositor_comments
'Adding full bibliography for 7246576--7246583.cif.'
_cod_database_code               7246582
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   0.783
_shelx_estimated_absorpt_t_min   0.735
_olex2_refinement_description
;
1. Restrained distances
 O24-H24B
 0.86 with sigma of 0.02
 O22-H22A
 0.87 with sigma of 0.02
 O19-H19B
 0.87 with sigma of 0.02
 O21-H21B
 0.87 with sigma of 0.02
 O23-H23B
 0.87 with sigma of 0.02
2.a Free rotating group:
 O18(H18A,H18B), O20(H20D,H20E), O22(H23B,H21B,H19B,H22A,H24B,H22B)
2.b Rotating group:
 O17(H17A,H17B), O19(H19A), O21(H21A), O23(H23A), O24(H24A)
2.c Aromatic/amide H refined with riding coordinates:
 C1(H1), C2(H2), C4(H4), C5(H5), C6(H6), C7(H7), C9(H9), C10(H10), C11(H11),
 C12(H12), C14(H14), C15(H15), C21(H21), C22(H22), C24(H24), C25(H25), C26(H26),
  C27(H27), C29(H29), C30(H30), C36(H36), C37(H37), C39(H39), C40(H40),
 C41(H41), C42(H42), C44(H44), C45(H45), C51(H51), C52(H52), C54(H54), C55(H55)
2.d Idealised Me refined as rotating group:
 C19(H19C,H19D,H19E), C20(H20A,H20B,H20C), C34(H34A,H34B,H34C), C35(H35A,H35B,
 H35C), C49(H49A,H49B,H49C), C50(H50A,H50B,H50C), C59(H59A,H59B,H59C), C60(H60A,
 H60B,H60C)
;
_shelx_res_checksum              25829
_olex2_submission_special_instructions 'No special instructions were received'