Exploitation of knowledge databases in the synthesis of zinc(II) malonates with photo-sensitive and photo-insensitive <i>N</i>,<i>N</i>'-containing linkers
Zorina-Tikhonova, Ekaterina N.; Chistyakov, Aleksandr S.; Kiskin, Mikhail A.; Sidorov, Aleksei A.; Dorovatovskii, Pavel V.; Zubavichus, Yan V.; Voronova, Eugenia D.; Godovikov, Ivan A.; Korlyukov, Alexander A.; Eremenko, Igor L.; Vologzhanina, Anna V.; IUCrJ 5 (2018) –; doi:10.1107/S2052252518001641

data_1549169
_publ_section_title
;
 Exploitation of knowledge databases in the synthesis of zinc(II)
 malonates with photo-sensitive and photo-insensitive
 <i>N</i>,<i>N</i>'-containing linkers
;
_journal_issue                   3
_journal_name_full               IUCrJ
_journal_page_first
;
;
_journal_paper_doi               10.1107/S2052252518001641
_journal_volume                  5
_journal_year                    2018
_chemical_formula_moiety         'C22 H22.5 N2.5 O4 Zn'
_chemical_formula_sum            'C22 H22.5 N2.5 O4 Zn'
_chemical_formula_weight         451.29
_chemical_name_systematic
;
Catena(tris(mu-1,2-bis(4-pyridine)ethylene-N,N')-(mu-tetrakis(4-pyridyl)
cyclobutane-N,N')-tetrakis(mu-diethylmalonato-O,O')-tetrazinc(II)
;
_space_group_crystal_system      orthorhombic
_space_group_IT_number           60
_space_group_name_Hall           '-P 2n 2ab'
_space_group_name_H-M_alt        'P b c n'
_symmetry_space_group_name_Hall  '-P 2n 2ab'
_symmetry_space_group_name_H-M   'P b c n'
_atom_sites_solution_hydrogens   geom
_audit_creation_method           SHELXL-2014
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   9.845(8)
_cell_length_b                   22.082(17)
_cell_length_c                   21.905(17)
_cell_measurement_reflns_used    3429
_cell_measurement_temperature    120(2)
_cell_measurement_theta_max      24.95
_cell_measurement_theta_min      2.09
_cell_volume                     4762(6)
_computing_structure_refinement  'SHELXL-2014 (Sheldrick, 2014)'
_diffrn_ambient_temperature      120(2)
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.982
_diffrn_measurement_device_type  'Bruker Apex II CCD area detector'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.2024
_diffrn_reflns_av_unetI/netI     0.1287
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.982
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       31
_diffrn_reflns_limit_k_min       -31
_diffrn_reflns_limit_l_max       31
_diffrn_reflns_limit_l_min       -31
_diffrn_reflns_number            40353
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.982
_diffrn_reflns_theta_full        26.000
_diffrn_reflns_theta_max         30.741
_diffrn_reflns_theta_min         1.859
_exptl_absorpt_coefficient_mu    1.059
_exptl_absorpt_correction_T_max  0.903
_exptl_absorpt_correction_T_min  0.786
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   SADABS
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.259
_exptl_crystal_description       prism
_exptl_crystal_F_000             1872
_exptl_crystal_size_max          0.43
_exptl_crystal_size_mid          0.29
_exptl_crystal_size_min          0.21
_refine_diff_density_max         1.291
_refine_diff_density_min         -0.764
_refine_diff_density_rms         0.104
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.008
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     252
_refine_ls_number_reflns         7285
_refine_ls_number_restraints     21
_refine_ls_restrained_S_all      1.008
_refine_ls_R_factor_all          0.2350
_refine_ls_R_factor_gt           0.1144
_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^)+(0.0300P)^2^+41.9000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1887
_refine_ls_wR_factor_ref         0.2372
_reflns_Friedel_coverage         0.000
_reflns_number_gt                3089
_reflns_number_total             7285
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            lq5010.cif
_cod_data_source_block           7a
_cod_original_formula_sum        'C22 H22.50 N2.50 O4 Zn'
_cod_database_code               1549169
_shelxl_version_number           2014-3
_olex2_refinement_description
;
1. Others
 Fixed Sof: N3(0.5) C24(0.5) H24(0.5) C25(0.5) H25(0.5) C21(0.5) C22(0.5)
 H22(0.5) C23(0.5) H23(0.5) C20(0.5) H20(0.5)
 Fixed Uiso: H24(0.233) H25(0.233) H22(0.233) H23(0.233) H4A(0.077) H4B(0.077)
 H5A(0.148) H5B(0.148) H5C(0.148) H6A(0.078) H6B(0.078) H7A(0.15) H7B(0.15)
 H7C(0.15) H8(0.054) H9(0.059) H11(0.059) H12(0.054) H13(0.066) H14(0.074)
 H15(0.086) H17(0.121) H18(0.1) H19(0.117) H20(0.233)
 Fixed X: H24(0.6863) H25(0.8869) H22(0.7079) H23(0.5074) H4A(0.5671)
 H4B(0.6515) H5A(0.46) H5B(0.5387) H5C(0.4304) H6A(0.8688) H6B(0.7465)
 H7A(0.9442) H7B(0.8274) H7C(0.9446) H8(0.2064) H9(0.0433) H11(0.3232)
 H12(0.4792) H13(0.1006) H14(0.7977) H15(0.9655) H17(0.6808) H18(0.5228)
 H19(0.916) H20(0.9592)
 Fixed Y: H24(0.519) H25(0.4731) H22(0.4214) H23(0.4673) H4A(0.2802)
 H4B(0.3152) H5A(0.3724) H5B(0.4047) H5C(0.3547) H6A(0.3939) H6B(0.4213)
 H7A(0.347) H7B(0.3804) H7C(0.4179) H8(0.3088) H9(0.3807) H11(0.5092)
 H12(0.4345) H13(0.5423) H14(0.3128) H15(0.3225) H17(0.3053) H18(0.2997)
 H19(0.3032) H20(0.4104)
 Fixed Z: H24(0.3607) H25(0.3297) H22(0.1733) H23(0.2042) H4A(0.6504)
 H4B(0.6996) H5A(0.6231) H5B(0.6761) H5C(0.6911) H6A(0.5931) H6B(0.6294)
 H7A(0.6843) H7B(0.7194) H7C(0.6892) H8(0.4783) H9(0.4984) H11(0.4677)
 H12(0.4531) H13(0.499) H14(0.4458) H15(0.3726) H17(0.2452) H18(0.3193)
 H19(0.2064) H20(0.1896)
;
_shelx_res_checksum              78645
_shelx_hkl_checksum              95021