Lanthanoid complexes supported by retro-Claisen condensation products of β-triketonates.
Abad Galán, Laura; Sobolev, Alexandre N.; Zysman-Colman, Eli; Ogden, Mark I.; Massi, Massimiliano; Dalton transactions (Cambridge, England : 2003) 47 (2018) 17469–17478; doi:10.1039/c8dt03585g

data_7048081
_publ_section_title
;
 Lanthanoid complexes supported by retro-Claisen condensation products of
 \b-triketonates.
;
_journal_issue                   48
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              17469
_journal_page_last               17478
_journal_paper_doi               10.1039/c8dt03585g
_journal_volume                  47
_journal_year                    2018
_chemical_formula_moiety         'C96 H102 O14 Yb2, C H4 O'
_chemical_formula_sum            'C97 H106 O15 Yb2'
_chemical_formula_weight         1857.89
_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'
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/c 1'
_atom_sites_solution_hydrogens   geom
_audit_creation_method           SHELXL-2014/7
_audit_update_record
;
2018-10-10 deposited with the CCDC.
2018-11-13 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 102.091(1)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   18.0271(3)
_cell_length_b                   14.4367(2)
_cell_length_c                   34.8079(3)
_cell_measurement_reflns_used    43027
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      67.659
_cell_measurement_theta_min      3.939
_cell_volume                     8857.9(2)
_computing_cell_refinement       'CrysAlisPro 1.171.38.46 (Rigaku OD, 2015)'
_computing_data_collection       'CrysAlisPro 1.171.38.46 (Rigaku OD, 2015)'
_computing_data_reduction        'CrysAlisPro 1.171.38.46 (Rigaku OD, 2015)'
_computing_publication_material  'SHELXL-2014/7 (Sheldrick, 2015)'
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXS (Sheldrick, 2015)'
_diffrn_ambient_temperature      100(2)
_diffrn_detector_area_resol_mean 10.4738
_diffrn_measured_fraction_theta_full 0.996
_diffrn_measured_fraction_theta_max 0.996
_diffrn_measurement_device_type  'Oxford Diffraction Gemini-R Ultra, Ruby CCD'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      -0.0092303
_diffrn_orient_matrix_UB_12      -0.0161500
_diffrn_orient_matrix_UB_13      -0.0444999
_diffrn_orient_matrix_UB_21      -0.0577137
_diffrn_orient_matrix_UB_22      -0.0777366
_diffrn_orient_matrix_UB_23      0.0018436
_diffrn_orient_matrix_UB_31      -0.0649782
_diffrn_orient_matrix_UB_32      0.0712990
_diffrn_orient_matrix_UB_33      -0.0080684
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_source         'Enhance Ultra (Cu) X-ray Source'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54178
_diffrn_reflns_av_unetI/netI     0.0206
_diffrn_reflns_Laue_measured_fraction_full 0.996
_diffrn_reflns_Laue_measured_fraction_max 0.996
_diffrn_reflns_limit_h_max       21
_diffrn_reflns_limit_h_min       -21
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       41
_diffrn_reflns_limit_l_min       -41
_diffrn_reflns_number            26738
_diffrn_reflns_point_group_measured_fraction_full 0.996
_diffrn_reflns_point_group_measured_fraction_max 0.996
_diffrn_reflns_theta_full        67.679
_diffrn_reflns_theta_max         67.681
_diffrn_reflns_theta_min         3.958
_exptl_absorpt_coefficient_mu    4.306
_exptl_absorpt_correction_T_max  1.0
_exptl_absorpt_correction_T_min  0.57211
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.38.46 (Rigaku Oxford Diffraction, 2015)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            'pale yellow'
_exptl_crystal_density_diffrn    1.393
_exptl_crystal_description       plate
_exptl_crystal_F_000             3792
_exptl_crystal_size_max          0.300
_exptl_crystal_size_mid          0.270
_exptl_crystal_size_min          0.120
_refine_diff_density_max         1.990
_refine_diff_density_min         -1.352
_refine_diff_density_rms         0.148
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.250
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1050
_refine_ls_number_reflns         26738
_refine_ls_number_restraints     7
_refine_ls_restrained_S_all      1.251
_refine_ls_R_factor_all          0.0727
_refine_ls_R_factor_gt           0.0696
_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^)+(0.0359P)^2^+89.9172P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1772
_refine_ls_wR_factor_ref         0.1785
_reflns_Friedel_coverage         0.000
_reflns_number_gt                25451
_reflns_number_total             26738
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c8dt03585g2.cif
_cod_data_source_block           mxm260la
_cod_depositor_comments
'Adding full bibliography for 7048079--7048089.cif.'
_cod_database_code               7048081
_shelx_shelxl_version_number     2014/7
_shelx_estimated_absorpt_t_min   0.358
_shelx_estimated_absorpt_t_max   0.626
_oxdiff_twin_integration_method  simultaneous
_twin_special_details
;
Component 2 rotated by -179.9721\% 
 around [-0.00 0.00 1.00] (reciprocal) or [0.37 0.00 0.93] (direct)
;
_shelx_res_checksum              96220