An insight into the route from CO<sub>2</sub> fixation to CO<sub>3</sub><sup>2-</sup>-bridged dinuclear lanthanide(III) complexes featuring inner coordination post-synthetic modification.
Singh, Vaibhav; Urunikulavan, Vajeeha; Bar, Arun Kumar; Dalton transactions (Cambridge, England : 2003) 54 (2025) 4566–4576; doi:10.1039/d4dt03050h

data_7717980
_publ_section_title
;
 An insight into the route from CO<sub>2</sub> fixation to
 CO<sub>3</sub><sup>2-</sup>-bridged dinuclear lanthanide(III) complexes
 featuring inner coordination post-synthetic modification.
;
_journal_issue                   11
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              4566
_journal_page_last               4576
_journal_paper_doi               10.1039/d4dt03050h
_journal_volume                  54
_journal_year                    2025
_chemical_formula_moiety         'C83 H68 N10 O9 P2 Y2'
_chemical_formula_sum            'C83 H68 N10 O9 P2 Y2'
_chemical_formula_weight         1589.23
_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   geom
_atom_sites_solution_primary     dual
_audit_creation_date             2024-03-31
_audit_creation_method
;
Olex2 1.5
(compiled 2023.08.24 svn.re1ec1418 for OlexSys, GUI svn.r6817)
;
_audit_update_record
;
2024-08-20 deposited with the CCDC.	2025-02-04 downloaded from the CCDC.
;
_cell_angle_alpha                91.498(2)
_cell_angle_beta                 96.674(2)
_cell_angle_gamma                91.932(2)
_cell_formula_units_Z            4
_cell_length_a                   9.4938(5)
_cell_length_b                   24.7455(17)
_cell_length_c                   32.698(2)
_cell_measurement_reflns_used    9858
_cell_measurement_temperature    100.00
_cell_measurement_theta_max      23.09
_cell_measurement_theta_min      2.34
_cell_volume                     7621.8(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 2018/2 (Sheldrick, 2018)'
_diffrn_ambient_temperature      100.00
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.1123
_diffrn_reflns_av_unetI/netI     0.0715
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.997
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       29
_diffrn_reflns_limit_k_min       -29
_diffrn_reflns_limit_l_max       38
_diffrn_reflns_limit_l_min       -38
_diffrn_reflns_number            154166
_diffrn_reflns_point_group_measured_fraction_full 0.997
_diffrn_reflns_point_group_measured_fraction_max 0.997
_diffrn_reflns_theta_full        24.955
_diffrn_reflns_theta_max         24.955
_diffrn_reflns_theta_min         1.882
_diffrn_source_current           1.4
_diffrn_source_power             0.07
_diffrn_source_voltage           50.0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    1.622
_exptl_absorpt_correction_T_max  0.7451
_exptl_absorpt_correction_T_min  0.6382
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2016/2 (Bruker,2016/2) was used for absorption correction.
wR2(int) was 0.0935 before and 0.0628 after correction.
The Ratio of minimum to maximum transmission is 0.8565.
The \l/2 correction factor is Not present.
;
_exptl_crystal_colour            'metallic yellowish yellow'
_exptl_crystal_colour_lustre     metallic
_exptl_crystal_colour_modifier   yellowish
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    1.385
_exptl_crystal_description       plate
_exptl_crystal_F_000             3264
_exptl_crystal_size_max          0.15
_exptl_crystal_size_mid          0.08
_exptl_crystal_size_min          0.05
_refine_diff_density_max         1.831
_refine_diff_density_min         -1.220
_refine_diff_density_rms         0.084
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.027
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     2022
_refine_ls_number_reflns         26652
_refine_ls_number_restraints     72
_refine_ls_restrained_S_all      1.028
_refine_ls_R_factor_all          0.1186
_refine_ls_R_factor_gt           0.0711
_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^)+(0.0725P)^2^+24.9897P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1641
_refine_ls_wR_factor_ref         0.1899
_reflns_Friedel_coverage         0.000
_reflns_number_gt                17217
_reflns_number_total             26652
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d4dt03050h2.cif
_cod_data_source_block           mo_vs110c_test_0m
_cod_depositor_comments
'Adding full bibliography for 7717973--7717980.cif.'
