Supramolecular D⋯A-layered structures based on germanium complexes with 2,3-dihydroxynaphthalene and N,N′-bidentate ligands
Shangin, Pavel G.; Krylova, Irina V.; Lalov, Andrey V.; Kozmenkova, Anna Y.; Saverina, Evgeniya A.; Buikin, Petr A.; Korlyukov, Alexander A.; Starikova, Alyona A.; Nikolaevskaya, Elena N.; Egorov, Mikhail P.; Syroeshkin, Mikhail A.; RSC Advances 11 (2021) 21527–21536; doi:10.1039/D1RA02691G

data_7243083
_publ_section_title
;
 Supramolecular D&#x22EF;A-layered structures based on germanium complexes
 with 2,3-dihydroxynaphthalene and N,N&#x2032;-bidentate ligands
;
_journal_issue                   35
_journal_name_full               'RSC Advances'
_journal_page_first              21527
_journal_page_last               21536
_journal_paper_doi               10.1039/D1RA02691G
_journal_volume                  11
_journal_year                    2021
_chemical_formula_moiety         'C32 H20 Ge N2 O4'
_chemical_formula_sum            'C32 H20 Ge N2 O4'
_chemical_formula_weight         569.09
_space_group_crystal_system      monoclinic
_space_group_IT_number           4
_space_group_name_Hall           'P 2yb'
_space_group_name_H-M_alt        'P 1 21 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_audit_creation_date             2021-02-18
_audit_creation_method
;
Olex2 1.3
(compiled 2020.11.12 svn.r5f609507 for OlexSys, GUI svn.r6257)
;
_audit_update_record
;
2021-03-31 deposited with the CCDC.	2021-06-14 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 98.927(6)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   6.0837(5)
_cell_length_b                   15.6412(17)
_cell_length_c                   13.3288(13)
_cell_measurement_reflns_used    5193
_cell_measurement_temperature    296.15
_cell_measurement_theta_max      26.05
_cell_measurement_theta_min      3.03
_cell_volume                     1253.0(2)
_computing_cell_refinement       'SAINT V8.40A (Bruker, 2019)'
_computing_data_reduction        'SAINT V8.40A (Bruker, 2019)'
_computing_molecular_graphics    'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2014/6 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT 2014/5 (Sheldrick, 2014)'
_diffrn_ambient_temperature      296.15
_diffrn_measured_fraction_theta_full 0.958
_diffrn_measured_fraction_theta_max 0.949
_diffrn_measurement_device_type  'Bruker D8 Quest'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0667
_diffrn_reflns_av_unetI/netI     0.0922
_diffrn_reflns_Laue_measured_fraction_full 0.958
_diffrn_reflns_Laue_measured_fraction_max 0.949
_diffrn_reflns_limit_h_max       7
_diffrn_reflns_limit_h_min       -7
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       12
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_number            7650
_diffrn_reflns_point_group_measured_fraction_full 0.959
_diffrn_reflns_point_group_measured_fraction_max 0.950
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         26.060
_diffrn_reflns_theta_min         2.022
_diffrn_source_current           1.4
_diffrn_source_power             0.07
_diffrn_source_voltage           50.0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    1.266
_exptl_absorpt_correction_T_max  0.7453
_exptl_absorpt_correction_T_min  0.4575
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2016/2 (Bruker,2016/2) was used for absorption correction.
wR2(int) was 0.1731 before and 0.0894 after correction.
The Ratio of minimum to maximum transmission is 0.6138.
The \l/2 correction factor is Not present.
;
_exptl_crystal_colour            yellow
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    1.508
_exptl_crystal_description       plate
_exptl_crystal_F_000             580
_exptl_crystal_size_max          0.23
_exptl_crystal_size_mid          0.15
_exptl_crystal_size_min          0.01
_refine_diff_density_max         1.616
_refine_diff_density_min         -0.931
_refine_diff_density_rms         0.124
_refine_ls_abs_structure_details
;
 Refined as an inversion twin.
;
_refine_ls_abs_structure_Flack   0.09(4)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.078
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     353
_refine_ls_number_reflns         3873
_refine_ls_number_restraints     7
_refine_ls_restrained_S_all      1.077
_refine_ls_R_factor_all          0.0898
_refine_ls_R_factor_gt           0.0786
_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^)+(0.0300P)^2^+9.6500P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1812
_refine_ls_wR_factor_ref         0.1870
_reflns_Friedel_coverage         0.927
_reflns_Friedel_fraction_full    0.960
_reflns_Friedel_fraction_max     0.951
_reflns_number_gt                3382
_reflns_number_total             3873
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d1ra02691g2.cif
_cod_data_source_block           259alt
_cod_database_code               7243083
_shelxl_version_number           2014/6
_shelx_estimated_absorpt_t_max   0.987
_shelx_estimated_absorpt_t_min   0.759
_olex2_refinement_description
;
1. Twinned data refinement
 Scales: 0.91(4)
 0.09(4)
2. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
3. Uiso/Uaniso restraints and constraints
Uanis(C12) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
4.a Aromatic/amide H refined with riding coordinates:
 C1(H1), C2(H2), C3(H3), C5(H5), C6(H6), C8(H8), C9(H9), C10(H10), C14(H14),
 C16(H16), C17(H17), C18(H18), C19(H19), C21(H21), C24(H24), C26(H26), C27(H27),
  C28(H28), C29(H29), C31(H31)
;
_shelx_res_checksum              67958
_olex2_submission_special_instructions 'No special instructions were received'