Synthesis and molecular structure of enantiomerically pure pentadienyl complexes of the rare-earth metals.
Fecker, Ann Christin; Freytag, Matthias; Jones, Peter G.; Walter, Marc D.; Dalton transactions (Cambridge, England : 2003) 48 (2019) 8297–8302; doi:10.1039/c9dt01721f

data_7700031
_publ_section_title
;
 Synthesis and molecular structure of enantiomerically pure pentadienyl
 complexes of the rare-earth metals.
;
_journal_issue                   23
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              8297
_journal_page_last               8302
_journal_paper_doi               10.1039/c9dt01721f
_journal_volume                  48
_journal_year                    2019
_chemical_absolute_configuration ad
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_chemical_formula_weight         670.08
_space_group_crystal_system      orthorhombic
_space_group_IT_number           19
_space_group_name_Hall           'P 2ac 2ab'
_space_group_name_H-M_alt        'P 21 21 21'
_symmetry_space_group_name_Hall  'P 2ac 2ab'
_symmetry_space_group_name_H-M   'P 21 21 21'
_atom_sites_solution_hydrogens   mixed
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2019-04-24 deposited with the CCDC.    2019-05-10 downloaded from the CCDC.
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_cell_angle_gamma                90
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_cell_measurement_reflns_used    6886
_cell_measurement_temperature    100(2)
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_computing_cell_refinement
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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)
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_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    'Bruker XP'
_computing_publication_material  SHELXL-2017
_computing_structure_refinement  'SHELXL-2017/1 (Sheldrick, 2017)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      100(2)
_diffrn_detector_area_resol_mean 16.1419
_diffrn_measured_fraction_theta_full 0.983
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_diffrn_measurement_method       '\w scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.1079
_diffrn_reflns_av_unetI/netI     0.0815
_diffrn_reflns_Laue_measured_fraction_full 0.983
_diffrn_reflns_Laue_measured_fraction_max 0.942
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       39
_diffrn_reflns_limit_l_min       -39
_diffrn_reflns_number            65007
_diffrn_reflns_point_group_measured_fraction_full 0.961
_diffrn_reflns_point_group_measured_fraction_max 0.908
_diffrn_reflns_theta_full        30.000
_diffrn_reflns_theta_max         30.892
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_diffrn_source                   'sealed tube'
_exptl_absorpt_coefficient_mu    1.566
_exptl_absorpt_correction_T_max  1.00000
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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)
;
_exptl_crystal_colour            orange
_exptl_crystal_density_diffrn    1.321
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             1404
_exptl_crystal_size_max          0.2
_exptl_crystal_size_mid          0.15
_exptl_crystal_size_min          0.08
_refine_diff_density_max         1.314
_refine_diff_density_min         -1.016
_refine_diff_density_rms         0.146
_refine_ls_abs_structure_details
;
 Flack x determined using 3121 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   -0.027(10)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.052
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     406
_refine_ls_number_reflns         9665
_refine_ls_number_restraints     21
_refine_ls_restrained_S_all      1.051
_refine_ls_R_factor_all          0.0588
_refine_ls_R_factor_gt           0.0418
_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^)+(0.0162P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0625
_refine_ls_wR_factor_ref         0.0689
_reflns_Friedel_coverage         0.736
_reflns_Friedel_fraction_full    0.933
_reflns_Friedel_fraction_max     0.865
_reflns_number_gt                8234
_reflns_number_total             9665
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c9dt01721f2.cif
_cod_data_source_block           ann49
_cod_depositor_comments
'Adding full bibliography for 7700030--7700033.cif.'
_cod_original_cell_volume        3368.4(3)
_cod_database_code               7700031
_shelx_shelxl_version_number     2017/1
_shelx_estimated_absorpt_t_min   0.745
_shelx_estimated_absorpt_t_max   0.885
_shelx_res_checksum              38682