Tuning the bonding dimensions for coordination polymers based on rare earth metal ions
Zhou, Juan; Yu, Ting; Tang, Si si; He, Xiao Ming; Zhang, Xin Lei; Zhou, Lian; Sun, Lin; Zhang, Jun; CrystEngComm  (2022) –; doi:10.1039/D2CE01131J

data_7245563
_publ_section_title
;
 Tuning the bonding dimensions for coordination polymers based on rare
 earth metal ions
;
_journal_name_full               CrystEngComm
_journal_paper_doi               10.1039/D2CE01131J
_journal_year                    2022
_chemical_formula_moiety         'C21 H33 N6 O18 Tb2, 3(Br), 5(H2 O)'
_chemical_formula_sum            'C21 H43 Br3 N6 O23 Tb2'
_chemical_formula_weight         1305.18
_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             2022-08-12
_audit_creation_method
;
Olex2 1.2-beta
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_audit_update_record
;
2022-08-13 deposited with the CCDC.	2022-09-22 downloaded from the CCDC.
;
_cell_angle_alpha                87.302(3)
_cell_angle_beta                 86.119(3)
_cell_angle_gamma                78.386(3)
_cell_formula_units_Z            2
_cell_length_a                   8.791(2)
_cell_length_b                   11.185(3)
_cell_length_c                   20.117(5)
_cell_measurement_reflns_used    4895
_cell_measurement_temperature    296.1(1)
_cell_measurement_theta_max      26.532
_cell_measurement_theta_min      2.369
_cell_volume                     1932.0(8)
_computing_cell_refinement       'SAINT v8.27A (Bruker, 2012)'
_computing_data_reduction        'SAINT v8.27A (Bruker, 2012)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_computing_structure_solution    'ShelXT (Sheldrick, 2015)'
_diffrn_ambient_temperature      296.1(1)
_diffrn_detector                 'Bruker D8 Venture with photon2 CMOS detector'
_diffrn_detector_area_resol_mean 7.9
_diffrn_detector_type            'CMOS detector'
_diffrn_measured_fraction_theta_full 0.980
_diffrn_measured_fraction_theta_max 0.973
_diffrn_measurement_device       'three-circle diffractometer'
_diffrn_measurement_device_type  'Bruker D8 Venture with photon2 CMOS detector'
_diffrn_measurement_method       '\w and \f scans'
_diffrn_radiation_monochromator  'mirror optics'
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0525
_diffrn_reflns_av_unetI/netI     0.1522
_diffrn_reflns_Laue_measured_fraction_full 0.980
_diffrn_reflns_Laue_measured_fraction_max 0.973
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       26
_diffrn_reflns_limit_l_min       -26
_diffrn_reflns_number            18484
_diffrn_reflns_point_group_measured_fraction_full 0.980
_diffrn_reflns_point_group_measured_fraction_max 0.973
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.551
_diffrn_reflns_theta_min         2.149
_diffrn_source                   'microfocus sealed X-ray tube'
_diffrn_source_type              'Incoatec I\ms'
_exptl_absorpt_coefficient_mu    6.826
_exptl_absorpt_correction_T_max  0.62
_exptl_absorpt_correction_T_min  0.41
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS; Bruker, 2000'
_exptl_crystal_colour            colourless
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    2.244
