Structural and spectroscopic investigations of nine-coordinate redox active lanthanide complexes with a pincer O,N,O ligand.
Mouchel Dit Leguerrier, D.; Barré, R; Bryden, M.; Imbert, D.; Philouze, C.; Jarjayes, O.; Luneau, D.; Molloy, J. K.; Thomas, F.; Dalton transactions (Cambridge, England : 2003) 49 (2020) 8238–8246; doi:10.1039/d0dt01388a

data_7704634
_publ_section_title
;
 Structural and spectroscopic investigations of nine-coordinate redox
 active lanthanide complexes with a pincer O,N,O ligand.
;
_journal_issue                   24
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              8238
_journal_page_last               8246
_journal_paper_doi               10.1039/d0dt01388a
_journal_volume                  49
_journal_year                    2020
_chemical_formula_moiety         'C84 H120 Gd N3 O6'
_chemical_formula_sum            'C84 H120 Gd N3 O6'
_chemical_formula_weight         1425.07
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2ybc'
_space_group_name_H-M_alt        'P 1 21/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_audit_creation_date             2020-02-13
_audit_creation_method
;
Olex2 1.2
(compiled 2014.07.22 svn.r2960 for OlexSys, GUI svn.r4862)
;
_audit_update_record
;
2020-03-18 deposited with the CCDC.	2020-05-28 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 93.35(3)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   13.308(3)
_cell_length_b                   21.282(4)
_cell_length_c                   29.272(6)
_cell_measurement_reflns_used    93803
_cell_measurement_temperature    200.0
_cell_measurement_theta_max      25.000
_cell_measurement_theta_min      2.131
_cell_volume                     8276(3)
_computing_cell_refinement       EvalCCD
_computing_data_collection       Collect
_computing_data_reduction        EvalCCD
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'olex2.refine (Bourhis et al., 2013)'
_computing_structure_solution    'ShelXS-1997 (Sheldrick, 2008)'
_diffrn_ambient_temperature      200.0
_diffrn_detector                 'CCD area detector'
_diffrn_detector_type            'APEX II'
_diffrn_measured_fraction_theta_full 0.996
_diffrn_measured_fraction_theta_max 0.996
_diffrn_measurement_device       '\k-geometry 4 circles diffractometer'
_diffrn_measurement_device_type  'Bruker-AXS-enraf-nonius KappaAPEXII'
_diffrn_measurement_method       'Phi and omega scans'
_diffrn_radiation_collimation    'Montel optic'
_diffrn_radiation_detector       CCD
_diffrn_radiation_monochromator  'Multilayer mirrors'
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0922
_diffrn_reflns_av_unetI/netI     0.0606
_diffrn_reflns_Laue_measured_fraction_full 0.996
_diffrn_reflns_Laue_measured_fraction_max 0.996
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       25
_diffrn_reflns_limit_k_min       -21
_diffrn_reflns_limit_l_max       34
_diffrn_reflns_limit_l_min       -34
_diffrn_reflns_number            95585
_diffrn_reflns_point_group_measured_fraction_full 0.996
_diffrn_reflns_point_group_measured_fraction_max 0.996
_diffrn_reflns_theta_full        25.000
_diffrn_reflns_theta_max         25.000
_diffrn_reflns_theta_min         2.131
_diffrn_source                   'Incoatec ISG250'
_diffrn_source_target            Mo
_diffrn_source_type              'Microfocus sealed tube'
_exptl_absorpt_coefficient_mu    0.850
_exptl_absorpt_correction_T_max  1
_exptl_absorpt_correction_T_min  0.513975
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2004/1 (Bruker,2004) was used for absorption correction.
R(int) was 0.4163 before and 0.1097 after correction.
The Ratio of minimum to maximum transmission is 0.5140.
The \l/2 correction factor is 0.0015.
;
_exptl_crystal_colour            green
_exptl_crystal_colour_primary    green
_exptl_crystal_density_diffrn    1.144
_exptl_crystal_description       plate
_exptl_crystal_F_000             3028
_exptl_crystal_size_max          0.38
_exptl_crystal_size_mid          0.16
_exptl_crystal_size_min          0.04
_refine_diff_density_max         1.563
_refine_diff_density_min         -1.640
_refine_diff_density_rms         0.086
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.125
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1683
_refine_ls_number_reflns         14521
_refine_ls_number_restraints     2594
_refine_ls_restrained_S_all      1.057
_refine_ls_R_factor_all          0.0856
_refine_ls_R_factor_gt           0.0498
_refine_ls_shift/su_max          0.003
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0537P)^2^+11.3764P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1067
_refine_ls_wR_factor_ref         0.1260
_reflns_Friedel_coverage         0.000
_reflns_number_gt                10641
_reflns_number_total             14521
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d0dt01388a2.cif
_cod_data_source_block           sad
_cod_depositor_comments
'Adding full bibliography for 7704633--7704634.cif.'
