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_7700033
_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
_chemical_formula_sum            'C39 H57 Pr'
_chemical_formula_weight         666.75
_space_group_crystal_system      monoclinic
_space_group_IT_number           4
_space_group_name_Hall           'P 2yb'
_space_group_name_H-M_alt        'P 1 21 1'
_symmetry_space_group_name_Hall  'P 2yb'
_symmetry_space_group_name_H-M   'P 1 21 1'
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-2017/1
_audit_update_record
;
2019-04-24 deposited with the CCDC.    2019-05-10 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 97.142(3)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   9.4762(3)
_cell_length_b                   18.0442(7)
_cell_length_c                   19.7324(7)
_cell_measurement_reflns_used    17227
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      29.3750
_cell_measurement_theta_min      2.4300
_cell_volume                     3347.9(2)
_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
;
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-97
_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 0.985
_diffrn_measured_fraction_theta_max 0.961
_diffrn_measurement_device_type  'Oxford Diffraction Xcalibur, Eos'
_diffrn_measurement_method       '\w scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0997
_diffrn_reflns_av_unetI/netI     0.0741
_diffrn_reflns_Laue_measured_fraction_full 0.985
_diffrn_reflns_Laue_measured_fraction_max 0.961
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       25
_diffrn_reflns_limit_k_min       -25
_diffrn_reflns_limit_l_max       28
_diffrn_reflns_limit_l_min       -28
_diffrn_reflns_number            154014
_diffrn_reflns_point_group_measured_fraction_full 0.967
_diffrn_reflns_point_group_measured_fraction_max 0.940
_diffrn_reflns_theta_full        30.500
_diffrn_reflns_theta_max         30.891
_diffrn_reflns_theta_min         2.166
_diffrn_source                   'sealed tube'
_exptl_absorpt_coefficient_mu    1.480
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.90667
_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)
;
_exptl_crystal_colour            orange
_exptl_crystal_density_diffrn    1.323
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             1400
_exptl_crystal_size_max          0.3
_exptl_crystal_size_mid          0.15
_exptl_crystal_size_min          0.02
_refine_diff_density_max         0.999
_refine_diff_density_min         -0.767
_refine_diff_density_rms         0.129
_refine_ls_abs_structure_details
;
 Flack x determined using 7004 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   -0.035(5)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.031
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     813
_refine_ls_number_reflns         19885
_refine_ls_number_restraints     97
_refine_ls_restrained_S_all      1.029
_refine_ls_R_factor_all          0.0578
_refine_ls_R_factor_gt           0.0392
_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^)+(0.0238P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0629
_refine_ls_wR_factor_ref         0.0689
_reflns_Friedel_coverage         0.901
_reflns_Friedel_fraction_full    0.949
_reflns_Friedel_fraction_max     0.917
_reflns_number_gt                16814
_reflns_number_total             19885
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c9dt01721f2.cif
_cod_data_source_block           ann67
_cod_depositor_comments
'Adding full bibliography for 7700030--7700033.cif.'
_cod_database_code               7700033
_shelx_shelxl_version_number     2017/1
_shelx_estimated_absorpt_t_min   0.665
_shelx_estimated_absorpt_t_max   0.971
_shelx_res_checksum              89578