Solid-State Structure and Solution Behavior of Eight-Coordinate Sm(III) Poly(pyrazolyl)borate Compounds
Irene Lopes; Anna C. Hillier; Sung Ying Liu; Ângela Domingos; José Ascenso; Adelino Galvão; Andrea Sella; Noémia Marques; Inorganic Chemistry 40 (2001) 1116–1125; doi:10.1021/ic001056x

data_4319395
_publ_section_title
;
 Solid-State Structure and Solution Behavior of Eight-Coordinate Sm(III)
 Poly(pyrazolyl)borate Compounds
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              1116
_journal_page_last               1125
_journal_paper_doi               10.1021/ic001056x
_journal_volume                  40
_journal_year                    2001
_chemical_formula_structural     '[(HB(C5H7N2)3)2Sm(S2CNEt2)]'
_chemical_formula_sum            'C35 H54 B2 N13 S2 Sm'
_chemical_formula_weight         893.00
_chemical_name_common            'Bis Tp* samarium diethyldithiocarbamate'
_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
_cell_angle_alpha                84.19(3)
_cell_angle_beta                 82.14(3)
_cell_angle_gamma                71.92(3)
_cell_formula_units_Z            2
_cell_length_a                   11.459(2)
_cell_length_b                   12.787(3)
_cell_length_c                   15.062(3)
_cell_measurement_temperature    150(2)
_cell_volume                     2074.2(8)
_computing_cell_refinement       'COLLECT software(R.Hooft, Nonius B.V.,1998)'
_computing_data_collection       'COLLECT software(R.t, Nonius B.V.,1998)'
_computing_data_reduction        'process-DENZO(Z.Otwinowski and W.Minor)'
_computing_molecular_graphics    'ORTEP (Johnson,1976)'
_computing_structure_refinement  'SHELXL-93 (Sheldrick, 1993)'
_computing_structure_solution    'SHELXS-86 (Sheldrick, 1990)'
_diffrn_ambient_temperature      150(2)
_diffrn_measurement_device       'Delft FAST TV Area detector'
_diffrn_measurement_method       '0.2 deg frame increments through phi'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'rotating anode'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0000
_diffrn_reflns_av_sigmaI/netI    0.1047
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_number            5663
_diffrn_reflns_theta_max         24.98
_diffrn_reflns_theta_min         1.88
_exptl_absorpt_coefficient_mu    1.559
_exptl_absorpt_correction_type   DIFABS
_exptl_crystal_colour            pale-yellow
_exptl_crystal_density_diffrn    1.430
_exptl_crystal_density_meas      ?
_exptl_crystal_description       block
_exptl_crystal_F_000             918
_exptl_crystal_size_max          0.25
_exptl_crystal_size_mid          0.2
_exptl_crystal_size_min          0.2
_refine_diff_density_max         1.360
_refine_diff_density_min         -0.868
_refine_diff_density_rms         0.158
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_all   1.014
_refine_ls_goodness_of_fit_obs   1.074
_refine_ls_matrix_type           full
_refine_ls_number_parameters     478
_refine_ls_number_reflns         5645
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.175
_refine_ls_restrained_S_obs      1.074
_refine_ls_R_factor_all          0.0514
_refine_ls_R_factor_obs          0.0451
_refine_ls_shift/esd_max         0.000
_refine_ls_shift/esd_mean        0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0475P)^2^+2.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.1381
_refine_ls_wR_factor_obs         0.1181
_reflns_number_observed          4979
_reflns_number_total             5663
_reflns_observed_criterion       >2sigma(I)
_cod_data_source_file            ic001056x_1.cif
_cod_data_source_block           s92
_cod_depositor_comments
;
The following automatic conversions were performed:

'_exptl_crystal_density_meas' value 'not measured' was changed to '?'
- the value is perceived as not measured.

Automatic conversion script
Id: cif_fix_values 3008 2015-01-20 13:52:24Z robertas 

The following automatic conversions were performed:

'_refine_ls_weighting_scheme' value 'calc
w=1/[\s^2^(Fo^2^)+(0.0475P)^2^+2.0000P] 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^)+(0.0475P)^2^+2.0000P] 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        2074.2(7)
_cod_database_code               4319395