_cod_database_code               7704634
_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 C(H,H,H) groups, All C(H,H,H,H,H,H) groups
2. Restrained distances
 C131-C132
 2.5 with sigma of 0.02
 C131-C129
 1.5 with sigma of 0.02
 C47-C48
 2.5 with sigma of 0.02
 C45-C47
 1.5 with sigma of 0.02
 C51-C52
 2.5 with sigma of 0.02
 C51-C50
 2.5 with sigma of 0.02
 C52-C50
 2.5 with sigma of 0.02
 C51-C49
 1.5 with sigma of 0.02
 C49-C52
 1.5 with sigma of 0.02
 C49-C50
 1.5 with sigma of 0.02
3. Rigid bond restraints
 All non-hydrogen atoms
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
4. Uiso/Uaniso restraints and constraints
All non-hydrogen atoms have similar U: within 1.7A with sigma of 0.04 and sigma
for terminal atoms of 0.08
Uanis(C111) \\sim Ueq: with sigma of 0.1 and sigma for terminal atoms of 0.2
Uanis(C50) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
Uanis(C52) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
Uanis(C132) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
Uanis(C131) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
Uanis(C104) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
Uanis(C19) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
Uanis(C24) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
Uanis(C79) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
5. Others
 Sof(O8)=Sof(O9)=Sof(H36A)=Sof(H8B)=Sof(H70D)=Sof(H70E)=Sof(H70F)=Sof(C153)=
 Sof(C111)=Sof(H11A)=Sof(H11B)=Sof(H11C)=Sof(C113)=Sof(C147)=Sof(C152)=
 Sof(C116)=Sof(H116)=Sof(C115)=Sof(C148)=Sof(H148)=Sof(C114)=Sof(H114)=
 Sof(C118)=Sof(C151)=Sof(C137)=Sof(C117)=Sof(C119)=Sof(C95)=Sof(C133)=Sof(C91)=
 Sof(C112)=Sof(H11D)=Sof(H11E)=Sof(H11F)=Sof(C106)=Sof(H10A)=Sof(H10B)=
 Sof(H10C)=Sof(C96)=Sof(C90)=Sof(C144)=Sof(H144)=Sof(C146)=Sof(C92)=Sof(H92)=
 Sof(C150)=Sof(H150)=Sof(C166)=Sof(H16A)=Sof(H16B)=Sof(H16C)=Sof(C108)=
 Sof(H10D)=Sof(H10E)=Sof(H10F)=Sof(C129)=Sof(C145)=Sof(C105)=Sof(C89)=Sof(C126)=
 Sof(H12A)=Sof(H12B)=Sof(H12C)=Sof(C98)=Sof(H98A)=Sof(H98B)=Sof(H98C)=Sof(C110)=
 Sof(H11G)=Sof(H11H)=Sof(H11I)=Sof(C88)=Sof(H88)=Sof(C93)=Sof(C127)=Sof(H12D)=
 Sof(H12E)=Sof(H12F)=Sof(C94)=Sof(H94)=Sof(C139)=Sof(H13A)=Sof(H13B)=Sof(H13C)=
 Sof(C140)=Sof(H14A)=Sof(H14B)=Sof(H14C)=Sof(C130)=Sof(H13D)=Sof(H13E)=
 Sof(H13F)=Sof(C97)=Sof(C149)=Sof(C124)=Sof(C135)=Sof(H13G)=Sof(H13H)=Sof(H13I)=
 Sof(C87)=Sof(C134)=Sof(H13J)=Sof(H13K)=Sof(H13L)=Sof(C123)=Sof(C121)=Sof(C107)=
 Sof(H10G)=Sof(H10H)=Sof(H10I)=Sof(C162)=Sof(H16G)=Sof(H16H)=Sof(H16I)=
