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_1549171
_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
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_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
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Catena(1,2-Bis(4-pyridine)ethylene-N)-tetraaqua-zinc(II) (mu-tetrakis(4-pyridyl)
cyclobutane-N,N')-tetraaqua-zinc(II) tetrakis(hydrogen diethylmalonate)
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_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
_atom_sites_solution_primary     dual
_audit_creation_date             2016-10-28
_audit_creation_method
;
Olex2 1.2
(compiled 2016.09.09 svn.r3337 for OlexSys, GUI svn.r5227)
;
_cell_angle_alpha                90
_cell_angle_beta                 110.021(1)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   26.8028(19)
_cell_length_b                   6.8933(5)
_cell_length_c                   23.0690(17)
_cell_measurement_reflns_used    3655
_cell_measurement_temperature    120
_cell_measurement_theta_max      30.43
_cell_measurement_theta_min      2.87
_cell_volume                     4004.6(5)
_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 0.994
_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  0.0499
_diffrn_reflns_av_unetI/netI     0.0461
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.994
_diffrn_reflns_limit_h_max       38
_diffrn_reflns_limit_h_min       -38
_diffrn_reflns_limit_k_max       9
_diffrn_reflns_limit_k_min       -9
_diffrn_reflns_limit_l_max       32
_diffrn_reflns_limit_l_min       -33
_diffrn_reflns_number            25740
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.994
_diffrn_reflns_theta_full        26.000
_diffrn_reflns_theta_max         30.630
_diffrn_reflns_theta_min         1.617
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.679
_exptl_absorpt_correction_T_max  0.3368
_exptl_absorpt_correction_T_min  0.2936
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2014/5 (Bruker,2014/5) was used for absorption correction.
wR2(int) was 0.0672 before and 0.0464 after correction.
The Ratio of minimum to maximum transmission is 0.8717.
The \l/2 correction factor is 0.00150.
;
_exptl_crystal_colour            colourless
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.357
_exptl_crystal_description       prism
_exptl_crystal_F_000             1720
_exptl_crystal_size_max          0.68
_exptl_crystal_size_mid          0.35
_exptl_crystal_size_min          0.19
_refine_diff_density_max         0.665
_refine_diff_density_min         -0.359
_refine_diff_density_rms         0.069
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.033
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     314
_refine_ls_number_reflns         6154
_refine_ls_number_restraints     4
_refine_ls_restrained_S_all      1.033
_refine_ls_R_factor_all          0.0950
_refine_ls_R_factor_gt           0.0549
_refine_ls_shift/su_max          0.004
_refine_ls_shift/su_mean         0.001
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.1000P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1497
_refine_ls_wR_factor_ref         0.1762
_reflns_Friedel_coverage         0.000
_reflns_number_gt                3847
_reflns_number_total             6154
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            lq5010.cif
_cod_data_source_block           8a
_cod_database_code               1549171
_shelxl_version_number           2014-3
_olex2_refinement_description
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1. Others
 Fixed Sof: H9A(0.5) H9B(0.5) H12(0.5) H12A(0.5) C1(0.15) H1(0.15) C2(0.15)
 H2(0.15) C8(0.5) C11(0.5) H11(0.5) C1A(0.425) C2A(0.425) C1B(0.425) C2B(0.425)
 C8A(0.5) C11A(0.5) H11A(0.5) H1AA(0.85) H2BA(0.425) H2AA(0.425)
 Fixed U12: Zn1(0)
 Fixed U23: Zn1(0)
 Fixed Uiso: H1A(0.046) H2A(0.046) H1B(0.045) H2B(0.045) H4(0.037) H5(0.03)
 H6(0.034) H7(0.044) H9A(0.047) H9B(0.047) H10(0.034) H12(0.04) H12A(0.04)
 H1(0.034) H2(0.025) H11(0.045) H11A(0.041) H13A(0.089) H13B(0.089) H13C(0.089)
 H14A(0.059) H14B(0.059) H16A(0.085) H16B(0.085) H17A(0.15) H17B(0.15)
 H17C(0.15) H1AA(0.053) H2BA(0.053) H2AA(0.053)
 Fixed X: Zn1(0.5) H1A(0.5371) H2A(0.4722) H1B(0.5312) H2B(0.4623) H4(0.6501)
 H5(0.5632) H6(0.6997) H7(0.6121) H9A(0.8441) H9B(0.8444) H10(0.9269)
 H12(0.8596) H12A(0.8605) H1(0.765) H2(0.7255) H11(0.7808) H11A(0.778)
 H13A(0.4897) H13B(0.4914) H13C(0.4508) H14A(0.4453) H14B(0.4053) H16A(0.3669)
 H16B(0.3287) H17A(0.2869) H17B(0.3279) H17C(0.2854)
 Fixed Y: H1A(0.5579) H2A(0.0419) H1B(0.4281) H2B(-0.0758) H4(0.2473)
 H5(0.2449) H6(0.236) H7(0.2368) H9A(0.1907) H9B(0.2775) H10(0.2336)
 H12(0.2077) H12A(0.2779) H1(0.1925) H2(0.2422) H11(0.321) H11A(0.179)
 H13A(0.244) H13B(0.3155) H13C(0.4131) H14A(0.0212) H14B(0.1154) H16A(-0.0794)
 H16B(0.0228) H17A(0.2034) H17B(0.1222) H17C(-0.0206)
 Fixed Z: Zn1(0.75) H1A(0.8152) H2A(0.6454) H1B(0.8547) H2B(0.6849) H4(0.6628)
 H5(0.661) H6(0.8492) H7(0.8427) H9A(0.791) H9B(0.7917) H10(0.7816) H12(0.602)
 H12A(0.6026) H1(0.7713) H2(0.6479) H11(0.6099) H11A(0.6072) H13A(0.4123)
 H13B(0.4789) H13C(0.4181) H14A(0.4538) H14B(0.3921) H16A(0.4804) H16B(0.419)
 H17A(0.4762) H17B(0.5397) H17C(0.4938)
;
_shelx_res_checksum              65416
_shelx_hkl_checksum              69310
_olex2_submission_special_instructions 'No special instructions were received'