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_7246580
_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         'C22 H24 Cu N2 O8, 0.5(H2 O)'
_chemical_formula_sum            'C22 H25 Cu N2 O8.5'
_chemical_formula_weight         516.98
_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
_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
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2023-03-28 deposited with the CCDC.	2023-04-06 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 98.301(18)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   9.193(2)
_cell_length_b                   12.176(5)
_cell_length_c                   20.620(8)
_cell_measurement_reflns_used    789
_cell_measurement_temperature    100
_cell_measurement_theta_max      29.471
_cell_measurement_theta_min      2.942
_cell_volume                     2283.9(14)
_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)'
_diffrn_ambient_temperature      100
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device_type  'Bruker Quest'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0864
_diffrn_reflns_av_unetI/netI     0.0916
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       29
_diffrn_reflns_limit_l_min       -29
_diffrn_reflns_number            27039
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         30.527
_diffrn_reflns_theta_min         1.948
_diffrn_source_current           1.4
_diffrn_source_power             0.07
_diffrn_source_voltage           50.0
_exptl_absorpt_coefficient_mu    1.010
_exptl_absorpt_correction_T_max  0.7461
_exptl_absorpt_correction_T_min  0.6727
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2016/2 (Bruker,2016/2) was used for absorption correction.
wR2(int) was 0.1176 before and 0.0630 after correction.
The Ratio of minimum to maximum transmission is 0.9016.
The \l/2 correction factor is Not present.
;
_exptl_crystal_colour            violet
_exptl_crystal_colour_primary    violet
_exptl_crystal_density_diffrn    1.504
_exptl_crystal_description       plate
_exptl_crystal_F_000             1072
_exptl_crystal_size_max          0.29
_exptl_crystal_size_mid          0.22
_exptl_crystal_size_min          0.03
_refine_diff_density_max         3.206
_refine_diff_density_min         -1.186
_refine_diff_density_rms         0.165
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.002
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     313
_refine_ls_number_reflns         6976
_refine_ls_number_restraints     42
_refine_ls_restrained_S_all      1.010
_refine_ls_R_factor_all          0.1371
_refine_ls_R_factor_gt           0.0883
_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^)+(0.0200P)^2^+28.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1828
_refine_ls_wR_factor_ref         0.2072
_reflns_Friedel_coverage         0.000
_reflns_number_gt                4503
_reflns_number_total             6976
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d3ce00081h2.cif
_cod_data_source_block           4
_cod_depositor_comments
'Adding full bibliography for 7246576--7246583.cif.'
_cod_original_cell_volume        2283.8(15)
_cod_original_formula_sum        'C22 H25 Cu N2 O8.50'
_cod_database_code               7246580
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   0.970
_shelx_estimated_absorpt_t_min   0.758
_olex2_refinement_description
;
1. Uiso/Uaniso restraints and constraints
Uanis(C10) \\sim Ueq: with sigma of 0.005 and sigma for terminal atoms of 0.005
Uanis(O8) \\sim Ueq: with sigma of 0.005 and sigma for terminal atoms of 0.005
2. Rigid body (RIGU) restrains
 C10, C7, C9, C8, C6
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
3. Others
 Fixed Sof: O1W(0.5) H1WA(0.5) H1WB(0.5)
4.a Riding coordinates:
 O1W(H1WA,H1WB)
4.b Aromatic/amide H refined with riding coordinates:
 C11(H11), C12(H12), C14(H14), C15(H15), C16(H16), C17(H17), C18(H18),
 C20(H20), C21(H21), C22(H22)
4.c Idealised Me refined as rotating group:
 C4(H4A,H4B,H4C), C5(H5A,H5B,H5C), C9(H9A,H9B,H9C), C10(H10A,H10B,H10C)
4.d Idealised tetrahedral OH refined as rotating group:
 O3(H3), O7(H7)
;
_shelx_res_checksum              76262
_olex2_submission_special_instructions 'No special instructions were received'