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_4320302
_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            'C30 H44 B2 Cl N12 Sm'
_chemical_formula_weight         780.19
_space_group_IT_number           33
_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_Hall  'P 2c -2n'
_symmetry_space_group_name_H-M   'P n a 21'
_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                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   18.610(3)
_cell_length_b                   10.383(2)
_cell_length_c                   18.634(3)
_cell_measurement_reflns_used    15
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      26.46
_cell_measurement_theta_min      20.49
_cell_volume                     3600.6(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  0.0000
_diffrn_reflns_av_sigmaI/netI    0.0731
_diffrn_reflns_limit_h_max       22
_diffrn_reflns_limit_h_min       0
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_number            3411
_diffrn_reflns_theta_max         25.36
_diffrn_reflns_theta_min         2.19
_diffrn_standards_decay_%        none
_diffrn_standards_interval_count 300
_diffrn_standards_number         6
_exptl_absorpt_coefficient_mu    1.744
_exptl_absorpt_correction_T_max  0.7058
_exptl_absorpt_correction_T_min  0.6320
_exptl_absorpt_correction_type   empirical
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.439
_exptl_crystal_description       parallelepiped
_exptl_crystal_F_000             1588
_exptl_crystal_size_max          0.56
_exptl_crystal_size_mid          0.52
_exptl_crystal_size_min          0.50
_refine_diff_density_max         0.393
_refine_diff_density_min         -0.435
_refine_diff_density_rms         0.081
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   0.07(2)
_refine_ls_extinction_coef       0.00047(5)
_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   0.976
_refine_ls_goodness_of_fit_obs   1.140
_refine_ls_matrix_type           full
_refine_ls_number_parameters     471
_refine_ls_number_reflns         3411
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.976
_refine_ls_restrained_S_obs      1.140
_refine_ls_R_factor_all          0.0814
_refine_ls_R_factor_obs          0.0456
_refine_ls_shift/esd_max         0.005
_refine_ls_shift/esd_mean        0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0203P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.0683
_refine_ls_wR_factor_obs         0.0607
_reflns_number_observed          2171
_reflns_number_total             3411
_reflns_observed_criterion       >2sigma(I)
_cod_data_source_file            ic010325w_08.cif
_cod_data_source_block           ase1
_cod_depositor_comments
;
The following automatic conversions were performed:

'_symmetry_cell_setting' value 'Orthorhombic' changed to
'orthorhombic' 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^)+(0.0203P)^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^)+(0.0203P)^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_database_code               4320302