Supporting coordination through hydrogen bonding in lanthanide complexes of 7-azaindole-N-oxide
Wood, Oskar G.; Jones, Leanne; Hawes, Chris S.; CrystEngComm 25 (2023) 6371–6378; doi:10.1039/D3CE00985H

data_7247625
_publ_section_title
;
 Supporting coordination through hydrogen bonding in lanthanide complexes
 of 7-azaindole-N-oxide
;
_journal_issue                   45
_journal_name_full               CrystEngComm
_journal_page_first              6371
_journal_page_last               6378
_journal_paper_doi               10.1039/D3CE00985H
_journal_volume                  25
_journal_year                    2023
_chemical_formula_moiety         'C42 H36 Cl6 Eu2 N12 O6'
_chemical_formula_sum            'C42 H36 Cl6 Eu2 N12 O6'
_chemical_formula_weight         1321.45
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     dual
_audit_creation_date             2023-08-02
_audit_creation_method
;
Olex2 1.5
(compiled 2023.03.06 svn.rbb2c1857 for OlexSys, GUI svn.r6748)
;
_audit_update_record
;
2023-08-10 deposited with the CCDC.	2023-11-01 downloaded from the CCDC.
;
_cell_angle_alpha                79.1160(10)
_cell_angle_beta                 80.1310(10)
_cell_angle_gamma                79.9150(10)
_cell_formula_units_Z            1
_cell_length_a                   8.4097(3)
_cell_length_b                   10.7232(4)
_cell_length_c                   13.8568(5)
_cell_measurement_reflns_used    9966
_cell_measurement_temperature    150.00
_cell_measurement_theta_max      28.223
_cell_measurement_theta_min      2.486
_cell_volume                     1195.72(8)
_computing_cell_refinement       'SAINT V8.40B (?, 2016)'
_computing_data_reduction        'SAINT V8.40B (?, 2016)'
_computing_molecular_graphics    'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_structure_refinement  'XL  (Sheldrick, 2008)'
_computing_structure_solution    'SHELXT 2014/5 (Sheldrick, 2014)'
_diffrn_ambient_temperature      150.00
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.996
_diffrn_measurement_device_type  'Bruker D8 Quest ECO'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0410
_diffrn_reflns_av_unetI/netI     0.0379
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.996
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            26086
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.996
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         28.335
_diffrn_reflns_theta_min         2.661
_diffrn_source_current           20.0
_diffrn_source_power             1.0
_diffrn_source_voltage           50.0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    2.994
_exptl_absorpt_correction_T_max  0.7457
_exptl_absorpt_correction_T_min  0.6910
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2016/2 (Bruker,2016/2) was used for absorption correction.
wR2(int) was 0.0592 before and 0.0525 after correction.
The Ratio of minimum to maximum transmission is 0.9266.
The \l/2 correction factor is Not present.
;
_exptl_crystal_colour            colourless
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.835
_exptl_crystal_description       block
_exptl_crystal_F_000             648
_exptl_crystal_size_max          0.16
_exptl_crystal_size_mid          0.1
_exptl_crystal_size_min          0.08
_refine_diff_density_max         2.124
_refine_diff_density_min         -1.364
_refine_diff_density_rms         0.118
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.078
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     394
_refine_ls_number_reflns         5964
_refine_ls_number_restraints     174
_refine_ls_restrained_S_all      1.068
_refine_ls_R_factor_all          0.0454
_refine_ls_R_factor_gt           0.0331
_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^)+(0.0113P)^2^+3.0433P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0603
_refine_ls_wR_factor_ref         0.0644
_reflns_Friedel_coverage         0.000
_reflns_number_gt                5114
_reflns_number_total             5964
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d3ce00985h2.cif
_cod_data_source_block           4
_cod_depositor_comments
'Adding full bibliography for 7247622--7247628.cif.'
_cod_database_code               7247625
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   0.796
_shelx_estimated_absorpt_t_min   0.646
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All N(H) groups
2. Restrained distances
 N4-H4 = N2-H2
 0.88 with sigma of 0.02
 N7-C22 \\sim N7-C26 \\sim N5-C19 \\sim N5-C15 \\sim N6-C19 \\sim N8-C26
 with sigma of 0.02
 N8-C28 \\sim N6-C21
 with sigma of 0.02
 C19-C18 \\sim C25-C26
 with sigma of 0.02
 C27-C25 \\sim C20-C18
 with sigma of 0.02
 C16-C15 \\sim C17-C16 \\sim C17-C18 \\sim C23-C22 \\sim C23-C24 \\sim C25-C24
 with sigma of 0.02
 C20-C21 \\sim C27-C28
 with sigma of 0.02
3. Rigid body (RIGU) restrains
 N5, N6, C15, C16, C17, C18, C19, C20, C21, N7, N8, C22, C23, C24, C25, C26,
 C27, C28
 with sigma for 1-2 distances of 0.001 and sigma for 1-3 distances of 0.001
4. Others
 Fixed Sof: N5(0.5) N6(0.5) H6A(0.5) C15(0.5) H15(0.5) C16(0.5) H16(0.5)
 C17(0.5) H17(0.5) C18(0.5) C19(0.5) C20(0.5) H20(0.5) C21(0.5) H21(0.5)
 N7(0.5) N8(0.5) H8A(0.5) C22(0.5) H22(0.5) C23(0.5) H23(0.5) C24(0.5) H24(0.5)
 C25(0.5) C26(0.5) C27(0.5) H27(0.5) C28(0.5) H28(0.5)
5.a Aromatic/amide H refined with riding coordinates:
 C1(H1), C2(H2A), C3(H3), C6(H6), C7(H7), C8(H8), C9(H9), C10(H10), C13(H13),
 C14(H14), N6(H6A), C15(H15), C16(H16), C17(H17), C20(H20), C21(H21), N8(H8A),
 C22(H22), C23(H23), C24(H24), C27(H27), C28(H28)
;
_shelx_res_checksum              42010
_olex2_submission_special_instructions 'No special instructions were received'