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_1549163
_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         '0.25(C68 H64 N8 O16 Zn4), 0.25(H2 O)'
_chemical_formula_sum            'C17 H17 N2 O4.25 Zn'
_chemical_formula_weight         382.69
_chemical_name_systematic
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Catena((mu-Dimethylmalonato-O,O')(mu-1,2-bis(4-pyridine)ethylene-N,N')-
zinc(II) (mu-Dimethylmalonato-O,O')(mu!4$-tetrakis(4-
pyridyl)cyclobutane-N,N',N'',N''')-
zinc(II) hydrate)
;
_space_group_crystal_system      orthorhombic
_space_group_IT_number           52
_space_group_name_Hall           '-P 2a 2bc'
_space_group_name_H-M_alt        'P n n a'
_symmetry_space_group_name_Hall  '-P 2a 2bc'
_symmetry_space_group_name_H-M   'P n n a'
_atom_sites_solution_hydrogens   mixed
_audit_creation_date             2017-08-14
_audit_creation_method
;
Olex2 1.2
(compiled 2017.07.20 svn.r3457 for OlexSys, GUI svn.r5370)
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   8.3000(17)
_cell_length_b                   10.400(2)
_cell_length_c                   19.740(4)
_cell_measurement_reflns_used    259
_cell_measurement_temperature    100
_cell_measurement_theta_max      37.22
_cell_measurement_theta_min      4.79
_cell_volume                     1704.0(6)
_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      100
_diffrn_measured_fraction_theta_full 0.948
_diffrn_measured_fraction_theta_max 0.889
_diffrn_measurement_device_type  'Mar CCD'
_diffrn_measurement_method       '\f scans'
_diffrn_radiation_type           synchrotron
_diffrn_radiation_wavelength     0.9699
_diffrn_reflns_av_R_equivalents  0.0868
_diffrn_reflns_av_unetI/netI     0.0784
_diffrn_reflns_Laue_measured_fraction_full 0.948
_diffrn_reflns_Laue_measured_fraction_max 0.889
_diffrn_reflns_limit_h_max       8
_diffrn_reflns_limit_h_min       -8
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -10
_diffrn_reflns_limit_l_max       25
_diffrn_reflns_limit_l_min       -24
_diffrn_reflns_number            10296
_diffrn_reflns_point_group_measured_fraction_full 0.948
_diffrn_reflns_point_group_measured_fraction_max 0.889
_diffrn_reflns_theta_full        35.587
_diffrn_reflns_theta_max         38.514
_diffrn_reflns_theta_min         4.513
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    3.318
_exptl_absorpt_correction_T_max  0.7462
_exptl_absorpt_correction_T_min  0.6453
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   SCALA
_exptl_crystal_colour            colourless
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.492
_exptl_crystal_description       prism
_exptl_crystal_F_000             788
_exptl_crystal_size_max          0.53
_exptl_crystal_size_mid          0.49
_exptl_crystal_size_min          0.26
_refine_diff_density_max         0.627
_refine_diff_density_min         -0.887
_refine_diff_density_rms         0.099
_refine_ls_extinction_coef       0.0051(16)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     SHELXL
_refine_ls_goodness_of_fit_ref   1.045
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     117
_refine_ls_number_reflns         1696
_refine_ls_number_restraints     30
_refine_ls_restrained_S_all      1.073
_refine_ls_R_factor_all          0.1459
_refine_ls_R_factor_gt           0.0934
_refine_ls_shift/su_max          0.009
_refine_ls_shift/su_mean         0.006
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0200P)^2^+10.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1857
_refine_ls_wR_factor_ref         0.2141
_reflns_Friedel_coverage         0.000
_reflns_number_gt                976
_reflns_number_total             1696
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            lq5010.cif
_cod_data_source_block           2a
_cod_database_code               1549163
_shelxl_version_number           2014-3
_olex2_refinement_description
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1. Others
 Fixed Sof: C1(0.5) H1(0.5) C2(0.5) H2(0.5) C3(0.5) C4(0.5) H4(0.5) C5(0.5)
 H5(0.5) O3(0.125) H3A(0.25) H3B(0.25) C1A(0.5) H1A(0.5) C5A(0.5) H5A(0.5)
 C2A(0.5) H2A(0.5) C3A(0.5) C4A(0.5) H4A(0.5) C1AA(0.5) C0AA(0.25) C2AA(0.25)
 C9B(0.5) H9BA(0.5) H9BB(0.5) H9BC(0.5) C9A(0.5) H9AA(0.5) H9AB(0.5) H9AC(0.5)
 Fixed U12: C8(0)
 Fixed U13: Zn1(0) C8(0) O3(0)
 Fixed U23: Zn1(0) O3(0)
 Fixed Uiso: H1(0.076) H2(0.066) H4(0.083) H5(0.081) H3A(0.12) H3B(0.12)
 H1A(0.076) H5A(0.081) H2A(0.066) H4A(0.083) H9BA(0.143) H9BB(0.143)
 H9BC(0.143) H9AA(0.127) H9AB(0.127) H9AC(0.127)
 Fixed X: Zn1(0.75) H1(0.6612) H2(0.5728) H4(0.4694) H5(0.519) O3(0.25)
 H3A(0.3021) H3B(0.1816) H1A(0.7171) H5A(0.6351) H2A(0.6261) H4A(0.5631)
 H9BA(0.2399) H9BB(0.2517) H9BC(0.3987) H9AA(0.2402) H9AB(0.1665) H9AC(0.2976)
 Fixed Y: Zn1(0.5) H1(0.7859) H2(0.9531) H4(0.6987) H5(0.5367) C8(0.25)
 O3(0.5) H3A(0.4881) H3B(0.44) H1A(0.7855) H5A(0.5275) H2A(0.9435) H4A(0.6879)
 H9BA(0.3942) H9BB(0.2668) H9BC(0.3663) H9AA(0.3992) H9AB(0.277) H9AC(0.3653)
 Fixed Z: H1(0.3109) H2(0.3739) H4(0.5188) H5(0.4405) C8(0.25) H3A(0.3881)
 H3B(0.4297) H1A(0.3112) H5A(0.4586) H2A(0.3803) H4A(0.5328) H9BA(0.2029)
 H9BB(0.1577) H9BC(0.1593) H9AA(0.2547) H9AB(0.2164) H9AC(0.1794)
;
_shelx_res_checksum              21955
_shelx_hkl_checksum              22492
_olex2_submission_special_instructions 'No special instructions were received'