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_1549167
_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
'C10 H16 N2 O4 Zn, 2(C7 H11 O4), C10 H8 N2, 2(H2 O)'
_chemical_formula_sum            'C34 H50 N4 O14 Zn'
_chemical_formula_weight         804.15
_chemical_name_systematic
;
Catena((mu-4,4'-bipyridine-N,N')-tetraaqua-zinc(II) bis(hydrogen 
diethylmalonate) 4,4'-bipyridine dihydrate)
;
_space_group_crystal_system      monoclinic
_space_group_IT_number           15
_space_group_name_Hall           '-C 2yc'
_space_group_name_H-M_alt        'C 1 2/c 1'
_symmetry_space_group_name_Hall  '-C 2yc'
_symmetry_space_group_name_H-M   'C 1 2/c 1'
_atom_sites_solution_hydrogens   mixed
_audit_creation_date             2016-04-26
_audit_creation_method
;
Olex2 1.2
(compiled 2016.02.19 svn.r3266 for OlexSys, GUI svn.r5155)
;
_cell_angle_alpha                90
_cell_angle_beta                 120.3080(10)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   22.6008(12)
_cell_length_b                   11.4154(6)
_cell_length_c                   17.1552(9)
_cell_measurement_reflns_used    5437
_cell_measurement_temperature    120
_cell_measurement_theta_max      30.76
_cell_measurement_theta_min      2.64
_cell_volume                     3821.1(4)
_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 0.995
_diffrn_measured_fraction_theta_max 0.925
_diffrn_measurement_device_type  apex
_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  0.0291
_diffrn_reflns_av_unetI/netI     0.0269
_diffrn_reflns_Laue_measured_fraction_full 0.995
_diffrn_reflns_Laue_measured_fraction_max 0.925
_diffrn_reflns_limit_h_max       34
_diffrn_reflns_limit_h_min       -34
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       26
_diffrn_reflns_limit_l_min       -26
_diffrn_reflns_number            27960
_diffrn_reflns_point_group_measured_fraction_full 0.995
_diffrn_reflns_point_group_measured_fraction_max 0.925
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         33.701
_diffrn_reflns_theta_min         2.067
_diffrn_source                   'sealed tube'
_exptl_absorpt_coefficient_mu    0.713
_exptl_absorpt_correction_T_max  0.7466
_exptl_absorpt_correction_T_min  0.5685
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2014/5 (Bruker,2014/5) was used for absorption correction.
wR2(int) was 0.0902 before and 0.0395 after correction.
The Ratio of minimum to maximum transmission is 0.7615.
The \l/2 correction factor is 0.00150.
;
_exptl_crystal_colour            colourless
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.398
_exptl_crystal_description       prism
_exptl_crystal_F_000             1696
_exptl_crystal_size_max          0.46
_exptl_crystal_size_mid          0.28
_exptl_crystal_size_min          0.13
_refine_diff_density_max         0.399
_refine_diff_density_min         -0.481
_refine_diff_density_rms         0.070
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.021
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     264
_refine_ls_number_reflns         7041
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.021
_refine_ls_R_factor_all          0.0381
_refine_ls_R_factor_gt           0.0289
_refine_ls_shift/su_max          0.003
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0381P)^2^+1.5000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0708
_refine_ls_wR_factor_ref         0.0749
_reflns_Friedel_coverage         0.000
_reflns_number_gt                5947
_reflns_number_total             7041
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            lq5010.cif
_cod_data_source_block           6
_cod_database_code               1549167
_shelxl_version_number           2014-3
_shelx_estimated_absorpt_t_max   0.913
_shelx_estimated_absorpt_t_min   0.735
_olex2_refinement_description
;
1. Others
 Fixed U12: Zn01(0) N1(0) N2(0) C3(0) C4(0)
 Fixed U23: Zn01(0) N1(0) N2(0) C3(0) C4(0)
 Fixed Uiso: H1A(0.025) H1(0.017) H2(0.016) H5(0.015) H6A(0.015) H15A(0.029)
 H15B(0.029) H16A(0.062) H16B(0.062) H16C(0.062) H17A(0.029) H17B(0.029)
 H18A(0.063) H18B(0.063) H18C(0.063) H7(0.024) H8(0.023) H10(0.022) H11(0.024)
 H7A(0.041) H7B(0.041)
 Fixed X: Zn01(0.5) H1A(0.3831) N1(0.5) N2(0.5) H1(0.5648) H2(0.5664) C3(0.5)
 C4(0.5) H5(0.5853) H6A(0.5845) H15A(0.1985) H15B(0.1776) H16A(0.284)
 H16B(0.2378) H16C(0.3008) H17A(0.1618) H17B(0.183) H18A(0.2527) H18B(0.2682)
 H18C(0.1969) H7(0.4308) H8(0.4131) H10(0.6004) H11(0.6114) H7A(0.7092)
 H7B(0.6879)
 Fixed Y: H1A(0.4978) H1(0.7125) H2(0.9155) H5(1.0941) H6A(1.2972)
 H15A(0.3954) H15B(0.3846) H16A(0.2888) H16B(0.2169) H16C(0.2937) H17A(0.6081)
 H17B(0.6056) H18A(0.744) H18B(0.746) H18C(0.7952) H7(0.682) H8(0.8765)
 H10(0.9487) H11(0.7517) H7A(0.9914) H7B(1.003)
 Fixed Z: Zn01(0.75) H1A(0.7342) N1(0.75) N2(0.75) H1(0.8809) H2(0.8853)
 C3(0.75) C4(0.75) H5(0.8747) H6A(0.8687) H15A(0.395) H15B(0.2913) H16A(0.337)
 H16B(0.3666) H16C(0.4394) H17A(0.2802) H17B(0.3843) H18A(0.3168) H18B(0.4188)
 H18C(0.339) H7(0.9528) H8(0.9099) H10(1.1241) H11(1.1616) H7A(1.0097)
 H7B(1.0723)
;
_shelx_res_checksum              40556
_shelx_hkl_checksum              79726
_olex2_submission_special_instructions 'No special instructions were received'