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_7247623
_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
'C35 H32 Cl N10 O6 Yb, C21 H18 Cl3 N6 O3 Yb, 2(Cl)'
_chemical_formula_sum            'C56 H50 Cl6 N16 O9 Yb2'
_chemical_formula_weight         1649.90
_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                118.4950(10)
_cell_angle_beta                 93.0430(10)
_cell_angle_gamma                103.0590(10)
_cell_formula_units_Z            2
_cell_length_a                   13.2616(4)
_cell_length_b                   16.7698(6)
_cell_length_c                   16.9393(6)
_cell_measurement_reflns_used    9852
_cell_measurement_temperature    150.00
_cell_measurement_theta_max      25.74
_cell_measurement_theta_min      2.49
_cell_volume                     3167.76(19)
_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 0.998
_diffrn_measured_fraction_theta_max 0.994
_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  0.0793
_diffrn_reflns_av_unetI/netI     0.0702
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.994
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            62610
_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         26.439
_diffrn_reflns_theta_min         2.446
_diffrn_source_current           20.0
_diffrn_source_power             1.0
_diffrn_source_voltage           50.0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    3.255
_exptl_absorpt_correction_T_max  0.7454
_exptl_absorpt_correction_T_min  0.6784
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2016/2 (Bruker,2016/2) was used for absorption correction.
wR2(int) was 0.0705 before and 0.0604 after correction.
The Ratio of minimum to maximum transmission is 0.9101.
The \l/2 correction factor is Not present.
;
_exptl_crystal_colour            colourless
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.730
_exptl_crystal_description       block
_exptl_crystal_F_000             1624
_exptl_crystal_size_max          0.17
_exptl_crystal_size_mid          0.09
_exptl_crystal_size_min          0.04
_refine_diff_density_max         1.140
_refine_diff_density_min         -0.863
_refine_diff_density_rms         0.140
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.036
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     827
_refine_ls_number_reflns         12991
_refine_ls_number_restraints     77
_refine_ls_restrained_S_all      1.034
_refine_ls_R_factor_all          0.0832
_refine_ls_R_factor_gt           0.0446
_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^)+(0.0197P)^2^+10.0079P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0743
_refine_ls_wR_factor_ref         0.0852
_reflns_Friedel_coverage         0.000
_reflns_number_gt                8968
_reflns_number_total             12991
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d3ce00985h2.cif
_cod_data_source_block           5
_cod_depositor_comments
'Adding full bibliography for 7247622--7247628.cif.'
_cod_original_cell_volume        3167.75(19)
_cod_database_code               7247623
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   0.881
_shelx_estimated_absorpt_t_min   0.608
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All N(H) groups
 At 1.5 times of:
  All O(H,H) groups
2. Restrained distances
 N10-H10 = N2-H2 = N4-H4 = N8-H8 = N6-H6 = N16-H16A = N12-H12 = N14-H14A
 0.88 with sigma of 0.02
3. Rigid body (RIGU) restrains
 N5, N6, C15, C16, C17, C18, C19, C20, C21
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
4.a Rotating group:
 O9(H9A,H9B)
4.b Aromatic/amide H refined with riding coordinates:
 C1(H1), C2(H2A), C3(H3), C6(H6A), C7(H7), C8(H8A), C9(H9), C10(H10A),
 C13(H13), C14(H14), C15(H15), C16(H16), C17(H17), C20(H20), C21(H21), C22(H22),
  C23(H23), C24(H24), C27(H27), C28(H28), C29(H29), C30(H30), C31(H31),
 C34(H34), C35(H35), C36(H36), C37(H37), C38(H38), C41(H41), C42(H42), C43(H43),
  C44(H44), C45(H45), C48(H48), C49(H49), C50(H50), C51(H51), C52(H52),
 C55(H55), C56(H56)
;
_shelx_res_checksum              14835
_olex2_submission_special_instructions 'No special instructions were received'