 Sof(C143)=Sof(C122)=Sof(H122)=Sof(C164)=Sof(H16J)=Sof(H16K)=Sof(H16L)=
 Sof(C161)=Sof(C99)=Sof(H99A)=Sof(H99B)=Sof(H99C)=Sof(C102)=Sof(H10J)=Sof(H10K)=
 Sof(H10L)=Sof(C167)=Sof(H16M)=Sof(H16N)=Sof(H16O)=Sof(C155)=Sof(H15A)=
 Sof(H15B)=Sof(H15C)=Sof(C154)=Sof(H15D)=Sof(H15E)=Sof(H15F)=Sof(C168)=
 Sof(H16P)=Sof(H16Q)=Sof(H16R)=Sof(C163)=Sof(H16S)=Sof(H16T)=Sof(H16U)=
 Sof(C103)=Sof(H10M)=Sof(H10N)=Sof(H10O)=Sof(C141)=Sof(C156)=Sof(H15J)=
 Sof(H15K)=Sof(H15L)=Sof(C132)=Sof(H13M)=Sof(H13N)=Sof(H13O)=Sof(C131)=
 Sof(H13P)=Sof(H13Q)=Sof(H13R)=Sof(C142)=Sof(H142)=Sof(O10)=Sof(C104)=Sof(H10P)=
 Sof(H10Q)=Sof(H10R)=Sof(C101)=Sof(C138)=Sof(H13S)=Sof(H13T)=Sof(H13U)=Sof(O7)=
 Sof(C85)=Sof(C157)=Sof(C159)=Sof(H15M)=Sof(H15N)=Sof(H15O)=Sof(C158)=Sof(H15P)=
 Sof(H15Q)=Sof(H15R)=Sof(C160)=Sof(H16V)=Sof(H16W)=Sof(H16X)=Sof(C136)=
 Sof(H13V)=Sof(H13W)=Sof(H13X)=Sof(C125)=Sof(C128)=Sof(H12G)=Sof(H12H)=
 Sof(H12I)=Sof(O11)=Sof(O12)=1-FVAR(1)
 Sof(O1)=Sof(H36)=Sof(H8A)=Sof(H70A)=Sof(H70B)=Sof(H70C)=Sof(C63)=Sof(C57)=
 Sof(C67)=Sof(C64)=Sof(H64)=Sof(C66)=Sof(H66)=Sof(C46)=Sof(H46A)=Sof(H46B)=
 Sof(H46C)=Sof(C21)=Sof(C33)=Sof(C77)=Sof(C34)=Sof(C27)=Sof(H27A)=Sof(H27B)=
 Sof(H27C)=Sof(C68)=Sof(C29)=Sof(C65)=Sof(C32)=Sof(H32)=Sof(C12)=Sof(C39)=
 Sof(C30)=Sof(H30)=Sof(C38)=Sof(H38)=Sof(C26)=Sof(H26A)=Sof(H26B)=Sof(H26C)=
 Sof(C40)=Sof(C6)=Sof(C16)=Sof(H16D)=Sof(H16E)=Sof(H16F)=Sof(C82)=Sof(H82A)=
 Sof(H82B)=Sof(H82C)=Sof(C11)=Sof(C83)=Sof(H83A)=Sof(H83B)=Sof(H83C)=Sof(C1)=
 Sof(C5)=Sof(C71)=Sof(H71A)=Sof(H71B)=Sof(H71C)=Sof(C42)=Sof(H42A)=Sof(H42B)=
 Sof(H42C)=Sof(C61)=Sof(C60)=Sof(H60)=Sof(C45)=Sof(C73)=Sof(C69)=Sof(C17)=
 Sof(C10)=Sof(H10)=Sof(C37)=Sof(C74)=Sof(H74A)=Sof(H74B)=Sof(H74C)=Sof(C59)=
 Sof(C2)=Sof(H2)=Sof(C76)=Sof(H76A)=Sof(H76B)=Sof(H76C)=Sof(C62)=Sof(C48)=
 Sof(H48A)=Sof(H48B)=Sof(H48C)=Sof(C9)=Sof(C44)=Sof(H44A)=Sof(H44B)=Sof(H44C)=
 Sof(C31)=Sof(C56)=Sof(H56A)=Sof(H56B)=Sof(H56C)=Sof(C28)=Sof(H28A)=Sof(H28B)=
 Sof(H28C)=Sof(C4)=Sof(H4)=Sof(C78)=Sof(H78A)=Sof(H78B)=Sof(H78C)=Sof(C54)=
 Sof(H54A)=Sof(H54B)=Sof(H54C)=Sof(C3)=Sof(C20)=Sof(H20A)=Sof(H20B)=Sof(H20C)=
 Sof(C75)=Sof(H75A)=Sof(H75B)=Sof(H75C)=Sof(C22)=Sof(H22A)=Sof(H22B)=Sof(H22C)=
 Sof(C15)=Sof(H15G)=Sof(H15H)=Sof(H15I)=Sof(C35)=Sof(C14)=Sof(H14D)=Sof(H14E)=
 Sof(H14F)=Sof(C72)=Sof(H72A)=Sof(H72B)=Sof(H72C)=Sof(C55)=Sof(H55A)=Sof(H55B)=
 Sof(H55C)=Sof(C58)=Sof(H58)=Sof(O2)=Sof(C25)=Sof(C18)=Sof(H18A)=Sof(H18B)=
 Sof(H18C)=Sof(C19)=Sof(H19A)=Sof(H19B)=Sof(H19C)=Sof(O5)=Sof(C24)=Sof(H24A)=
 Sof(H24B)=Sof(H24C)=Sof(C23)=Sof(H23A)=Sof(H23B)=Sof(H23C)=Sof(C7)=Sof(C49)=
