Synthesis and catalytic activity of homoleptic lanthanide-tris(cyclopropylethinyl)amidinates
Sroor, Farid M.; Hrib, Cristian G.; Hilfert, Liane; Busse, Sabine; Edelmann, Frank T.; New J. Chem. 39 (2015) 7595–; doi:10.1039/C5NJ00555H

data_7054823
_publ_section_title
;
 Synthesis and catalytic activity of homoleptic
 lanthanide-tris(cyclopropylethinyl)amidinates
;
_journal_issue                   10
_journal_name_full               'New J. Chem.'
_journal_page_first              7595
_journal_paper_doi               10.1039/C5NJ00555H
_journal_volume                  39
_journal_year                    2015
_chemical_formula_sum            'C36 H57 Ho N6'
_chemical_formula_weight         738.81
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_audit_update_record
;
2015-02-23 deposited with the CCDC.
2015-04-15 downloaded from the CCDC.
;
_cell_angle_alpha                101.28(3)
_cell_angle_beta                 105.35(3)
_cell_angle_gamma                108.19(3)
_cell_formula_units_Z            2
_cell_length_a                   9.776(2)
_cell_length_b                   13.149(3)
_cell_length_c                   16.983(3)
_cell_measurement_reflns_used    44289
_cell_measurement_temperature    153(2)
_cell_measurement_theta_max      29.65
_cell_measurement_theta_min      2.24
_cell_volume                     1905.5(10)
_computing_cell_refinement       'STOE X-AREA'
_computing_data_collection       'STOE X-AREA'
_computing_data_reduction        'STOE X-RED'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      153(2)
_diffrn_detector_area_resol_mean 6.67
_diffrn_measured_fraction_theta_full 0.987
_diffrn_measured_fraction_theta_max 0.987
_diffrn_measurement_device_type  'STOE IPDS 2T'
_diffrn_measurement_method       'rotation method'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0598
_diffrn_reflns_av_sigmaI/netI    0.0470
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            21302
_diffrn_reflns_theta_full        29.21
_diffrn_reflns_theta_max         29.21
_diffrn_reflns_theta_min         2.31
_exptl_absorpt_coefficient_mu    2.106
_exptl_absorpt_correction_T_max  0.3338
_exptl_absorpt_correction_T_min  0.3176
_exptl_absorpt_correction_type   sphere
_exptl_absorpt_process_details
;
Interpolation using  Int.Tab. Vol. C (1992) p. 523,Tab. 6.3.3.3
for values of muR in the range 0-2.5, and Int.Tab. Vol.II (1959)
p.302; Table 5.3.6 B for muR in the range 2.6-10.0.
The interpolation procedure of C.W.Dwiggins Jr (Acta Cryst.(1975)
A31,146-148) is used with some modification.
;
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    1.288
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             764
_exptl_crystal_size_max          0.40
_exptl_crystal_size_mid          0.40
_exptl_crystal_size_min          0.20
_exptl_crystal_size_rad          0.4000
_refine_diff_density_max         2.465
_refine_diff_density_min         -1.743
_refine_diff_density_rms         0.107
_refine_ls_extinction_coef       0.0092(7)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     SHELXL
_refine_ls_goodness_of_fit_ref   1.040
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     461
_refine_ls_number_reflns         10209
_refine_ls_number_restraints     38
_refine_ls_restrained_S_all      1.038
_refine_ls_R_factor_all          0.0379
_refine_ls_R_factor_gt           0.0343
_refine_ls_shift/su_max          0.003
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0573P)^2^+0.5995P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0891
_refine_ls_wR_factor_ref         0.0908
_reflns_number_gt                9422
_reflns_number_total             10209
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c5nj00555h2.cif
_cod_data_source_block           ip298
_cod_depositor_comments
'Adding full bibliography for 7054823--7054824.cif.'
_cod_original_cell_volume        1905.6(7)
_cod_original_sg_symbol_H-M      P-1
_cod_database_code               7054823