Formation and structural characterization of a europium(II) mono(scorpionate) complex and a sterically crowded pyraza-bole.
Liebing, Phil; Kühling, Marcel; Takats, Josef; Hilfert, Liane; Edelmann, Frank T.; Acta crystallographica. Section E, Crystallographic communications 73 (2017) 1921–1925; doi:10.1107/S2056989017016498

data_2311538
_publ_section_title
;
 Formation and structural characterization of a europium(II)
 mono(scorpionate) complex and a sterically crowded pyraza-bole.
;
_journal_coeditor_code           ZL2718
_journal_issue                   'Pt 12'
_journal_name_full
'Acta crystallographica. Section E, Crystallographic communications'
_journal_page_first              1921
_journal_page_last               1925
_journal_paper_doi               10.1107/S2056989017016498
_journal_volume                  73
_journal_year                    2017
_chemical_formula_iupac          '[Eu (C27 H46 B N6) I (C9 H16 N2)2]'
_chemical_formula_moiety         'C45 H78 B Eu I N10'
_chemical_formula_sum            'C45 H78 B Eu I N10'
_chemical_formula_weight         1048.84
_chemical_name_systematic
Bis(3,5-diisopropyl-1<i>H</i>-pyrazole)[hydrotris(3,5-diisopropylpyrazolyl)borato]iodidoeuropium(II)
_space_group_crystal_system      orthorhombic
_space_group_IT_number           61
_space_group_name_Hall           '-P 2ac 2ab'
_space_group_name_H-M_alt        'P b c a'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     heavy
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-2016/4
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   19.5319(4)
_cell_length_b                   26.6614(4)
_cell_length_c                   19.8681(3)
_cell_measurement_reflns_used    44511
_cell_measurement_temperature    153(2)
_cell_measurement_theta_max      26.193
_cell_measurement_theta_min      2.221
_cell_volume                     10346.3(3)
_computing_cell_refinement
;
X-AREA (Stoe & Cie, 2002)
;
_computing_data_collection
;
X-AREA (Stoe & Cie, 2002)
;
_computing_data_reduction
;
X-AREA and X-RED (Stoe & Cie, 2002)
;
_computing_molecular_graphics
;
DIAMOND (Brandenburg, 1999)
;
_computing_publication_material
;
publCIF (Westrip, 2010)
;
_computing_structure_refinement
;
SHELXL2016 (Sheldrick, 2015)
;
_computing_structure_solution
;
SIR97 (Altomare <i>et al.</i>,  1999)
;
_diffrn_ambient_temperature      153(2)
_diffrn_detector_area_resol_mean 6.67
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device_type  'Stoe IPDS 2T'
_diffrn_measurement_method       'area detector'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0447
_diffrn_reflns_limit_h_max       24
_diffrn_reflns_limit_h_min       -23
_diffrn_reflns_limit_k_max       32
_diffrn_reflns_limit_k_min       -32
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            43898
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         25.999
_diffrn_reflns_theta_min         2.221
_exptl_absorpt_coefficient_mu    1.848
_exptl_absorpt_correction_T_max  0.7160
_exptl_absorpt_correction_T_min  0.5349
_exptl_absorpt_correction_type   numerical
_exptl_absorpt_process_details
;
(X-AREA and X-RED; Stoe & Cie, 2002)
;
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.347
_exptl_crystal_description       block
_exptl_crystal_F_000             4312
_exptl_crystal_size_max          0.490
_exptl_crystal_size_mid          0.270
_exptl_crystal_size_min          0.210
_refine_diff_density_max         1.235
_refine_diff_density_min         -1.274
_refine_ls_extinction_coef       0.00019(2)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method
;
SHELXL2016 (Sheldrick, 2015)
;
_refine_ls_goodness_of_fit_ref   1.040
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     576
_refine_ls_number_reflns         10158
_refine_ls_number_restraints     24
_refine_ls_restrained_S_all      1.040
_refine_ls_R_factor_all          0.0455
_refine_ls_R_factor_gt           0.0313
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0226P)^2^+10.6820P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0592
_refine_ls_wR_factor_ref         0.0631
_reflns_number_gt                8229
_reflns_number_total             10158
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            zl2718sup1.cif
_cod_data_source_block           1
_cod_database_code               2311538
_shelx_estimated_absorpt_t_min   0.465
_shelx_estimated_absorpt_t_max   0.698
_shelx_hkl_checksum              96159
_shelx_res_checksum              65640