 Sof(C81)=Sof(C84)=Sof(H84A)=Sof(H84B)=Sof(H84C)=Sof(C80)=Sof(H80A)=Sof(H80B)=
 Sof(H80C)=Sof(C79)=Sof(H79A)=Sof(H79B)=Sof(H79C)=Sof(O6)=Sof(O4)=Sof(O3)=
 Sof(C43)=Sof(H43A)=Sof(H43B)=Sof(H43C)=Sof(C53)=Sof(C51)=Sof(H51A)=Sof(H51B)=
 Sof(H51C)=Sof(C52)=Sof(H52A)=Sof(H52B)=Sof(H52C)=Sof(C50)=Sof(H50A)=Sof(H50B)=
 Sof(H50C)=Sof(C47)=Sof(H47A)=Sof(H47B)=Sof(H47C)=FVAR(1)
6.a Me refined with riding coordinates:
 C70(H70A,H70B,H70C), C70(H70D,H70E,H70F)
6.b Aromatic/amide H refined with riding coordinates:
 C36(H36A), C36(H36), C8(H8B), C8(H8A), C64(H64), C66(H66), C116(H116),
 C148(H148), C114(H114), C32(H32), C30(H30), C38(H38), C144(H144), C92(H92),
 C150(H150), C60(H60), C88(H88), C94(H94), C10(H10), C2(H2), C122(H122), C4(H4),
  C142(H142), C58(H58)
6.c Idealised Me refined as rotating group:
 C111(H11A,H11B,H11C), C46(H46A,H46B,H46C), C27(H27A,H27B,H27C), C112(H11D,
 H11E,H11F), C106(H10A,H10B,H10C), C26(H26A,H26B,H26C), C166(H16A,H16B,H16C),
 C108(H10D,H10E,H10F), C16(H16D,H16E,H16F), C82(H82A,H82B,H82C), C83(H83A,H83B,
 H83C), C126(H12A,H12B,H12C), C98(H98A,H98B,H98C), C71(H71A,H71B,H71C),
 C110(H11G,H11H,H11I), C42(H42A,H42B,H42C), C127(H12D,H12E,H12F), C139(H13A,
 H13B,H13C), C140(H14A,H14B,H14C), C130(H13D,H13E,H13F), C74(H74A,H74B,H74C),
 C135(H13G,H13H,H13I), C134(H13J,H13K,H13L), C76(H76A,H76B,H76C), C107(H10G,
 H10H,H10I), C162(H16G,H16H,H16I), C48(H48A,H48B,H48C), C164(H16J,H16K,H16L),
 C44(H44A,H44B,H44C), C56(H56A,H56B,H56C), C28(H28A,H28B,H28C), C99(H99A,H99B,
 H99C), C102(H10J,H10K,H10L), C167(H16M,H16N,H16O), C78(H78A,H78B,H78C),
 C54(H54A,H54B,H54C), C155(H15A,H15B,H15C), C154(H15D,H15E,H15F), C20(H20A,H20B,
 H20C), C168(H16P,H16Q,H16R), C75(H75A,H75B,H75C), C22(H22A,H22B,H22C),
 C15(H15G,H15H,H15I), C163(H16S,H16T,H16U), C103(H10M,H10N,H10O), C156(H15J,
 H15K,H15L), C14(H14D,H14E,H14F), C132(H13M,H13N,H13O), C131(H13P,H13Q,H13R),
 C72(H72A,H72B,H72C), C55(H55A,H55B,H55C), C104(H10P,H10Q,H10R), C138(H13S,H13T,
 H13U), C18(H18A,H18B,H18C), C19(H19A,H19B,H19C), C24(H24A,H24B,H24C), C23(H23A,
 H23B,H23C), C159(H15M,H15N,H15O), C158(H15P,H15Q,H15R), C160(H16V,H16W,H16X),
 C136(H13V,H13W,H13X), C84(H84A,H84B,H84C), C128(H12G,H12H,H12I), C80(H80A,H80B,
 H80C), C79(H79A,H79B,H79C), C43(H43A,H43B,H43C), C51(H51A,H51B,H51C), C52(H52A,
 H52B,H52C), C50(H50A,H50B,H50C), C47(H47A,H47B,H47C)
;
_shelx_res_checksum              56042
_shelx_shelxl_version_number     2014/7
_olex2_submission_special_instructions 'No special instructions were received'