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_1549162
_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         'C17 H16 N2 O4 Zn, H2 O'
_chemical_formula_sum            'C17 H18 N2 O5 Zn'
_chemical_formula_weight         395.70
_chemical_name_systematic
;
Catena((mu-Dimethylmalonato-O,O')(mu-1,2-bis(4-pyridine)ethylene)-
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
_atom_sites_solution_primary     dual
_audit_creation_date             2016-10-19
_audit_creation_method
;
Olex2 1.2
(compiled 2016.09.09 svn.r3337 for OlexSys, GUI svn.r5227)
;
_cell_angle_alpha                90
_cell_angle_beta                 117.282(3)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   8.2852(11)
_cell_length_b                   10.4999(14)
_cell_length_c                   21.684(3)
_cell_measurement_reflns_used    3437
_cell_measurement_temperature    120
_cell_measurement_theta_max      29.66
_cell_measurement_theta_min      2.21
_cell_volume                     1676.5(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_detector_area_resol_mean 8
_diffrn_measured_fraction_theta_full 0.996
_diffrn_measured_fraction_theta_max 0.987
_diffrn_measurement_device_type  'Bruker SMART APEX 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  0.0607
_diffrn_reflns_av_unetI/netI     0.0601
_diffrn_reflns_Laue_measured_fraction_full 0.996
_diffrn_reflns_Laue_measured_fraction_max 0.987
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       31
_diffrn_reflns_limit_l_min       -31
_diffrn_reflns_number            19935
_diffrn_reflns_point_group_measured_fraction_full 0.996
_diffrn_reflns_point_group_measured_fraction_max 0.987
_diffrn_reflns_theta_full        28.000
_diffrn_reflns_theta_max         31.498
_diffrn_reflns_theta_min         2.114
_diffrn_source                   'sealed tube'
_exptl_absorpt_coefficient_mu    1.496
_exptl_absorpt_correction_T_max  0.7462
_exptl_absorpt_correction_T_min  0.6453
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2014/5 (Bruker,2014/5) was used for absorption correction.
wR2(int) was 0.0774 before and 0.0550 after correction.
The Ratio of minimum to maximum transmission is 0.8648.
The \l/2 correction factor is 0.00150.
;
_exptl_crystal_colour            colourless
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.568
_exptl_crystal_description       prism
_exptl_crystal_F_000             816
_exptl_crystal_size_max          0.53
_exptl_crystal_size_mid          0.49
_exptl_crystal_size_min          0.26
_refine_diff_density_max         1.031
_refine_diff_density_min         -0.756
_refine_diff_density_rms         0.110
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.998
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     236
_refine_ls_number_reflns         5502
_refine_ls_number_restraints     2
_refine_ls_restrained_S_all      0.998
_refine_ls_R_factor_all          0.0726
_refine_ls_R_factor_gt           0.0512
_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^+5.2300P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0948
_refine_ls_wR_factor_ref         0.1013
_reflns_Friedel_coverage         0.000
_reflns_number_gt                4217
_reflns_number_total             5502
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            lq5010.cif
_cod_data_source_block           2
_cod_database_code               1549162
_shelxl_version_number           2014-3
_olex2_refinement_description
;
1. Others
 Fixed Uiso: H1(0.019) H2(0.019) H4(0.021) H5(0.019) H6(0.02) H7(0.021)
 H8(0.019) H9(0.021) H11(0.018) H12(0.017) H16A(0.035) H16B(0.035) H16C(0.035)
 H17A(0.037) H17B(0.037) H17C(0.037)
 Fixed X: H1(-0.833) H2(-0.6864) H4(-0.5303) H5(-0.6763) H6(-0.442) H7(-
 1.0342) H8(-1.0156) H9(-1.0301) H11(-0.9703) H12(-0.9433) H16A(-0.7289) H16B(-
 0.5825) H16C(-0.5195) H17A(-0.3792) H17B(-0.4276) H17C(-0.4923)
 Fixed Y: H1(0.7562) H2(0.9287) H4(0.6997) H5(0.533) H6(0.921) H7(0.0909)
 H8(0.4662) H9(0.3097) H11(0.0454) H12(0.2086) H16A(0.3903) H16B(0.2897)
 H16C(0.4058) H17A(0.2616) H17B(0.1444) H17C(0.1432)
 Fixed Z: H1(0.3004) H2(0.369) H4(0.5375) H5(0.4636) H6(0.5576) H7(0.5393)
 H8(0.437) H9(0.5091) H11(0.3854) H12(0.3195) H16A(0.1644) H16B(0.1655)
 H16C(0.2193) H17A(0.3214) H17B(0.2686) H17C(0.3277)
;
_shelx_res_checksum              96096
_shelx_hkl_checksum              52517
_olex2_submission_special_instructions 'No special instructions were received'