_exptl_crystal_description       plate
_exptl_crystal_F_000             1260
_exptl_crystal_size_max          0.22
_exptl_crystal_size_mid          0.22
_exptl_crystal_size_min          0.13
_refine_diff_density_max         4.317
_refine_diff_density_min         -3.330
_refine_diff_density_rms         0.387
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.129
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     832
_refine_ls_number_reflns         8690
_refine_ls_number_restraints     2578
_refine_ls_restrained_S_all      0.987
_refine_ls_R_factor_all          0.1259
_refine_ls_R_factor_gt           0.0968
_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^)+(0.0001P)^2^+157.1224P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2422
_refine_ls_wR_factor_ref         0.2500
_reflns_Friedel_coverage         0.000
_reflns_number_gt                5895
_reflns_number_total             8690
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d2ce01131j2.cif
_cod_data_source_block           Compound3
_cod_original_cell_volume        1931.9(8)
_cod_database_code               7245563
_shelx_shelxl_version_number     2018/3
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
 At 1.5 times of:
  All O(H,H) groups
2. Restrained distances
 C16-C15 = C16A-C15A = C21A-C20A = C21-C20 = C14A-C13A = C14-C13 = C9-C8 = C9A-
 C8A = C7-C6 = C7A-C6A = C2-C1 = C2A-C1A
 1.48 with sigma of 0.01
 O16-Tb2
 2.4 with sigma of 0.02
 O1-C1 \\sim O1A-C1A
 with sigma of 0.02
 O2-C1 \\sim O2A-C1A
 with sigma of 0.02
 O3-C7 \\sim O3A-C7A
 with sigma of 0.02
 O1-O2 \\sim O1A-O2A
 with sigma of 0.04
 O12-C21 \\sim O12A-C21A
 with sigma of 0.02
 O9-C15 \\sim O9A-C15A
 with sigma of 0.02
 O10-C15 \\sim O10A-C15A
 with sigma of 0.02
 O11-C21 \\sim O11A-C21A
 with sigma of 0.02
 O12-O11 \\sim O12A-O11A
 with sigma of 0.04
 O9-O10 \\sim O9A-O10A
 with sigma of 0.04
 N5-C15 \\sim N5A-C15A
 with sigma of 0.04
 O5-C8 \\sim O5A-C8A
 with sigma of 0.02
 O6-C8 \\sim O6A-C8A
 with sigma of 0.02
 O7-C14 \\sim O7A-C14A
 with sigma of 0.02
 O8-C14 \\sim O8A-C14A
 with sigma of 0.02
 O5-O6 \\sim O5A-O6A
 with sigma of 0.04
 O7-O8 \\sim O7A-O8A
 with sigma of 0.04
 N4-C14 \\sim N4A-C14A
 with sigma of 0.04
 C1-C2 \\sim C1A-C2A
 with sigma of 0.02
 C6-C7 \\sim C6A-C7A
 with sigma of 0.02
 O1-C2 \\sim O1A-C2A
 with sigma of 0.04
 O2-C2 \\sim O2A-C2A
 with sigma of 0.04
 O3-C6 \\sim O3A-C6A
 with sigma of 0.04
 N5-C16 \\sim N5A-C16A
 with sigma of 0.02
 N5-C17 \\sim N5A-C17A
 with sigma of 0.02
 N5-C19 \\sim N5A-C19A
 with sigma of 0.02
 C15-C16 \\sim C15A-C16A
 with sigma of 0.02
 C17-C18 \\sim C17A-C18A
 with sigma of 0.02
 C20-C21 \\sim C20A-C21A
 with sigma of 0.02
 O12-C20 \\sim O12A-C20A
 with sigma of 0.04
 O9-C16 \\sim O9A-C16A
 with sigma of 0.04
 O10-C16 \\sim O10A-C16A
 with sigma of 0.04
 O11-C20 \\sim O11A-C20A
 with sigma of 0.04
 N5-C18 \\sim N5A-C18A
 with sigma of 0.04
 C16-C17 \\sim C16A-C17A
 with sigma of 0.04
 C16-C19 \\sim C16A-C19A
 with sigma of 0.04
 C17-C19 \\sim C17A-C19A
 with sigma of 0.04
 C18-C19 \\sim C18A-C19A
 with sigma of 0.04
 C18-C20 \\sim C18A-C20A
 with sigma of 0.04
 C19-C20 \\sim C19A-C20A