_cod_database_code               7717980
_shelx_shelxl_version_number     2019/1
_shelx_estimated_absorpt_t_max   0.923
_shelx_estimated_absorpt_t_min   0.793
_olex2_refinement_description
;
1. Uiso/Uaniso restraints and constraints
Uanis(C1I) \\sim Ueq: with sigma of 0.015 and sigma for terminal atoms of 0.03
Uanis(C91) \\sim Ueq: with sigma of 0.015 and sigma for terminal atoms of 0.03
Uanis(C152) \\sim Ueq: with sigma of 0.015 and sigma for terminal atoms of 0.03
Uanis(C144) \\sim Ueq, Uanis(C1C) \\sim Ueq, Uanis(C145) \\sim Ueq, Uanis(C1F)
\\sim Ueq, Uanis(C146) \\sim Ueq, Uanis(C1I) \\sim Ueq, Uanis(C1E) \\sim Ueq,
Uanis(C148) \\sim Ueq, Uanis(C143) \\sim Ueq: with sigma of 0.015 and sigma for
terminal atoms of 0.03
Uanis(O14) \\sim Ueq: with sigma of 0.015 and sigma for terminal atoms of 0.03
Uanis(Y1) = Uanis(C47)
Uanis(Y4) = Uanis(C107)
2. Others
 Fixed Sof: H139(0.4) H13A(0.6) H146(0.5) H14A(0.5) H15A(0.5) H15B(0.5)
 H151(0.5) H15C(0.5) C142(0.4) H142(0.4) C144(0.6) H144(0.6) C140(0.4)
 H140(0.4) C87A(0.5) H87A(0.5) C88A(0.5) H88A(0.5) C90A(0.5) C141(0.5)
 H141(0.5) C148(0.5) H148(0.5) C145(0.5) H145(0.5) C153(0.5) H153(0.5) C1A(0.6)
 H1A(0.6) C1B(0.6) H1B(0.6) C1C(0.4) H1C(0.4) C87B(0.5) H87B(0.5) C88B(0.5)
 H88B(0.5) C90B(0.5) C1D(0.5) H1D(0.5) C1E(0.5) H1E(0.5) C1F(0.5) H1F(0.5)
 C1G(0.5) H1G(0.5) C89A(0.5) H89A(0.5) C89B(0.5) H89B(0.5) C152(0.5) H152(0.5)
 C1H(0.5) H1H(0.5) C147(0.5) H147(0.5) C1I(0.5) H1I(0.5)
3.a Secondary CH2 refined with riding coordinates:
 C154(H15A,H15B)
3.b Aromatic/amide H refined with riding coordinates:
 C12(H12), C59(H59), C65(H65), C6(H6), C15(H15), C4(H4), C5(H5), C13(H13),
 C58(H58), C16(H16), C51(H51), C126(H126), C14(H14), C64(H64), C49(H49),
 C23(H23), C19(H19), C55(H55), C75(H75), C57(H57), C20(H20), C74(H74), C53(H53),
  C73(H73), C61(H61), C165(H165), C71(H71), C50(H50), C42(H42), C129(H129),
 C166(H166), C21(H21), C160(H160), C132(H132), C106(H106), C22(H22), C128(H128),
  C159(H159), C130(H130), C63(H63), C127(H127), C83(H83), C136(H136),
 C135(H135), C162(H162), C77(H77), C139(H139), C139(H13A), C28(H28), C27(H27),
 C67(H67), C56(H56), C52(H52), C102(H102), C164(H164), C46(H46), C82(H82),
 C43(H43), C158(H158), C105(H105), C62(H62), C134(H134), C70(H70), C133(H133),
 C29(H29), C76(H76), C45(H45), C163(H163), C138(H138), C111(H111), C44(H44),
 C157(H157), C156(H156), C123(H123), C39(H39), C79(H79), C113(H113), C104(H104),
  C81(H81), C35(H35), C103(H103), C119(H119), C121(H121), C37(H37), C36(H36),
 C122(H122), C69(H69), C99(H99), C112(H112), C95(H95), C68(H68), C98(H98),
 C38(H38), C150(H150), C80(H80), C120(H120), C97(H97), C96(H96), C146(H146),
 C146(H14A), C151(H151), C151(H15C), C142(H142), C144(H144), C140(H140),
 C87A(H87A), C88A(H88A), C141(H141), C148(H148), C145(H145), C153(H153),
 C1A(H1A), C1B(H1B), C1C(H1C), C87B(H87B), C88B(H88B), C1D(H1D), C1E(H1E),
 C1F(H1F), C1G(H1G), C89A(H89A), C89B(H89B), C152(H152), C1H(H1H), C147(H147),
 C1I(H1I)
3.c Idealised Me refined as rotating group:
 C1(H1J,H1K,H1L), C9(H9A,H9B,H9C), C24(H24A,H24B,H24C), C108(H10A,H10B,H10C),
 C32(H32A,H32B,H32C), C116(H11A,H11B,H11C), C84(H84A,H84B,H84C), C92(H92A,H92B,
 H92C)
;
_smtbx_masks_void_probe_radius   1.2
_smtbx_masks_void_truncation_radius 1.2
_shelx_res_checksum              3938
_shelx_fab_checksum              29625
_olex2_submission_special_instructions 'No special instructions were received'