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_7048083
_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_absolute_configuration ad
_chemical_formula_moiety         'C78 H84 Cs O10 Yb'
_chemical_formula_sum            'C78 H84 Cs O10 Yb'
_chemical_formula_weight         1487.40
_space_group_crystal_system      monoclinic
_space_group_IT_number           5
_space_group_name_Hall           'C 2y'
_space_group_name_H-M_alt        'C 1 2 1'
_symmetry_space_group_name_Hall  'C 2y'
_symmetry_space_group_name_H-M   'C 1 2 1'
_atom_sites_solution_hydrogens   geom
_audit_creation_method           SHELXL-2018/3
_audit_update_record
;
2018-10-10 deposited with the CCDC.
2018-11-13 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 118.445(4)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   30.1708(10)
_cell_length_b                   8.39620(10)
_cell_length_c                   14.9290(9)
_cell_measurement_reflns_used    16589
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      32.48
_cell_measurement_theta_min      3.697
_cell_volume                     3325.3(3)
_computing_cell_refinement       'CrysAlisPro 1.171.39.46 (Rigaku OD, 2015)'
_computing_data_collection       'CrysAlisPro 1.171.39.46 (Rigaku OD, 2015)'
_computing_data_reduction        'CrysAlisPro 1.171.39.46 (Rigaku OD, 2015)'
_computing_molecular_graphics    'X-Seed v. 4.0 (Barbour, 2001)'
_computing_publication_material  'SHELXL-2018/3 (Sheldrick, 2015)'
_computing_structure_refinement  'SHELXL-2018/3 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT-2015/1 (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 0.956
_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      -0.0007031
_diffrn_orient_matrix_UB_12      0.0743117
_diffrn_orient_matrix_UB_13      0.0218732
_diffrn_orient_matrix_UB_21      0.0267250
_diffrn_orient_matrix_UB_22      0.0013526
_diffrn_orient_matrix_UB_23      0.0269718
_diffrn_orient_matrix_UB_31      0.0004172
_diffrn_orient_matrix_UB_32      0.0401578
_diffrn_orient_matrix_UB_33      -0.0413989
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'normal-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_unetI/netI     0.0340
_diffrn_reflns_Laue_measured_fraction_full 0.996
_diffrn_reflns_Laue_measured_fraction_max 0.956
_diffrn_reflns_limit_h_max       45
_diffrn_reflns_limit_h_min       -45
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_number            18749
_diffrn_reflns_point_group_measured_fraction_full 0.997
_diffrn_reflns_point_group_measured_fraction_max 0.933
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         32.692
_diffrn_reflns_theta_min         3.165
_exptl_absorpt_coefficient_mu    2.006
_exptl_absorpt_correction_T_max  1.0
_exptl_absorpt_correction_T_min  0.91569
_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            colorless
_exptl_crystal_density_diffrn    1.486
_exptl_crystal_description       needle
_exptl_crystal_F_000             1514
_exptl_crystal_size_max          0.240
_exptl_crystal_size_mid          0.190
_exptl_crystal_size_min          0.080
_refine_diff_density_max         5.529
_refine_diff_density_min         -1.200
_refine_diff_density_rms         0.145
_refine_ls_abs_structure_details
;
 Classical Flack method preferred over Parsons because s.u. lower.
;
_refine_ls_abs_structure_Flack   0.010(5)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.000
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     414
_refine_ls_number_reflns         18749
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.000
_refine_ls_R_factor_all          0.0391
_refine_ls_R_factor_gt           0.0368
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0744P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1007
_refine_ls_wR_factor_ref         0.1029
_reflns_Friedel_coverage         0.843
_reflns_Friedel_fraction_full    0.999
_reflns_Friedel_fraction_max     0.906
_reflns_number_gt                17754
_reflns_number_total             18749
_reflns_threshold_expression     'I > 2\s(I)'
_twin_special_details
;
Component 2 rotated by 179.9953\% 
 around [1.00 0.00 0.01] (reciprocal) or [0.71 0.00 0.71] (direct)
;
_cod_data_source_file            c8dt03585g2.cif
_cod_data_source_block           mxm259la
_cod_depositor_comments
'Adding full bibliography for 7048079--7048089.cif.'
_cod_database_code               7048083
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_min   0.645
_shelx_estimated_absorpt_t_max   0.856
_oxdiff_twin_integration_method  simultaneous
_shelx_res_checksum              67758