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_1549166
_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 N3 O4 Zn, H2 O'
_chemical_formula_sum            'C22 H24 N3 O5 Zn'
_chemical_formula_weight         475.81
_chemical_name_systematic
;
Catena((mu-4,4'-bipyridine-N,N')-bis(4,4'-bipyridine)-bis(mu-diethylmalonato-
O,O')-dizinc(II) dihydrate)
;
_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'
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/c 1'
_atom_sites_solution_hydrogens   mixed
_audit_creation_date             2017-03-21
_audit_creation_method
;
Olex2 1.2
(compiled 2017.03.02 svn.r3394 for OlexSys, GUI svn.r5324)
;
_cell_angle_alpha                90
_cell_angle_beta                 99.143(2)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   11.1832(8)
_cell_length_b                   8.2422(6)
_cell_length_c                   23.8320(17)
_cell_measurement_reflns_used    1045
_cell_measurement_temperature    120
_cell_measurement_theta_max      29.78
_cell_measurement_theta_min      1.92
_cell_volume                     2168.8(3)
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'XL (Sheldrick, 2008)'
_diffrn_ambient_temperature      120
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.994
_diffrn_measurement_device_type  'Bruker Smart 1000 CCD area detector'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0732
_diffrn_reflns_av_unetI/netI     0.0765
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.994
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_k_min       -10
_diffrn_reflns_limit_l_max       34
_diffrn_reflns_limit_l_min       -34
_diffrn_reflns_number            23649
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.994
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         30.868
_diffrn_reflns_theta_min         1.731
_exptl_absorpt_coefficient_mu    1.171
_exptl_absorpt_correction_T_max  0.3368
_exptl_absorpt_correction_T_min  0.2655
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2014/5 (Bruker,2014/5) was used for absorption correction.
wR2(int) was 0.0782 before and 0.0561 after correction.
The Ratio of minimum to maximum transmission is 0.7883.
The \l/2 correction factor is 0.00150.
;
_exptl_crystal_colour            colourless
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.457
_exptl_crystal_description       plate
_exptl_crystal_F_000             988
_exptl_crystal_size_max          0.42
_exptl_crystal_size_mid          0.3
_exptl_crystal_size_min          0.06
_refine_diff_density_max         0.438
_refine_diff_density_min         -0.453
_refine_diff_density_rms         0.095
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.013
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     282
_refine_ls_number_reflns         6785
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.013
_refine_ls_R_factor_all          0.0808
_refine_ls_R_factor_gt           0.0471
_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^)+(0.0400P)^2^+0.0490P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0891
_refine_ls_wR_factor_ref         0.1028
_reflns_Friedel_coverage         0.000
_reflns_number_gt                4755
_reflns_number_total             6785
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            lq5010.cif
_cod_data_source_block           5
_cod_database_code               1549166
_shelxl_version_number           2014-3
_shelx_estimated_absorpt_t_max   0.933
_shelx_estimated_absorpt_t_min   0.639
_olex2_refinement_description
;
1. Others
 Fixed Uiso: H4A(0.027) H4B(0.027) H5A(0.053) H5B(0.053) H5C(0.053) H6A(0.025)
 H6B(0.025) H7A(0.054) H7B(0.054) H7C(0.054) H8(0.03) H9(0.03) H11(0.024)
 H12(0.024) H13(0.023) H14(0.021) H16(0.021) H17(0.022) H19(0.023) H20(0.027)
 H21(0.026) H22(0.022) H1WA(0.06) H1WB(0.06)
 Fixed X: H4A(0.1626) H4B(0.0782) H5A(0.0243) H5B(0.1581) H5C(0.0711)
 H6A(0.3095) H6B(0.2044) H7A(0.1624) H7B(0.0593) H7C(0.1348) H8(0.5488)
 H9(0.5249) H11(0.5026) H12(0.5306) H13(0.7751) H14(0.9229) H16(0.7642)
 H17(0.6182) H19(0.8588) H20(1.0089) H21(1.2297) H22(1.0873) H1WA(1.2508)
 H1WB(1.2753)
 Fixed Y: H4A(0.9707) H4B(0.8167) H5A(1.0317) H5B(1.033) H5C(0.8808)
 H6A(0.5727) H6B(0.6705) H7A(0.4793) H7B(0.5654) H7C(0.4172) H8(1.0664)
 H9(1.2338) H11(1.6149) H12(1.4376) H13(1.0438) H14(0.8581) H16(0.5371)
 H17(0.7304) H19(0.3507) H20(0.1649) H21(0.5069) H22(0.706) H1WA(0.0895) H1WB(-
 0.0344)
 Fixed Z: H4A(0.2516) H4B(0.2566) H5A(0.3126) H5B(0.3484) H5C(0.3524)
 H6A(0.3427) H6B(0.3661) H7A(0.2649) H7B(0.2939) H7C(0.3252) H8(0.4462)
 H9(0.5216) H11(0.4139) H12(0.3419) H13(0.4148) H14(0.4494) H16(0.3319)
 H17(0.3016) H19(0.3856) H20(0.4164) H21(0.4823) H22(0.4537) H1WA(0.4633)
 H1WB(0.4393)
;
_shelx_res_checksum              9106
_shelx_hkl_checksum              24241
_olex2_submission_special_instructions 'No special instructions were received'