Lanthanide Chalcogenolate Complexes: Synthesis and Crystal Structures of the Isoleptic Series [Sm(TpMe,Me)2ER] (E = O, S, Se, Te; TpMe,Me=tris-3,5-Dimethylpyrazolylborate)
Anna C. Hillier; Sung-Ying Liu; Andrea Sella; Mark R. J. Elsegood; Inorganic Chemistry 39 (2000) 2635–2644; doi:10.1021/ic9914793

data_4321051
_publ_section_title
;
 Lanthanide Chalcogenolate Complexes: Synthesis and Crystal Structures of
 the Isoleptic Series [Sm(TpMe,Me)2ER] (E = O, S, Se, Te;
 TpMe,Me=tris-3,5-Dimethylpyrazolylborate)
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              2635
_journal_page_last               2644
_journal_paper_doi               10.1021/ic9914793
_journal_volume                  39
_journal_year                    2000
_chemical_formula_sum            'C43 H57 B2 N12 Se Sm'
_chemical_formula_weight         992.94
_chemical_name_systematic
;
 ?
;
_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
_cell_angle_alpha                79.443(2)
_cell_angle_beta                 77.428(2)
_cell_angle_gamma                89.827(2)
_cell_formula_units_Z            4
_cell_length_a                   10.7819(6)
_cell_length_b                   19.3011(10)
_cell_length_c                   23.0235(12)
_cell_measurement_reflns_used    21830
_cell_measurement_temperature    160(2)
_cell_measurement_theta_max      28.80
_cell_measurement_theta_min      2.76
_cell_volume                     4593.8(4)
_computing_cell_refinement       'local programs'
_computing_data_collection       'Bruker SMART'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'SHELXTL and local programs'
_computing_structure_refinement  'Bruker SHELXTL'
_computing_structure_solution    'Bruker SHELXTL'
_diffrn_ambient_temperature      160(2)
_diffrn_measured_fraction_theta_full 0.985
_diffrn_measured_fraction_theta_max 0.883
_diffrn_measurement_device_type  'Bruker SMART CCD diffractometer'
_diffrn_measurement_method       '\w rotation with narrow frames'
_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  0.0191
_diffrn_reflns_av_sigmaI/netI    0.0411
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       25
_diffrn_reflns_limit_k_min       -26
_diffrn_reflns_limit_l_max       31
_diffrn_reflns_limit_l_min       -30
_diffrn_reflns_number            37580
_diffrn_reflns_theta_full        26.00
_diffrn_reflns_theta_max         28.91
_diffrn_reflns_theta_min         1.85
_diffrn_standards_decay_%        0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    2.09
_exptl_absorpt_correction_T_max  0.728
_exptl_absorpt_correction_T_min  0.470
_exptl_absorpt_correction_type   empirical
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.421
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             2020
_exptl_crystal_size_max          0.42
_exptl_crystal_size_mid          0.26
_exptl_crystal_size_min          0.16
_refine_diff_density_max         0.720
_refine_diff_density_min         -0.709
_refine_diff_density_rms         0.072
_refine_ls_extinction_coef       0.00010(3)
_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   0.922
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1100
_refine_ls_number_reflns         21400
_refine_ls_number_restraints     173
_refine_ls_restrained_S_all      0.926
_refine_ls_R_factor_all          0.0432
_refine_ls_R_factor_gt           0.0282
_refine_ls_shift/su_max          0.004
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0367P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0626
_refine_ls_wR_factor_ref         0.0647
_reflns_number_gt                15804
_reflns_number_total             21400
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic9914793_3.cif
_cod_data_source_block           3a
_cod_database_code               4321051