Versatile Ln2(μ-NR)2-Imide Platforms for Ligand Exchange and Isoprene Polymerization
Schädle, Dorothea; Schädle, Christoph; Schneider, David; Maichle-Mössmer, Cäcilia; Anwander, Reiner; Organometallics 34 (2015) 4994–; doi:10.1021/acs.organomet.5b00589

data_4087774
_publ_section_title
;
 Versatile Ln2(\m-NR)2-Imide Platforms for Ligand Exchange and Isoprene
 Polymerization
;
_journal_issue                   20
_journal_name_full               Organometallics
_journal_page_first              4994
_journal_paper_doi               10.1021/acs.organomet.5b00589
_journal_volume                  34
_journal_year                    2015
_chemical_formula_sum            'C39 H77 Al La2 N4 Si4'
_chemical_formula_weight         1018.95
_space_group_crystal_system      monoclinic
_space_group_IT_number           9
_space_group_name_Hall           'C -2yc'
_space_group_name_H-M_alt        'C 1 c 1'
_atom_sites_solution_hydrogens   geom
_cell_angle_alpha                90
_cell_angle_beta                 93.3330(10)
_cell_angle_gamma                90
_cell_formula_units_Z            16
_cell_length_a                   20.8139(5)
_cell_length_b                   37.7028(10)
_cell_length_c                   25.5412(6)
_cell_measurement_reflns_used    3055
_cell_measurement_temperature    100.(2)
_cell_measurement_theta_max      34.7041
_cell_measurement_theta_min      2.3459
_cell_volume                     20009.4(9)
_computing_cell_refinement       'APEX2 v2013.6-2 (Bruker AXS)'
_computing_data_collection       'COSMO v1.61'
_computing_data_reduction        'SAINT V8.27B (Bruker AXS Inc., 2012)'
_computing_molecular_graphics    'Ortep3, POV-Ray'
_computing_structure_refinement  'SHELXL-2013 (Sheldrick, 2013)'
_computing_structure_solution    'SHELXS-2013 (Sheldrick, 2013)'
_diffrn_ambient_temperature      100.(2)
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 1.000
_diffrn_measurement_device_type  'Bruker ApexDuo'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_radiation_monochromator  'QUAZAR optics'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0515
_diffrn_reflns_limit_h_max       27
_diffrn_reflns_limit_h_min       -27
_diffrn_reflns_limit_k_max       50
_diffrn_reflns_limit_k_min       -50
_diffrn_reflns_limit_l_max       34
_diffrn_reflns_limit_l_min       -34
_diffrn_reflns_number            196947
_diffrn_reflns_theta_full        28.28
_diffrn_reflns_theta_max         28.28
_diffrn_reflns_theta_min         1.34
_diffrn_source                   'ImuS-focus sealed tube'
_exptl_absorpt_coefficient_mu    1.827
_exptl_absorpt_correction_T_max  0.80
_exptl_absorpt_correction_T_min  0.55
_exptl_absorpt_correction_type   numerical
_exptl_absorpt_process_details   'SADABS V2012/1 (Bruker AXS Inc.)'
_exptl_crystal_colour            'clear colourless'
_exptl_crystal_density_diffrn    1.353
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             8348
_exptl_crystal_size_max          0.370
_exptl_crystal_size_mid          0.130
_exptl_crystal_size_min          0.130
_refine_diff_density_max         1.650
_refine_diff_density_min         -0.708
_refine_ls_abs_structure_details
;
Flack x determined using 19887 quotients [(I+)-(I-)]/[(I+)+(I-)]
(Parsons and Flack (2004), Acta Cryst. A60, s61).
;
_refine_ls_abs_structure_Flack   0.139(3)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.995
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1890
_refine_ls_number_reflns         49365
_refine_ls_number_restraints     2
_refine_ls_restrained_S_all      0.995
_refine_ls_R_factor_all          0.0409
_refine_ls_R_factor_gt           0.0335
_refine_ls_shift/su_max          0.005
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0342P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0676
_refine_ls_wR_factor_ref         0.0708
_reflns_number_gt                44444
_reflns_number_total             49365
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            om5b00589_si_002.cif
_cod_data_source_block           Compound_4-La
_cod_depositor_comments
;

2020-06-08
Z value and formula fixed to values more according to usual
chemical conventions.                 miguel
;
_cod_original_formula_sum            'C156 H307 Al4 La8 N16 Si16'
_cod_original_formula_weight         4075.80
_cod_original_formula_units_Z            4
_cod_database_code               4087774
_shelx_res_checksum              74926