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_1549172
_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         'C19 H22 N2 O4 Zn, 0.38(H2 O)'
_chemical_formula_sum            'C19 H22.75 N2 O4.38 Zn'
_chemical_formula_weight         414.51
_chemical_name_systematic
;
 ?
;
_space_group_crystal_system      orthorhombic
_space_group_IT_number           20
_space_group_name_Hall           'C 2c 2'
_space_group_name_H-M_alt        'C 2 2 21'
_symmetry_space_group_name_Hall  'C 2c 2'
_symmetry_space_group_name_H-M   'C 2 2 21'
_atom_sites_solution_hydrogens   mixed
_audit_creation_date             2017-05-08
_audit_creation_method
;
Olex2 1.2
(compiled 2017.03.28 svn.r3405 for OlexSys, GUI svn.r5335)
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            16
_cell_length_a                   24.662(3)
_cell_length_b                   37.180(5)
_cell_length_c                   8.7826(12)
_cell_measurement_reflns_used    4172
_cell_measurement_temperature    120
_cell_measurement_theta_max      25.68
_cell_measurement_theta_min      2.52
_cell_volume                     8053.1(18)
_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      120.0
_diffrn_measured_fraction_theta_full 0.996
_diffrn_measured_fraction_theta_max 0.993
_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  0.1034
_diffrn_reflns_av_unetI/netI     0.1183
_diffrn_reflns_Laue_measured_fraction_full 0.996
_diffrn_reflns_Laue_measured_fraction_max 0.993
_diffrn_reflns_limit_h_max       35
_diffrn_reflns_limit_h_min       -35
_diffrn_reflns_limit_k_max       52
_diffrn_reflns_limit_k_min       -53
_diffrn_reflns_limit_l_max       12
_diffrn_reflns_limit_l_min       -12
_diffrn_reflns_number            41027
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.994
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         30.695
_diffrn_reflns_theta_min         2.191
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    1.247
_exptl_absorpt_correction_T_max  0.3368
_exptl_absorpt_correction_T_min  0.2620
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2014/5 (Bruker,2014/5) was used for absorption correction.
wR2(int) was 0.1078 before and 0.0719 after correction.
The Ratio of minimum to maximum transmission is 0.7779.
The \l/2 correction factor is 0.00150.
;
_exptl_crystal_colour            colourless
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.368
_exptl_crystal_description       prism
_exptl_crystal_F_000             3452
_exptl_crystal_size_max          0.53
_exptl_crystal_size_mid          0.15
_exptl_crystal_size_min          0.14
_refine_diff_density_max         1.258
_refine_diff_density_min         -1.123
_refine_diff_density_rms         0.117
_refine_ls_abs_structure_details
;
 Refined as an inversion twin.
;
_refine_ls_abs_structure_Flack   0.01(2)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.014
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     461
_refine_ls_number_reflns         12430
_refine_ls_number_restraints     14
_refine_ls_restrained_S_all      1.019
_refine_ls_R_factor_all          0.1123
_refine_ls_R_factor_gt           0.0646
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0480P)^2^+17.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1268
_refine_ls_wR_factor_ref         0.1497
_reflns_Friedel_coverage         0.830
_reflns_Friedel_fraction_full    1.000
_reflns_Friedel_fraction_max     0.995
