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_7246581
_publ_section_title
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 Design and synthesis of copper(ii) malonates with N,N&#x2032;-containing
 linkers
;
_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 H70 Cu4 N6 O16, 5(H2 O)'
_chemical_formula_sum            'C64 H80 Cu4 N6 O21'
_chemical_formula_weight         1523.50
_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   mixed
_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                 97.09(3)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   20.737(4)
_cell_length_b                   8.4420(17)
_cell_length_c                   40.952(8)
_cell_measurement_reflns_used    3587
_cell_measurement_temperature    100
_cell_measurement_theta_max      26.364
_cell_measurement_theta_min      2.487
_cell_volume                     7114(2)
_computing_cell_refinement       'SAINT v8.34A (Bruker, 2013)'
_computing_data_reduction        'SAINT v8.34A (Bruker, 2013)'
_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      100.00
_diffrn_measured_fraction_theta_full 0.995
_diffrn_measured_fraction_theta_max 0.996
_diffrn_measurement_device_type  'Mar CCD area detector'
_diffrn_measurement_method       'omega scans'
_diffrn_radiation_wavelength     0.788
_diffrn_reflns_av_unetI/netI     0.0318
_diffrn_reflns_Laue_measured_fraction_full 0.995
_diffrn_reflns_Laue_measured_fraction_max 0.996
_diffrn_reflns_limit_h_max       26
_diffrn_reflns_limit_h_min       -26
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_l_max       53
_diffrn_reflns_limit_l_min       -42
_diffrn_reflns_number            8265
_diffrn_reflns_point_group_measured_fraction_full 0.995
_diffrn_reflns_point_group_measured_fraction_max 0.996
_diffrn_reflns_theta_full        28.216
_diffrn_reflns_theta_max         31.007
_diffrn_reflns_theta_min         2.334
_diffrn_source_current           30.0
_diffrn_source_power             1.5
_diffrn_source_voltage           50.0
_exptl_absorpt_coefficient_mu    1.653
_exptl_absorpt_correction_T_max  0.7461
_exptl_absorpt_correction_T_min  0.5837
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   SCALA
_exptl_crystal_colour            blue
_exptl_crystal_colour_primary    blue
_exptl_crystal_density_diffrn    1.422
_exptl_crystal_description       plate
_exptl_crystal_F_000             3160
_exptl_crystal_size_max          0.16
_exptl_crystal_size_mid          0.15
_exptl_crystal_size_min          0.02
_refine_diff_density_max         2.149
_refine_diff_density_min         -2.119
_refine_diff_density_rms         0.172
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.039
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     437
_refine_ls_number_reflns         8265
_refine_ls_number_restraints     6
_refine_ls_restrained_S_all      1.039
_refine_ls_R_factor_all          0.1042
_refine_ls_R_factor_gt           0.0864
_refine_ls_shift/su_max          0.000
_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^+100.0318P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2121
_refine_ls_wR_factor_ref         0.2228
_reflns_Friedel_coverage         0.000
_reflns_number_gt                6432
_reflns_number_total             8265
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d3ce00081h2.cif
_cod_data_source_block           6
_cod_depositor_comments
'Adding full bibliography for 7246576--7246583.cif.'
_cod_original_cell_volume        7114(3)
_cod_database_code               7246581
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   0.968
_shelx_estimated_absorpt_t_min   0.778
_olex2_refinement_description
;
1. Twinned data refinement
 Scales: 0.718(6)
 0.282(6)
2. 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, All O(H,H) groups
3. Uiso/Uaniso restraints and constraints
Uanis(O12) \\sim Ueq: with sigma of 0.005 and sigma for terminal atoms of 0.005
Uanis(O6) = Uanis(O5)
4. Others
 Fixed Sof: H10A(0.5) H10B(0.5) O11(0.5) H11C(0.5) H11D(0.5) O12(0.5)
 H12D(0.5) H12E(0.5)
5.a Riding coordinates:
 O9(H9A,H9B), O10(H10A,H10B), O11(H11C,H11D), O12(H12D,H12E)
5.b Secondary CH2 refined with riding coordinates:
 C4(H4A,H4B), C6(H6A,H6B), C11(H11A,H11B), C13(H13A,H13B)
5.c Aromatic/amide H refined with riding coordinates:
 C15(H15), C16(H16), C18(H18), C19(H19), C20(H20), C21(H21), C22(H22),
 C24(H24), C25(H25), C26(H26), C27(H27), C28(H28), C29(H29), C31(H31), C32(H32)
5.d Idealised Me refined as rotating group:
 C5(H5A,H5B,H5C), C7(H7A,H7B,H7C), C12(H12A,H12B,H12C), C14(H14A,H14B,H14C)
;
_shelx_res_checksum              92495
_olex2_submission_special_instructions 'No special instructions were received'