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_1549170
_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         'C24 H28 N4 O4 Zn, 2(C7 H10 O4)'
_chemical_formula_sum            'C38 H48 N4 O12 Zn'
_chemical_formula_weight         818.17
_chemical_name_systematic
;
(1,2-Bis(4-pyridine)ethylene-N)-tetraaqua-zinc(II) bis(hydrogen 
diethylmalonate)
;
_space_group_crystal_system      monoclinic
_space_group_IT_number           12
_space_group_name_Hall           '-C 2y'
_space_group_name_H-M_alt        'C 1 2/m 1'
_symmetry_space_group_name_Hall  '-C 2y'
_symmetry_space_group_name_H-M   'C 1 2/m 1'
_atom_sites_solution_hydrogens   mixed
_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                 117.532(2)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   22.881(2)
_cell_length_b                   6.8976(6)
_cell_length_c                   14.1573(12)
_cell_measurement_reflns_used    1056
_cell_measurement_temperature    120
_cell_measurement_theta_max      33.987
_cell_measurement_theta_min      2.005
_cell_volume                     1981.3(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_detector_area_resol_mean 8
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.994
_diffrn_measurement_device_type  'Bruker SMART APEX CCD area detector'
_diffrn_measurement_method       '\w and \f scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0392
_diffrn_reflns_av_unetI/netI     0.0374
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.994
_diffrn_reflns_limit_h_max       35
_diffrn_reflns_limit_h_min       -36
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_k_min       -10
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_number            17312
_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         34.599
_diffrn_reflns_theta_min         1.911
_diffrn_source                   'sealed tube'
_exptl_absorpt_coefficient_mu    0.686
_exptl_absorpt_correction_T_max  0.7468
_exptl_absorpt_correction_T_min  0.6615
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2014/5 (Bruker,2014/5) was used for absorption correction. wR2(int) 
was 0.1120 before and 0.0465 after correction. The Ratio of minimum to 
maximum transmission is 0.8858. The \l/2 correction factor is 0.00150.
;
_exptl_crystal_colour            colourless
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.371
_exptl_crystal_description       prism
_exptl_crystal_F_000             860
_exptl_crystal_size_max          0.7
_exptl_crystal_size_mid          0.52
_exptl_crystal_size_min          0.23
_refine_diff_density_max         2.141
_refine_diff_density_min         -1.678
_refine_diff_density_rms         0.095
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.033
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     182
_refine_ls_number_reflns         4490
_refine_ls_number_restraints     19
_refine_ls_restrained_S_all      1.178
_refine_ls_R_factor_all          0.0616
_refine_ls_R_factor_gt           0.0518
_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^)+(0.0620P)^2^+3.8680P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1252
_refine_ls_wR_factor_ref         0.1315
_reflns_Friedel_coverage         0.000
_reflns_number_gt                3929
_reflns_number_total             4490
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            lq5010.cif
_cod_data_source_block           8
_cod_database_code               1549170
_shelxl_version_number           2014-3
_olex2_refinement_description
;
1. Others
 Fixed Sof: C15(0.5) H15A(0.5) H15B(0.5) H15C(0.5) O4(0.5) O3(0.5) C14(0.5)
 H14A(0.5) H14B(0.5) C16(0.5) C17(0.5) H17A(0.5) H17B(0.5) C18(0.5) H18A(0.5)
 H18B(0.5) H18C(0.5)
 Fixed U12: Zn1(0) N1(0) N2(0) C9(0) C2(0) C007(0) C10(0) C6(0) C4(0) C3(0)
 C1(0) C8(0) C5(0) C7(0) C11(0) C12(0) C13(0)
 Fixed U23: Zn1(0) N1(0) N2(0) C9(0) C2(0) C007(0) C10(0) C6(0) C4(0) C3(0)
 C1(0) C8(0) C5(0) C7(0) C11(0) C12(0) C13(0)
 Fixed Uiso: H1A(0.024) H1B(0.024) H2(0.018) H007(0.019) H10(0.023) H6(0.019)
 H4(0.02) H1(0.018) H8(0.021) H5(0.022) H7(0.024) H11(0.023) H15A(0.065)
 H15B(0.065) H15C(0.065) H14A(0.041) H14B(0.041) H17A(0.048) H17B(0.048)
 H18A(0.083) H18B(0.083) H18C(0.083)
 Fixed X: Zn1(0.5) H1A(0.4736) H1B(0.4259) H2(0.2599) H007(0.4717) H10(0.0645)
 H6(0.1816) H4(0.3842) H1(0.3506) H8(0.1944) H5(0.2682) H7(0.1059) H11(-0.02)
 H15A(0.3198) H15B(0.259) H15C(0.2931) H14A(0.2658) H14B(0.2319) H17A(0.1372)
 H17B(0.1616) H18A(0.0456) H18B(0.0652) H18C(0.041)
 Fixed Y: Zn1(0.5) H1A(0.1809) H1B(0.2976) N1(0.5) N2(0.5) C9(0.5) C2(0.5)
 H2(0.5) C007(0.5) H007(0.5) C10(0.5) H10(0.5) C6(0.5) H6(0.5) C4(0.5) H4(0.5)
 C3(0.5) C1(0.5) H1(0.5) C8(0.5) H8(0.5) C5(0.5) H5(0.5) C7(0.5) H7(0.5)
 C11(0.5) H11(0.5) C12(0) H15A(0.1182) H15B(0.0266) H15C(-0.0927) C13(0)
 H14A(0.1238) H14B(0.2425) H17A(0.3206) H17B(0.2344) H18A(0.2662) H18B(0.0422)
 H18C(0.128)
 Fixed Z: Zn1(0.5) H1A(0.5702) H1B(0.5658) H2(0.2239) H007(0.2632) H10(-
 0.0649) H6(0.0609) H4(0.093) H1(0.3896) H8(-0.1853) H5(-0.0267) H7(-0.3537)
 H11(-0.2372) H15A(0.4684) H15B(0.4793) H15C(0.4211) H14A(0.305) H14B(0.3629)
 H17A(0.2293) H17B(0.1479) H18A(0.0612) H18B(0.0673) H18C(0.1484)
;
_shelx_res_checksum              76113
_shelx_hkl_checksum              24041
_olex2_submission_special_instructions 'No special instructions were received'