 with sigma of 0.04
 N4-C11 \\sim N4A-C11A
 with sigma of 0.02
 N4-C12 \\sim N4A-C12A
 with sigma of 0.02
 N4-C13 \\sim N4A-C13A
 with sigma of 0.02
 C8-C9 \\sim C8A-C9A
 with sigma of 0.02
 C10-C11 \\sim C10A-C11A
 with sigma of 0.02
 C13-C14 \\sim C13A-C14A
 with sigma of 0.02
 O5-C9 \\sim O5A-C9A
 with sigma of 0.04
 O6-C9 \\sim O6A-C9A
 with sigma of 0.04
 O7-C13 \\sim O7A-C13A
 with sigma of 0.04
 O8-C13 \\sim O8A-C13A
 with sigma of 0.04
 N4-C10 \\sim N4A-C10A
 with sigma of 0.04
 C9-C10 \\sim C9A-C10A
 with sigma of 0.04
 C9-C12 \\sim C9A-C12A
 with sigma of 0.04
 C10-C12 \\sim C10A-C12A
 with sigma of 0.04
 C11-C12 \\sim C11A-C12A
 with sigma of 0.04
 C11-C13 \\sim C11A-C13A
 with sigma of 0.04
 C12-C13 \\sim C12A-C13A
 with sigma of 0.04
 Tb1-C7 \\sim Tb1-C7A
 with sigma of 0.04
 Tb2-O10 \\sim Tb2-O10A
 with sigma of 0.02
 Tb2-C15 \\sim Tb2-C15A
 with sigma of 0.04
 Tb2-O8 \\sim Tb2-O8A
 with sigma of 0.02
 Tb1-O5 \\sim Tb1-O5A
 with sigma of 0.04
 Tb1-O6 \\sim Tb1-O6A
 with sigma of 0.04
 Tb1-C8 \\sim Tb1-C8A
 with sigma of 0.04
 Tb2-C14 \\sim Tb2-C14A
 with sigma of 0.04
 Tb1-C9 \\sim Tb1-C9A
 with sigma of 0.04
 O4-C7 \\sim O4A-C7A
 with sigma of 0.02
 O3-O4 \\sim O3A-O4A
 with sigma of 0.04
 N5-N6 \\sim N5A-N6A
 with sigma of 0.04
 N6-C21 \\sim N6A-C21A
 with sigma of 0.04
 N3-N4 \\sim N3A-N4A
 with sigma of 0.04
 N3-C8 \\sim N3A-C8A
 with sigma of 0.04
 N2-C5 \\sim N2A-C5A
 with sigma of 0.02
 N2-C4 \\sim N2A-C4A
 with sigma of 0.02
 N2-C6 \\sim N2A-C6A
 with sigma of 0.02
 C5-N1 \\sim C5A-N1A
 with sigma of 0.02
 N1-C3 \\sim N1A-C3A
 with sigma of 0.02
 N1-C2 \\sim N1A-C2A
 with sigma of 0.02
 C3-C4 \\sim C3A-C4A
 with sigma of 0.02
 O4-C6 \\sim O4A-C6A
 with sigma of 0.04
 N2-N1 \\sim N2A-N1A
 with sigma of 0.04
 N2-C3 \\sim N2A-C3A
 with sigma of 0.04
 N2-C7 \\sim N2A-C7A
 with sigma of 0.04
 C5-C3 \\sim C5A-C3A
 with sigma of 0.04
 C5-C4 \\sim C5A-C4A
 with sigma of 0.04
 C5-C2 \\sim C5A-C2A
 with sigma of 0.04
 C5-C6 \\sim C5A-C6A
 with sigma of 0.04
 N1-C4 \\sim N1A-C4A
 with sigma of 0.04
 N1-C1 \\sim N1A-C1A
 with sigma of 0.04
 C3-C2 \\sim C3A-C2A
 with sigma of 0.04
 C4-C6 \\sim C4A-C6A
 with sigma of 0.04
 N6-C18 \\sim N6A-C18A
 with sigma of 0.02
 N6-C19 \\sim N6A-C19A
 with sigma of 0.02
 N6-C20 \\sim N6A-C20A
 with sigma of 0.02
 N6-C17 \\sim N6A-C17A
 with sigma of 0.04
 N3-C9 \\sim N3A-C9A
 with sigma of 0.02
 N3-C10 \\sim N3A-C10A
 with sigma of 0.02
 N3-C12 \\sim N3A-C12A
 with sigma of 0.02
 N3-C11 \\sim N3A-C11A
 with sigma of 0.04
 Tb1-O4 \\sim Tb1-O4A
 with sigma of 0.02
3. Uiso/Uaniso restraints and constraints
Tb2 \\sim O9 \\sim O9A \\sim O10 \\sim O10A \\sim O11 \\sim O11A \\sim O12
\\sim O12A \\sim C15 \\sim C15A \\sim C21 \\sim C21A: within 2A with sigma of
0.001 and sigma for terminal atoms of 0.002
All non-hydrogen atoms have similar U: within 2A with sigma of 0.04 and sigma
for terminal atoms of 0.08
Uanis(C16A) \\sim Ueq: with sigma of 0.001 and sigma for terminal atoms of 0.002
Uanis(Tb2) \\sim Ueq, Uanis(O9) \\sim Ueq, Uanis(O10) \\sim Ueq, Uanis(C15)
\\sim Ueq, Uanis(O9A) \\sim Ueq, Uanis(O10A) \\sim Ueq, Uanis(C15A) \\sim Ueq,
