Tuning the coordination behavior of an unexplored asymmetric multidentate ligand for developing diverse heterometallic architectures with luminescent and magnetic properties
Song, Xue-Qin; Xia, Xue-Li; Song, Fu-Qiang; Liu, Guo-Hua; Wang, Li; CrystEngComm 23 (2021) 1000–1012; doi:10.1039/D0CE01298J

data_7241537
_publ_section_title
;
 Tuning the coordination behavior of an unexplored asymmetric multidentate
 ligand for developing diverse heterometallic architectures with
 luminescent and magnetic properties
;
_journal_issue                   4
_journal_name_full               CrystEngComm
_journal_page_first              1000
_journal_page_last               1012
_journal_paper_doi               10.1039/D0CE01298J
_journal_volume                  23
_journal_year                    2021
_chemical_formula_moiety         'C50 H60 N4 Ni3 O26 Tb2, 2(C2 H3 N), H2 O'
_chemical_formula_sum            'C54 H68 N6 Ni3 O27 Tb2'
_chemical_formula_weight         1727.11
_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
_audit_creation_date             2019-11-27
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_audit_update_record
;
2020-07-19 deposited with the CCDC.	2020-11-23 downloaded from the CCDC.
;
_cell_angle_alpha                99.724(3)
_cell_angle_beta                 93.835(3)
_cell_angle_gamma                102.377(3)
_cell_formula_units_Z            2
_cell_length_a                   11.3623(4)
_cell_length_b                   15.8821(6)
_cell_length_c                   20.2160(6)
_cell_measurement_reflns_used    7902
_cell_measurement_temperature    173(10)
_cell_measurement_theta_max      69.7320
_cell_measurement_theta_min      9.3850
_cell_volume                     3491.9(2)
_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      173(10)
_diffrn_detector_area_resol_mean 16.0733
_diffrn_measured_fraction_theta_full 0.965
_diffrn_measured_fraction_theta_max 0.940
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at zero, Eos'
_diffrn_measurement_method       '\w scans'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0460
_diffrn_reflns_av_unetI/netI     0.0656
_diffrn_reflns_Laue_measured_fraction_full 0.965
_diffrn_reflns_Laue_measured_fraction_max 0.940
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -24
_diffrn_reflns_number            22868
_diffrn_reflns_point_group_measured_fraction_full 0.965
_diffrn_reflns_point_group_measured_fraction_max 0.940
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         70.283
_diffrn_reflns_theta_min         3.979
_diffrn_source                   'SuperNova (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    11.330
_exptl_absorpt_correction_T_max  1.0000
_exptl_absorpt_correction_T_min  0.4581
_exptl_absorpt_correction_type   multi-scan
_exptl_crystal_colour            green
_exptl_crystal_density_diffrn    1.643
_exptl_crystal_description       block
_exptl_crystal_F_000             1728
_exptl_crystal_size_max          0.18
_exptl_crystal_size_mid          0.16
_exptl_crystal_size_min          0.12
_refine_diff_density_max         0.980
_refine_diff_density_min         -1.030
_refine_diff_density_rms         0.106
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.037
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     850
_refine_ls_number_reflns         12520
_refine_ls_number_restraints     3
_refine_ls_restrained_S_all      1.037
_refine_ls_R_factor_all          0.0516
_refine_ls_R_factor_gt           0.0395
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0436P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0957
_refine_ls_wR_factor_ref         0.1041
_reflns_Friedel_coverage         0.000
_reflns_number_gt                10407
_reflns_number_total             12520
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d0ce01298j2.cif
_cod_data_source_block           sxq_l5nitb_sq_s
_cod_depositor_comments
'Adding full bibliography for 7241533--7241538.cif.'
_cod_original_cell_volume        3492.0(2)
_cod_database_code               7241537
_shelx_shelxl_version_number     2014/7
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H,H) groups, H5 of C5, H4 of C4, H3 of C3, H10 of C10, H12 of C12,
  H14 of C14, H15 of C15, H16 of C16, H22 of C22, H23 of C23, H24 of C24, H27
  of C27, H29 of C29, H33 of C33, H34 of C34, H35 of C35, H26 of O26, H25 of
  O25, All N(H) groups
 At 1.5 times of:
  All C(H,H,H) groups, H4B of C54, H9 of O9, All O(H,H) groups
2. Restrained distances
 O9-H9
 0.85 with sigma of 0.01
 C29-H9
 1.915012 with sigma of 0.02
 Ni3-H9
 2.828925 with sigma of 0.02
3.a Riding coordinates:
 O25(H25)
3.b Free rotating group:
 O27(H27A,H27B)
3.c Ternary CH refined with riding coordinates:
 C10(H10), C29(H29), O26(H26)
3.d Secondary CH2 refined with riding coordinates:
 C9(H9A,H9B), C11(H11A,H11B), C28(H28A,H28B), C30(H30A,H30B)
3.e Aromatic/amide H refined with riding coordinates:
 C3(H3), C4(H4), C5(H5), C12(H12), C14(H14), C15(H15), C16(H16), C22(H22),
 C23(H23), C24(H24), C27(H27), C33(H33), C34(H34), C35(H35), N1(H1), N4(H4A)
3.f Idealised Me refined as rotating group:
 C1(H1A,H1B,H1C), C19(H19A,H19B,H19C), C20(H20A,H20B,H20C), C38(H38A,H38B,
 H38C), C39(H39A,H39B,H39C), C42(H42A,H42B,H42C), C43(H43A,H43B,H43C), C45(H45A,
 H45B,H45C), C48(H48A,H48B,H48C), C50(H50A,H50B,H50C), C51(H51A,H51B,H51C),
 C53(H53A,H53B,H53C)
;
_shelx_res_checksum              94443
_shelx_fab_checksum              82561
_olex2_submission_special_instructions 'No special instructions were received'