Synthesis and Structural Comparison of a Series of Divalent Ln(TpR,R')2 (Ln = Sm, Eu, Yb) and Trivalent Sm(TpMe2)2X (X = F, Cl, I, BPh4) Complexes
Anna C. Hillier; XingWang Zhang; Graham H. Maunder; Sung Ying Liu; Todd A. Eberspacher; Mathew V. Metz; Robert McDonald; Ângela Domingos; Noémia Marques; Victor W. Day; Andrea Sella; Josef Takats; Inorganic Chemistry 40 (2001) 5106–5116; doi:10.1021/ic010325w

data_4320304
_publ_contact_author_address
; Department of Chemistry
   University of Alberta
   Edmonton Alberta T6G 2G2
   Canada
;
_publ_contact_author_email       joe.takats@ualberta.ca
_publ_contact_author_fax         1(780)4928231
_publ_contact_author_name        'Dr Josef Takats'
_publ_contact_author_phone       1(780)4924944
_publ_section_title
;
 Synthesis and Structural Comparison of a Series of Divalent Ln(TpR,R')2
 (Ln = Sm, Eu, Yb) and Trivalent Sm(TpMe2)2X (X = F, Cl, I, BPh4)
 Complexes
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              5106
_journal_page_last               5116
_journal_paper_doi               10.1021/ic010325w
_journal_volume                  40
_journal_year                    2001
_chemical_formula_sum            'C64 H84 B3 N12 O2.5 Sm'
_chemical_formula_weight         1244.21
_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           'manual editing of SHELXL template'
_cell_angle_alpha                90.93(2)
_cell_angle_beta                 90.15(2)
_cell_angle_gamma                98.46(2)
_cell_formula_units_Z            2
_cell_length_a                   10.045(2)
_cell_length_b                   15.411(3)
_cell_length_c                   21.047(4)
_cell_measurement_reflns_used    15
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      32.47
_cell_measurement_theta_min      23.22
_cell_volume                     3222.2(11)
_computing_cell_refinement       'Syntex P1'
_computing_data_collection       'Syntex P1'
_computing_data_reduction        'Bruker SHELXTL'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'Bruker SHELXTL'
_computing_structure_solution    'Bruker SHELXTL'
_diffrn_ambient_temperature      293(2)
_diffrn_measurement_device       'Syntex P1 Diffractometer'
_diffrn_measurement_method       '\w scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'normal-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0453
_diffrn_reflns_av_sigmaI/netI    0.1336
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_number            7644
_diffrn_reflns_theta_max         21.50
_diffrn_reflns_theta_min         1.64
_diffrn_standards_decay_%        none
_diffrn_standards_interval_count 300
_diffrn_standards_number         6
_exptl_absorpt_coefficient_mu    0.964
_exptl_absorpt_correction_T_max  0.7714
_exptl_absorpt_correction_T_min  0.6151
_exptl_absorpt_correction_type   empirical
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.282
_exptl_crystal_description       'rectangular parallelepiped'
_exptl_crystal_F_000             1298
_exptl_crystal_size_max          0.68
_exptl_crystal_size_mid          0.62
_exptl_crystal_size_min          0.55
_refine_diff_density_max         0.424
_refine_diff_density_min         -0.440
_refine_diff_density_rms         0.090
_refine_ls_extinction_coef       0.0007(2)
_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_all   0.969
_refine_ls_goodness_of_fit_obs   1.102
_refine_ls_matrix_type           full
_refine_ls_number_parameters     823
_refine_ls_number_reflns         7389
_refine_ls_number_restraints     30
_refine_ls_restrained_S_all      0.970
_refine_ls_restrained_S_obs      1.104
_refine_ls_R_factor_all          0.1100
_refine_ls_R_factor_obs          0.0650
_refine_ls_shift/esd_max         -0.001
_refine_ls_shift/esd_mean        0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0492P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.1319
_refine_ls_wR_factor_obs         0.1168
_reflns_number_observed          4771
_reflns_number_total             7389
_reflns_observed_criterion       >2sigma(I)
_cod_data_source_file            ic010325w_10.cif
_cod_data_source_block           jtd4
_cod_depositor_comments
;
The following automatic conversions were performed:

'_symmetry_cell_setting' value 'Triclinic' changed to 'triclinic'
according to the built-in table from CIF Core dictionary named
'cif_core.dic' version 2.4.1 from 2010-06-29.

Automatic conversion script
Id: cif_fix_values 1646 2011-03-28 12:23:43Z adriana 

The following automatic conversions were performed:

'_refine_ls_weighting_scheme' value 'calc
w=1/[\s^2^(Fo^2^)+(0.0492P)^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^)+(0.0492P)^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 
;
_cod_original_formula_sum        'C64 H84 B3 N12 O2.50 Sm'
_cod_database_code               4320304