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_1549165
_publ_section_title
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 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         'C17 H18 N2 O4 Zn, H2 O'
_chemical_formula_sum            'C17 H20 N2 O5 Zn'
_chemical_formula_weight         397.72
_chemical_name_systematic
;
Catena((mu-Dimethylmalonato-O,O')(mu-1,2-bis(4-pyridine)ethane)-
zinc(II) monohydrate)
;
_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             2016-03-31
_audit_creation_method
;
Olex2 1.2
(compiled 2016.02.19 svn.r3266 for OlexSys, GUI svn.r5155)
;
_cell_angle_alpha                90
_cell_angle_beta                 115.928(4)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   8.4434(14)
_cell_length_b                   10.3811(18)
_cell_length_c                   21.551(4)
_cell_measurement_reflns_used    6048
_cell_measurement_temperature    120.0(2)
_cell_measurement_theta_max      32.46
_cell_measurement_theta_min      2.23
_cell_volume                     1698.8(5)
_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      120.0(2)
_diffrn_measured_fraction_theta_full 0.990
_diffrn_measured_fraction_theta_max 0.947
_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  0.0529
_diffrn_reflns_av_unetI/netI     0.0630
_diffrn_reflns_Laue_measured_fraction_full 0.990
_diffrn_reflns_Laue_measured_fraction_max 0.947
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       30
_diffrn_reflns_limit_l_min       -35
_diffrn_reflns_number            25908
_diffrn_reflns_point_group_measured_fraction_full 0.990
_diffrn_reflns_point_group_measured_fraction_max 0.947
_diffrn_reflns_theta_full        28.000
_diffrn_reflns_theta_max         36.592
_diffrn_reflns_theta_min         2.102
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    1.476
_exptl_absorpt_correction_T_max  0.7471
_exptl_absorpt_correction_T_min  0.5050
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2014/5 (Bruker,2014/5) was used for absorption correction.
wR2(int) was 0.1119 before and 0.0553 after correction.
The Ratio of minimum to maximum transmission is 0.6759.
The \l/2 correction factor is 0.00150.
;
_exptl_crystal_colour            colourless
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.555
_exptl_crystal_description       prism
_exptl_crystal_F_000             824
_exptl_crystal_size_max          0.32
_exptl_crystal_size_mid          0.21
_exptl_crystal_size_min          0.12
_refine_diff_density_max         3.116
_refine_diff_density_min         -0.765
_refine_diff_density_rms         0.152
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.999
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     232
_refine_ls_number_reflns         7954
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.999
_refine_ls_R_factor_all          0.0908
_refine_ls_R_factor_gt           0.0704
_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^)+(0.0150P)^2^+10.5140P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1450
_refine_ls_wR_factor_ref         0.1528
_reflns_Friedel_coverage         0.000
_reflns_number_gt                6155
_reflns_number_total             7954
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            lq5010.cif
_cod_data_source_block           4
_cod_database_code               1549165
_shelxl_version_number           2014-3
_olex2_refinement_description
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1. Others
 Fixed Uiso: H1WA(0.054) H6(0.022) H7(0.022) H9(0.021) H10(0.021) H11A(0.021)
 H11B(0.021) H5A(0.04) H5B(0.04) H5C(0.04) H4A(0.04) H4B(0.04) H4C(0.04)
 H16(0.024) H15(0.025) H13(0.019) H12(0.019) H17A(0.024) H17B(0.024)
 Fixed X: H1WA(0.4179) H1WB(0.3218) H6(0.672) H7(0.517) H9(0.6877) H10(0.8436)
 H11A(0.3533) H11B(0.5036) H5A(1.4214) H5B(1.4754) H5C(1.2754) H4A(1.4855)
 H4B(1.6031) H4C(1.5516) H16(0.9969) H15(1.0453) H13(1.0266) H12(0.9647)
 H17A(1.1806) H17B(1.1121)
 Fixed Y: H1WA(0.9927) H1WB(1.0708) H6(1.0243) H7(1.187) H9(1.4327)
 H10(1.2632) H11A(1.4152) H11B(1.4261) H5A(1.281) H5B(1.3998) H5C(1.3828)
 H4A(1.1327) H4B(1.2482) H4C(1.1298) H16(0.9604) H15(0.7981) H13(0.5411)
 H12(0.7091) H17A(0.4924) H17B(0.5808)
 Fixed Z: H1WA(0.104) H1WB(0.1088) H6(0.0385) H7(-0.0368) H9(0.1253)
 H10(0.1955) H11A(-0.0292) H11B(-0.055) H5A(0.1668) H5B(0.2194) H5C(0.1632)
 H4A(0.3258) H4B(0.3194) H4C(0.2666) H16(0.0572) H15(-0.0059) H13(0.1314)
 H12(0.1877) H17A(0.0501) H17B(-0.0176)
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_shelx_res_checksum              83130
_shelx_hkl_checksum              46887
_olex2_submission_special_instructions 'No special instructions were received'