Uanis(O12) \\sim Ueq, Uanis(O11) \\sim Ueq, Uanis(C21) \\sim Ueq, Uanis(O12A)
\\sim Ueq, Uanis(O11A) \\sim Ueq, Uanis(C21A) \\sim Ueq: with sigma of 0.001
and sigma for terminal atoms of 0.002
Uanis(O3) \\sim Ueq, Uanis(O4) \\sim Ueq, Uanis(C7) \\sim Ueq, Uanis(O3A) \\sim
Ueq, Uanis(O4A) \\sim Ueq, Uanis(C7A) \\sim Ueq: with sigma of 0.001 and sigma
for terminal atoms of 0.002
All non-hydrogen atoms restrained to be isotropic: with sigma of 0.1 and sigma
for terminal atoms of 0.2
All non-hydrogen atoms restrained to be isotropic: with sigma of 0.01 and sigma
for terminal atoms of 0.02
Uanis(O15) \\sim Ueq: with sigma of 0.005 and sigma for terminal atoms of 0.01
4. Rigid body (RIGU) restrains
 Tb2, O9, O9A, O10, O10A, O11, O11A, O12, O12A, C15, C15A, C21, C21A
 with sigma for 1-2 distances of 0.001 and sigma for 1-3 distances of 0.001
 All non-hydrogen atoms
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
5. Others
 Sof(O1A)=Sof(O2A)=Sof(O3A)=Sof(O4A)=Sof(N1A)=Sof(N2A)=Sof(C1A)=Sof(C2A)=
 Sof(H2AA)=Sof(H2AB)=Sof(C3A)=Sof(H3A)=Sof(C4A)=Sof(H4A)=Sof(C5A)=Sof(H5A)=
 Sof(C6A)=Sof(H6AA)=Sof(H6AB)=Sof(C7A)=1-FVAR(1)
 Sof(O1)=Sof(O2)=Sof(O3)=Sof(O4)=Sof(N2)=Sof(C5)=Sof(H5)=Sof(N1)=Sof(C3)=
 Sof(H3)=Sof(C4)=Sof(H4)=Sof(C1)=Sof(C2)=Sof(H2A)=Sof(H2B)=Sof(C6)=Sof(H6A)=
 Sof(H6B)=Sof(C7)=FVAR(1)
 Sof(O9A)=Sof(O10A)=Sof(O11A)=Sof(O12A)=Sof(N5A)=Sof(N6A)=Sof(C15A)=Sof(C16A)=
 Sof(H16E)=Sof(H16F)=Sof(C17A)=Sof(H17C)=Sof(C18A)=Sof(H18C)=Sof(C19A)=
 Sof(H19A)=Sof(C20A)=Sof(H20C)=Sof(H20D)=Sof(C21A)=1-FVAR(2)
 Sof(O9)=Sof(O10)=Sof(O11)=Sof(O12)=Sof(N5)=Sof(N6)=Sof(C15)=Sof(C16)=
 Sof(H16C)=Sof(H16D)=Sof(C17)=Sof(H17)=Sof(C18)=Sof(H18)=Sof(C19)=Sof(H19)=
 Sof(C20)=Sof(H20A)=Sof(H20B)=Sof(C21)=FVAR(2)
 Sof(O5A)=Sof(O6A)=Sof(O7A)=Sof(O8A)=Sof(N3A)=Sof(N4A)=Sof(C8A)=Sof(C9A)=
 Sof(H9AA)=Sof(H9AB)=Sof(C10A)=Sof(H10A)=Sof(C11A)=Sof(H11A)=Sof(C12A)=
 Sof(H12A)=Sof(C13A)=Sof(H13E)=Sof(H13F)=Sof(C14A)=1-FVAR(3)
 Sof(O5)=Sof(O6)=Sof(O7)=Sof(O8)=Sof(N3)=Sof(N4)=Sof(C8)=Sof(C9)=Sof(H9A)=
 Sof(H9B)=Sof(C10)=Sof(H10)=Sof(C11)=Sof(H11)=Sof(C12)=Sof(H12)=Sof(C13)=
 Sof(H13C)=Sof(H13D)=Sof(C14)=FVAR(3)
 Fixed X: O6A(0.044629) O9A(1.023281) O12A(0.497459)
 Fixed Y: O6A(0.496439) O9A(0.6061) O12A(1.37123)
 Fixed Z: O6A(0.555241) O9A(1.02505) O12A(1.023861)
6.a Riding coordinates:
 O13(H13A,H13B), O14(H14A,H14B), O15(H15A,H15B), O16(H16A,H16B), O17(H17A,
 H17B), O18(H18A,H18B), O19(H19B,H19C), O20(H20E,H20F), O21(H21A,H21B),
 O22(H22A,H22B), O23(H23A,H23B)
6.b Secondary CH2 refined with riding coordinates:
 C2(H2A,H2B), C2A(H2AA,H2AB), C6(H6A,H6B), C6A(H6AA,H6AB), C9(H9A,H9B),
 C9A(H9AA,H9AB), C13(H13C,H13D), C13A(H13E,H13F), C16(H16C,H16D), C16A(H16E,
 H16F), C20(H20A,H20B), C20A(H20C,H20D)
6.c Aromatic/amide H refined with riding coordinates:
 C5(H5), C3(H3), C4(H4), C3A(H3A), C4A(H4A), C5A(H5A), C10(H10), C10A(H10A),
 C11(H11), C11A(H11A), C12(H12), C12A(H12A), C17(H17), C17A(H17C), C18(H18),
 C18A(H18C), C19(H19), C19A(H19A)
6.d Fitted pentagon refined as free rotating group:
 N2(C5,N1,C3,C4)
;
_shelx_res_checksum              4587
_shelx_hkl_checksum              49784
_olex2_submission_special_instructions 'No special instructions were received'