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_1549168
_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         'C19 H20 N2 O4 Zn, 0.25(C12 H10 N2)'
_chemical_formula_sum            'C22 H22.5 N2.5 O4 Zn'
_chemical_formula_weight         451.29
_chemical_name_systematic
;
Catena((mu-1,2-bis(4-pyridine)ethylene-N,N')-
(mu-diethylmalonato-O,O')-zinc(II) 1,2-bis(4-pyridine)ethylene solvate)
;
_space_group_crystal_system      orthorhombic
_space_group_IT_number           63
_space_group_name_Hall           '-C 2c 2'
_space_group_name_H-M_alt        'C m c m'
_symmetry_space_group_name_Hall  '-C 2c 2'
_symmetry_space_group_name_H-M   'C m c m'
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     dual
_audit_creation_date             2017-08-02
_audit_creation_method
;
Olex2 1.2
(compiled 2017.03.28 svn.r3405 for OlexSys, GUI svn.r5337)
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   9.8266(5)
_cell_length_b                   22.0654(12)
_cell_length_c                   22.1641(11)
_cell_measurement_reflns_used    3505
_cell_measurement_temperature    120
_cell_measurement_theta_max      25.87
_cell_measurement_theta_min      2.27
_cell_volume                     4805.8(4)
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'XL (Sheldrick, 2008)'
_computing_structure_solution    'ShelXT (Sheldrick, 2015)'
_diffrn_ambient_temperature      120
_diffrn_measured_fraction_theta_full 0.990
_diffrn_measured_fraction_theta_max 0.988
_diffrn_measurement_device_type  'Bruker Smart 1000 CCD area detector'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0822
_diffrn_reflns_av_unetI/netI     0.0672
_diffrn_reflns_Laue_measured_fraction_full 0.990
_diffrn_reflns_Laue_measured_fraction_max 0.988
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       30
_diffrn_reflns_limit_k_min       -30
_diffrn_reflns_limit_l_max       30
_diffrn_reflns_limit_l_min       -30
_diffrn_reflns_number            22224
_diffrn_reflns_point_group_measured_fraction_full 0.990
_diffrn_reflns_point_group_measured_fraction_max 0.988
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         29.244
_diffrn_reflns_theta_min         2.062
_exptl_absorpt_coefficient_mu    1.050
_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            colourless
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.247
_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         0.972
_refine_diff_density_min         -1.030
_refine_diff_density_rms         0.101
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.000
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     209
_refine_ls_number_reflns         3498
_refine_ls_number_restraints     7
_refine_ls_restrained_S_all      1.005
_refine_ls_R_factor_all          0.0768
_refine_ls_R_factor_gt           0.0516
_refine_ls_shift/su_max          0.008
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0600P)^2^+15.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1293
_refine_ls_wR_factor_ref         0.1398
_reflns_Friedel_coverage         0.000
