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_4321050
_publ_section_title
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 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)
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_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            'C37 H51 B2 N12 S Sm'
_chemical_formula_weight         867.93
_chemical_name_systematic
;
 ?
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_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 108.628(2)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   15.0154(9)
_cell_length_b                   13.1853(8)
_cell_length_c                   21.1254(13)
_cell_measurement_reflns_used    12561
_cell_measurement_temperature    160(2)
_cell_measurement_theta_max      28.70
_cell_measurement_theta_min      2.52
_cell_volume                     3963.4(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 0.953
_diffrn_measured_fraction_theta_max 0.868
_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  0.0452
_diffrn_reflns_av_sigmaI/netI    0.0641
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_h_min       -19
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       27
_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_number            24634
_diffrn_reflns_theta_full        26.00
_diffrn_reflns_theta_max         28.88
_diffrn_reflns_theta_min         1.85
_diffrn_standards_decay_%        0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    1.578
_exptl_absorpt_correction_T_max  0.647
_exptl_absorpt_correction_T_min  0.568
_exptl_absorpt_correction_type   empirical
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.455
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             1780
_exptl_crystal_size_max          0.18
_exptl_crystal_size_mid          0.15
_exptl_crystal_size_min          0.12
_refine_diff_density_max         1.106
_refine_diff_density_min         -1.025
_refine_diff_density_rms         0.102
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.990
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     491
_refine_ls_number_reflns         9430
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.990
_refine_ls_R_factor_all          0.0644
_refine_ls_R_factor_gt           0.0350
_refine_ls_shift/su_max          0.003
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0344P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0687
_refine_ls_wR_factor_ref         0.0769
_reflns_number_gt                6867
_reflns_number_total             9430
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic9914793_2.cif
_cod_data_source_block           2b
_cod_depositor_comments
;
The following automatic conversions were performed:

'_refine_ls_weighting_scheme' value 'calc
w=1/[\s^2^(Fo^2^)+(0.0344P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' was
changed to 'calc'. New tag '_refine_ls_weighting_details' was
created. The value of the new tag was set to
'w=1/[\s^2^(Fo^2^)+(0.0344P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'.

Automatic conversion script
Id: cif_fix_values 3143 2015-03-26 13:38:13Z robertas 
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_cod_database_code               4321050