Isocarbonyl complexes of divalent samarium and ytterbium. The molecular structures of [{Ln(TptBu,Me)(THF)(μ-CO)2Mo(η-C5H4Me)(CO)}2] (Ln = Sm, Yb)
Hillier, Anna C.; Sella, Andrea; Elsegood, Mark R. J.; Journal of the Chemical Society, Dalton Transactions  (1998) 3871–; doi:10.1039/a806011h

data_7027044
_publ_section_title
;
 Isocarbonyl complexes of divalent samarium and ytterbium. The molecular
 structures of [{Ln(TptBu,Me)(THF)(\m-CO)2Mo(\h-C5H4Me)(CO)}2]
 (Ln&#x2005;=&#x2005;Sm, Yb)
;
_journal_issue                   22
_journal_name_full
'Journal of the Chemical Society, Dalton Transactions'
_journal_page_first              3871
_journal_paper_doi               10.1039/a806011h
_journal_year                    1998
_chemical_formula_sum            'C82 H130 B2 Mo2 N12 O10 Sm2'
_chemical_formula_weight         1958.18
_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                63.455(2)
_cell_angle_beta                 67.914(2)
_cell_angle_gamma                88.812(2)
_cell_formula_units_Z            1
_cell_length_a                   13.6825(5)
_cell_length_b                   13.7204(5)
_cell_length_c                   15.1643(6)
_cell_measurement_reflns_used    13261
_cell_measurement_temperature    160(2)
_cell_measurement_theta_max      28.32
_cell_measurement_theta_min      1.64
_cell_volume                     2322.26(16)
_computing_cell_refinement       'local programs'
_computing_data_collection       'Siemens SMART'
_computing_data_reduction        'Siemens SAINT'
_computing_molecular_graphics    'Siemens SHELXTL'
_computing_publication_material  'SHELXTL and local programs'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      160(2)
_diffrn_measured_fraction_theta_full 0.983
_diffrn_measured_fraction_theta_max 0.871
_diffrn_measurement_device_type  'Siemens 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  0.0201
_diffrn_reflns_av_sigmaI/netI    0.0363
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_number            17258
_diffrn_reflns_theta_full        26.00
_diffrn_reflns_theta_max         28.48
_diffrn_reflns_theta_min         1.71
_diffrn_standards_decay_%        0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    1.567
_exptl_absorpt_correction_T_max  0.502
_exptl_absorpt_correction_T_min  0.361
_exptl_absorpt_correction_type   empirical
_exptl_crystal_colour            'dark blue'
_exptl_crystal_density_diffrn    1.400
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             1004
_exptl_crystal_size_max          0.65
_exptl_crystal_size_mid          0.46
_exptl_crystal_size_min          0.44
_refine_diff_density_max         1.233
_refine_diff_density_min         -0.902
_refine_diff_density_rms         0.081
_refine_ls_extinction_coef       0.00045(16)
_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   1.046
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     512
_refine_ls_number_reflns         10241
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.046
_refine_ls_R_factor_all          0.0305
_refine_ls_R_factor_gt           0.0252
_refine_ls_shift/su_max          0.004
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0261P)^2^+1.1740P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0613
_refine_ls_wR_factor_ref         0.0641
_reflns_number_gt                9234
_reflns_number_total             10241
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            806011hsup1.cif
_cod_data_source_block           as15
_cod_depositor_comments
;
The following automatic conversions were performed:

'_refine_ls_weighting_scheme' value 'calc
w=1/[\s^2^(Fo^2^)+(0.0261P)^2^+1.1740P] 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^)+(0.0261P)^2^+1.1740P] where P=(Fo^2^+2Fc^2^)/3'.

Automatic conversion script
Id: cif_fix_values 3143 2015-03-26 13:38:13Z robertas 
;
_cod_original_cell_volume        2322.26(15)
_cod_original_sg_symbol_H-M      P-1
_cod_database_code               7027044