Dinuclear triple stranded phenyl-spaced 1,3-bis-β-diketonato lanthanide(iii) complexes: synthesis, structures and spectroscopy.
Brock, A. J.; Etchells, I. M.; Moore, E. G.; Clegg, J. K.; Dalton transactions (Cambridge, England : 2003) 50 (2021) 4874–4879; doi:10.1039/d1dt00393c

data_7706845
_publ_section_title
;
 Dinuclear triple stranded phenyl-spaced 1,3-bis-\b-diketonato
 lanthanide(iii) complexes: synthesis, structures and spectroscopy.
;
_journal_issue                   14
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              4874
_journal_page_last               4879
_journal_paper_doi               10.1039/d1dt00393c
_journal_volume                  50
_journal_year                    2021
_chemical_formula_moiety         'C66 H86 N2 O14 Y2'
_chemical_formula_sum            'C66 H86 N2 O14 Y2'
_chemical_formula_weight         1309.18
_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   geom
_atom_sites_solution_primary     direct
_audit_creation_date             2020-01-20
_audit_creation_method
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Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_audit_update_record
;
2020-01-21 deposited with the CCDC.	2021-03-15 downloaded from the CCDC.
;
_cell_angle_alpha                101.358(3)
_cell_angle_beta                 108.770(4)
_cell_angle_gamma                112.441(4)
_cell_formula_units_Z            2
_cell_length_a                   13.4348(6)
_cell_length_b                   17.2117(8)
_cell_length_c                   17.8147(7)
_cell_measurement_reflns_used    11636
_cell_measurement_temperature    190
_cell_measurement_theta_max      30.1340
_cell_measurement_theta_min      3.3870
_cell_volume                     3355.7(3)
_computing_cell_refinement
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.28 (release 01-02-2013 CrysAlis171 .NET)
(compiled Feb  1 2013,16:14:44)
;
_computing_data_collection
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CrysAlisPro, Agilent Technologies,
Version 1.171.36.28 (release 01-02-2013 CrysAlis171 .NET)
(compiled Feb  1 2013,16:14:44)
;
_computing_data_reduction
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CrysAlisPro, Agilent Technologies,
Version 1.171.36.28 (release 01-02-2013 CrysAlis171 .NET)
(compiled Feb  1 2013,16:14:44)
;
_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      190.15
_diffrn_detector_area_resol_mean 16.0696
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.995
_diffrn_measurement_details
;
  1 omega    0.00   90.00   1.0000   37.5000
omega____ theta____ kappa____ phi______ frames
    -       21.6102   57.0000  -30.0000 90

  2 omega   -8.00   92.00   1.0000   37.5000
omega____ theta____ kappa____ phi______ frames
    -       21.6102   77.0000  -90.0000 100

  3 omega   -4.00   64.00   1.0000   37.5000
omega____ theta____ kappa____ phi______ frames
    -       21.6102  -99.0000   60.0000 68

  4 omega  -53.00   48.00   1.0000   37.5000
omega____ theta____ kappa____ phi______ frames
    -      -22.5477   77.0000  -60.0000 101

  5 omega  -48.00   50.00   1.0000   37.5000
omega____ theta____ kappa____ phi______ frames
    -      -22.5477   38.0000   60.0000 98

  6 omega  -93.00    8.00   1.0000   37.5000
omega____ theta____ kappa____ phi______ frames
    -      -22.5477  -77.0000 -180.0000 101

  7 omega  -93.00    8.00   1.0000   37.5000
omega____ theta____ kappa____ phi______ frames
    -      -22.5477  -77.0000   90.0000 101

