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_1549161
_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
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_journal_coeditor_code           LQ5010
_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         '0.5(C40 H48 N4 O20 Zn4)'
_chemical_formula_sum            'C20 H24 N2 O10 Zn2'
_chemical_formula_weight         583.15
_chemical_name_systematic
;
Catena(bis(mu3-dimethylmalonato-O,O',O'',O''')-(mu2-4,4'-bipyridine-N,N')
-diaqua-dizinc(II))
;
_space_group_crystal_system      orthorhombic
_space_group_IT_number           58
_space_group_name_Hall           '-P 2 2n'
_space_group_name_H-M_alt        'P n n m'
_symmetry_space_group_name_Hall  '-P 2 2n'
_symmetry_space_group_name_H-M   'P n n m'
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     direct
_audit_creation_date             2016-03-16
_audit_creation_method
;
Olex2 1.2
(compiled 2016.02.19 svn.r3266 for OlexSys, GUI svn.r5155)
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   7.4159(16)
_cell_length_b                   19.318(4)
_cell_length_c                   7.3457(16)
_cell_measurement_reflns_used    1788
_cell_measurement_temperature    120
_cell_measurement_theta_max      28.83
_cell_measurement_theta_min      2.97
_cell_volume                     1052.3(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 0.998
_diffrn_measured_fraction_theta_max 0.958
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0938
_diffrn_reflns_av_unetI/netI     0.0764
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.958
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       31
_diffrn_reflns_limit_k_min       -31
_diffrn_reflns_limit_l_max       11
_diffrn_reflns_limit_l_min       -12
_diffrn_reflns_number            15845
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.958
_diffrn_reflns_theta_full        28.000
_diffrn_reflns_theta_max         36.737
_diffrn_reflns_theta_min         2.108
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    2.343
_exptl_absorpt_correction_T_max  0.3438
_exptl_absorpt_correction_T_min  0.2821
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2014/5 (Bruker,2014/5) was used for absorption correction.
wR2(int) was 0.0889 before and 0.0679 after correction.
The Ratio of minimum to maximum transmission is 0.8205.
The \l/2 correction factor is 0.00150.
;
_exptl_crystal_colour            colourless
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.840
_exptl_crystal_description       prism
_exptl_crystal_F_000             596
_exptl_crystal_size_max          0.15
_exptl_crystal_size_mid          0.11
_exptl_crystal_size_min          0.08
_refine_diff_density_max         0.828
_refine_diff_density_min         -2.177
_refine_diff_density_rms         0.159
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.043
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     103
_refine_ls_number_reflns         2674
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.043
_refine_ls_R_factor_all          0.1021
_refine_ls_R_factor_gt           0.0657
_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^+6.2000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1305
_refine_ls_wR_factor_ref         0.1448
_reflns_Friedel_coverage         0.000
_reflns_number_gt                1859
_reflns_number_total             2674
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            lq5010.cif
_cod_data_source_block           1
_cod_database_code               1549161
_shelxl_version_number           2014-3
_olex2_refinement_description
;
1. Others
 Fixed Sof: H3A(0.5) H3B(0.5) H3D(0.5) H3E(0.5) H3C(0.5) H4B(0.5) H4A(0.5)
 H4C(0.5) C9(0.5) H9(0.5) C8(0.5) H8(0.5) C7(0.5) H6(0.5)
 Fixed U13: Zn1(0) O3(0) N1(0) C6(0) C5(0) C2(0) C3(0) C4(0)
 Fixed U23: Zn1(0) O3(0) N1(0) C6(0) C5(0) C2(0) C3(0) C4(0)
 Fixed Uiso: H3A(0.029) H3B(0.029) H5(0.022) H3D(0.052) H3E(0.052) H3C(0.052)
 H4B(0.044) H4A(0.044) H4C(0.044) H9(0.02) H8(0.019) H6(0.022)
 Fixed X: H3A(0.2649) H3B(0.2603) H5(0.9016) H3D(0.8814) H3E(0.8971)
 H3C(1.0116) H4B(0.4648) H4A(0.5622) H4C(0.5482) H9(0.517) H8(0.7255)
 Fixed Y: H3A(0.8098) H3B(0.8074) H5(0.6947) H3D(0.9522) H3E(0.9453)
 H3C(0.8951) H4B(0.8739) H4A(0.9407) H4C(0.9311) H9(0.567) H8(0.476)
 Fixed Z: Zn1(0.5) O3(0.5) H3A(0.4078) H3B(0.5966) N1(0.5) C6(0.5) C5(0.5)
 H5(0.5) C2(0.5) C3(0.5) H3D(0.6013) H3E(0.3848) H3C(0.5139) C4(0.5)
 H4B(0.4833) H4A(0.4004) H4C(0.6163) H9(0.3879) H8(0.3701)
;
_shelx_res_checksum              37355
_shelx_hkl_checksum              34145
_olex2_submission_special_instructions 'No special instructions were received'