_reflns_number_gt                7821
_reflns_number_total             12430
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            lq5010.cif
_cod_data_source_block           9
_cod_original_cell_volume        8053.0(19)
_cod_database_code               1549172
_shelxl_version_number           2014-3
_olex2_refinement_description
;
1. Others
 Fixed Sof: C31(0.5) H31A(0.5) H31B(0.5) C32(0.5) H32A(0.5) H32B(0.5)
 H32C(0.5) O1W(0.5) H1WA(0.5) H1WB(0.5) O2W(0.25) H2W(0.5) C31A(0.5) H31C(0.5)
 H31D(0.5) C32A(0.5) H32D(0.5) H32E(0.5) H32F(0.5)
 Fixed U12: Zn1(0) Zn3(0) C26(0) C30(0)
 Fixed U13: Zn1(0) C30(0)
 Fixed U23: Zn3(0) C26(0)
 Fixed Uiso: H1(0.031) H2(0.035) H4(0.039) H5(0.033) H6A(0.042) H6B(0.042)
 H7A(0.035) H7B(0.035) H8(0.034) H9(0.032) H11(0.033) H12(0.032) H13(0.045)
 H14(0.047) H16(0.076) H17(0.076) H18A(0.076) H18B(0.076) H19A(0.076)
 H19B(0.076) H20(0.04) H21(0.048) H23(0.064) H24(0.063) H27A(0.04) H27B(0.04)
 H28A(0.074) H28B(0.074) H28C(0.074) H31A(0.046) H31B(0.046) H32A(0.1)
 H32B(0.1) H32C(0.1) H36A(0.05) H36B(0.05) H37A(0.108) H37B(0.108) H37C(0.108)
 H38A(0.039) H38B(0.039) H39A(0.064) H39B(0.064) H39C(0.064) H1WA(0.104)
 H1WB(0.104) H2W(0.104) H31C(0.046) H31D(0.046) H32D(0.1) H32E(0.1) H32F(0.1)
 Fixed X: Zn3(0) H1(0.4305) H2(0.3848) H4(0.2827) H5(0.3317) H6A(0.2951)
 H6B(0.2654) H7A(0.3592) H7B(0.3261) H8(0.3058) H9(0.3362) H11(0.2603)
 H12(0.23) H13(0.2059) H14(0.154) H16(0.1219) H17(0.1754) H18A(0.0713)
 H18B(0.0765) H19A(0.1419) H19B(0.151) H20(0.021) H21(0.0642) H23(0.1054)
 H24(0.0587) C26(0.5) H27A(0.5415) H27B(0.5487) H28A(0.4695) H28B(0.5015)
 H28C(0.4611) H31A(0.1511) H31B(0.1812) H32A(0.2349) H32B(0.1969) H32C(0.2259)
 H36A(0.0543) H36B(0.0914) H37A(0.0597) H37B(0.0374) H37C(0.0915) H38A(0.1354)
 H38B(0.0907) H39A(0.0609) H39B(0.0893) H39C(0.0444) H1WA(-0.0056) H1WB(0.0061)
 H2W(-0.0224) H31C(0.1776) H31D(0.1324) H32D(0.1702) H32E(0.225) H32F(0.1966)
 Fixed Y: Zn1(0.5) H1(0.4863) H2(0.4589) H4(0.4258) H5(0.4536) H6A(0.4322)
 H6B(0.4143) H7A(0.3895) H7B(0.3711) H8(0.3577) H9(0.3909) H11(0.3288)
 H12(0.2976) H13(0.3637) H14(0.3878) H16(0.2941) H17(0.2723) H18A(0.3448)
 H18B(0.3781) H19A(0.3547) H19B(0.3869) H20(0.4594) H21(0.4313) H23(0.3589)
 H24(0.3882) H27A(0.5915) H27B(0.6193) H28A(0.6429) H28B(0.6395) H28C(0.6145)
 C30(0.5) H31A(0.5343) H31B(0.5371) H32A(0.4935) H32B(0.4789) H32C(0.5093)
 H36A(0.2436) H36B(0.2566) H37A(0.1891) H37B(0.2148) H37C(0.2052) H38A(0.193)
 H38B(0.1846) H39A(0.2018) H39B(0.2339) H39C(0.2279) H1WA(0.3056) H1WB(0.316)
 H2W(0.304) H31C(0.5347) H31D(0.528) H32D(0.4887) H32E(0.5045) H32F(0.4702)
 Fixed Z: Zn1(1.5) Zn3(-0.75) H1(1.1723) H2(0.9882) H4(1.2899) H5(1.4671)
 H6A(0.9123) H6B(1.0213) H7A(0.9324) H7B(1.0304) H8(0.4631) H9(0.653)
 H11(0.9334) H12(0.7354) H13(0.2854) H14(0.1103) H16(-0.0322) H17(0.1429) H18A(-
 0.1372) H18B(-0.0711) H19A(-0.2792) H19B(-0.2074) H20(-0.4222) H21(-0.24) H23(-
 0.5306) H24(-0.7023) C26(1.25) H27A(1.4381) H27B(1.3372) H28A(1.406)
 H28B(1.5353) H28C(1.5057) C30(-1) H31A(-0.8511) H31B(-0.9826) H32A(-0.917)
 H32B(-0.8182) H32C(-0.776) H36A(0.6837) H36B(0.7862) H37A(0.8013) H37B(0.897)
 H37C(0.9125) H38A(0.4614) H38B(0.5472) H39A(0.3252) H39B(0.3362) H39C(0.4282)
 H1WA(0.6331) H1WB(0.4846) H2W(0.2444) H31C(-0.8867) H31D(-0.8007) H32D(-
 0.6563) H32E(-0.7272) H32F(-0.8032)
;
_shelx_res_checksum              72800
_shelx_hkl_checksum              33908