_reflns_number_gt                2496
_reflns_number_total             3498
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            lq5010.cif
_cod_data_source_block           7
_cod_original_formula_sum        'C22 H22.50 N2.50 O4 Zn'
_cod_database_code               1549168
_shelxl_version_number           2014-3
_olex2_refinement_description
;
1. Others
 Fixed Sof: C12A(0.25) H12A(0.25) C12B(0.25) H12B(0.25) H6(0.5) N1(0.5)
 N2(0.5) C1(0.5) H1(0.5) C2(0.5) H2(0.5) C3(0.5) C4(0.5) H4(0.5) C5(0.5)
 H5(0.5) C7(0.5) H7(0.5) C8(0.5) H8(0.5) C9(0.5) C10(0.5) H10(0.5) C11(0.5)
 H11(0.5) O1(0.5) O2(0.5) O3(0.5) O4(0.5) C13(0.5) C14(0.5) C15(0.5) C16(0.5)
 H16A(0.5) H16B(0.5) C17(0.5) H17A(0.5) H17B(0.5) H17C(0.5) C18(0.5) H18A(0.5)
 H18B(0.5) C19(0.5) H19A(0.5) H19B(0.5) H19C(0.5) N3(0.125) C12(0.125)
 H12(0.125) C1A(0.125) H1A(0.125) C1B(0.125) C1C(0.125) H1C(0.125) C1D(0.125)
 H1D(0.125) C1E(0.125) H1E(0.125) N9(0.125) C1F(0.125) C1G(0.125) H1G(0.125)
 C1H(0.125) C1I(0.125) H1I(0.125) C1J(0.125) H1J(0.125) C1K(0.125) H1K(0.125)
 Fixed U12: Zn1(0) C6(0) C2(0) C3(0) C4(0)
 Fixed U13: Zn1(0) C12A(0) C12B(0) C6(0) C2(0) C3(0) C4(0)
 Fixed U23: C12A(0) C12B(0)
 Fixed Uiso: H12A(0.028) H12B(0.028) H6(0.036) H1(0.027) H2(0.036) H4(0.036)
 H5(0.031) H7(0.047) H8(0.075) H10(0.075) H11(0.048) H16A(0.037) H16B(0.037)
 H17A(0.086) H17B(0.086) H17C(0.086) H18A(0.038) H18B(0.038) H19A(0.086)
 H19B(0.086) H19C(0.086) N3(0.06) C12(0.06) H12(0.072) C1A(0.06) H1A(0.072)
 C1B(0.06) C1C(0.06) H1C(0.072) C1D(0.06) H1D(0.072) C1E(0.06) H1E(0.072)
 N9(0.06) C1F(0.06) C1G(0.06) H1G(0.072) C1H(0.06) C1I(0.06) H1I(0.072)
 C1J(0.06) H1J(0.072) C1K(0.06) H1K(0.072)
 Fixed X: Zn1(0) H12A(0.3787) C12B(0.5) H12B(0.5884) H6(-0.3699) H1(-0.2939)
 H2(-0.4588) H4(-0.1741) H5(-0.0155) H7(0.0244) H8(0.1857) H10(0.4735)
 H11(0.303) H16A(0.4318) H16B(0.3375) H17A(0.5495) H17B(0.4347) H17C(0.5292)
 H18A(0.2334) H18B(0.1138) H19A(0.0371) H19B(0.1565) H19C(0.0369) H12(-0.0122)
 H1A(0.195) H1C(0.3823) H1D(0.1698) H1E(0.4409) H1G(0.8166) H1I(0.6293)
 H1J(0.8419) H1K(0.5708)
 Fixed Y: H12A(0.1909) H12B(0.1907) C6(0) H6(-0.0301) H1(0.191) H2(0.1196) H4(-
 0.0115) H5(0.0642) H7(0.1987) H8(0.1975) H10(0.1868) H11(0.1918) H16A(0.2855)
 H16B(0.3195) H17A(0.3664) H17B(0.4126) H17C(0.3786) H18A(0.423) H18B(0.3906)
 H19A(0.4156) H19B(0.3759) H19C(0.3435) H12(0.536) H1A(0.5443) H1C(0.5378)
 H1D(0.531) H1E(0.5472) H1G(0.5318) H1I(0.5382) H1J(0.5451) H1K(0.5288)
 Fixed Z: C12A(0.25) H12A(0.2154) H12B(0.2935) C6(0.5) H6(0.5088) H1(0.4775)
 H2(0.497) H4(0.4729) H5(0.4545) H7(0.3218) H8(0.2478) H10(0.3778) H11(0.4497)
 H16A(0.3485) H16B(0.3005) H17A(0.3056) H17B(0.3281) H17C(0.3762) H18A(0.3746)
 H18B(0.4114) H19A(0.3135) H19B(0.2844) H19C(0.3212) H12(0.2372) H1A(0.2867)
 H1C(0.1237) H1D(0.0793) H1E(0.286) H1G(0.1753) H1I(0.3383) H1J(0.3827)
 H1K(0.176)
;
_shelx_res_checksum              48159
_shelx_hkl_checksum              57703
_olex2_submission_special_instructions 'No special instructions were received'