  8 omega  -98.00  -49.00   1.0000   37.5000
omega____ theta____ kappa____ phi______ frames
    -      -22.5477 -178.0000   90.0000 49
;
_diffrn_measurement_device_type  'Xcalibur, Sapphire3, Gemini ultra'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_UB_11      -0.0027825000
_diffrn_orient_matrix_UB_12      0.0271356000
_diffrn_orient_matrix_UB_13      -0.0250362000
_diffrn_orient_matrix_UB_21      -0.0133827000
_diffrn_orient_matrix_UB_22      0.0254004000
_diffrn_orient_matrix_UB_23      0.0279404000
_diffrn_orient_matrix_UB_31      0.0620549000
_diffrn_orient_matrix_UB_32      0.0302123000
_diffrn_orient_matrix_UB_33      0.0251666000
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0529
_diffrn_reflns_av_unetI/netI     0.0745
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.995
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_h_min       -18
_diffrn_reflns_limit_k_max       23
_diffrn_reflns_limit_k_min       -22
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_limit_l_min       -24
_diffrn_reflns_number            48926
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.995
_diffrn_reflns_theta_full        26.000
_diffrn_reflns_theta_max         28.700
_diffrn_reflns_theta_min         3.295
_diffrn_source                   'Enhance (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    1.782
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.49999
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.28 (release 01-02-2013 CrysAlis171 .NET)
(compiled Feb  1 2013,16:14:44)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            colourless
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.296
_exptl_crystal_description       block
_exptl_crystal_F_000             1372
_exptl_crystal_size_max          0.5
_exptl_crystal_size_mid          0.5
_exptl_crystal_size_min          0.5
_refine_diff_density_max         0.761
_refine_diff_density_min         -0.599
_refine_diff_density_rms         0.075
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.026
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     769
_refine_ls_number_reflns         17239
_refine_ls_number_restraints     65
_refine_ls_restrained_S_all      1.052
_refine_ls_R_factor_all          0.0794
_refine_ls_R_factor_gt           0.0470
_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^)+(0.0497P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1036
_refine_ls_wR_factor_ref         0.1171
_reflns_Friedel_coverage         0.000
_reflns_number_gt                12177
_reflns_number_total             17239
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d1dt00393c2.cif
_cod_data_source_block           jkc14ab10
_cod_depositor_comments
'Adding full bibliography for 7706844--7706847.cif.'
_cod_database_code               7706845
_shelx_shelxl_version_number     2018/3
_chemical_oxdiff_formula         'P6 N4 C32 H54'
_reflns_odcompleteness_completeness 99.85
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     28.22
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Restrained distances
 C01V-C02B \\sim C01V-C0AA
 with sigma of 0.02
 C01V-C02C \\sim C01V-C02D
 with sigma of 0.02
3. Uiso/Uaniso restraints and constraints
Uanis(C02C) \\sim Ueq, Uanis(C02D) \\sim Ueq, Uanis(C02B) \\sim Ueq,
Uanis(C0AA) \\sim Ueq: with sigma of 0.005 and sigma for terminal atoms of 0.01
Uanis(C028) \\sim Ueq, Uanis(C027) \\sim Ueq: with sigma of 0.005 and sigma for
terminal atoms of 0.01
Uanis(C028) \\sim Ueq, Uanis(C027) \\sim Ueq: with sigma of 0.001 and sigma for
terminal atoms of 0.002
Uanis(C02C) = Uanis(C02D)
Uanis(C02B) = Uanis(C0AA)
4. Rigid body (RIGU) restrains
 C01V, C026, C02B, C02C
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 C01V, C02C, C02D, C02B, C0AA
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
5. Others
 Sof(C02D)=Sof(H4AA)=Sof(HR)=Sof(HS)=Sof(C0AA)=Sof(H0AB)=Sof(H0AC)=Sof(H0AD)=1-
 FVAR(1)
 Sof(C02B)=Sof(H2AA)=Sof(HN)=Sof(HO)=Sof(C02C)=Sof(H3AA)=Sof(HP)=Sof(HQ)=FVAR(1)
6.a Me refined with riding coordinates:
 C01L(H01A,H01D,H01H), C01N(H01J,H01L,H01M), C01R(H01N,H01Q,H01R), C01S(H01S,
 H01T,H01U), C01T(H01V,H01W,H01X), C01U(H01Y,H,HA), C01W(H01Z,HB,HC), C01X(H01,
 HD,HE), C01Y(H0AA,HF,HG), C020(H02A,H02B,H02C), C021(H02D,H02E,H02F),
 C022(H02G,H02H,H02I), C023(H02J,H02K,H02L), C024(H02M,H02N,H02O), C025(H02P,
 H02Q,H02R), C027(H02V,H02W,H02X), C028(H02Y,HH,HI), C029(H02Z,HJ,HK), C02A(H02,
 HL,HM)
6.b Aromatic/amide H refined with riding coordinates:
 C00J(H00J), C00M(H00M), C00R(H00R), C00T(H00T), C00U(H00U), C00X(H00X),
 C00Y(H00Y), C015(H015), C017(H017), C019(H019), C01B(H01B), C01C(H01C),
 C01E(H01E), C01F(H01F), C01G(H01G), C01I(H01I), C01K(H01K), C01O(H01O),
 C01P(H01P), C01Z(H1AA)
6.c Idealised Me refined as rotating group:
 C026(H02S,H02T,H02U), C02B(H2AA,HN,HO), C02C(H3AA,HP,HQ), C02D(H4AA,HR,HS),
 C0AA(H0AB,H0AC,H0AD)
;
_shelx_res_checksum              38386
_shelx_hkl_checksum              7593
_olex2_submission_special_instructions 'No special instructions were received'