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_4319397
_publ_section_title
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 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     '[Sm(HB(3,5Me2pz)3)2(OC5H4N)]'
_chemical_formula_sum            'C35 H48 B2 N13 O Sm'
_chemical_formula_weight         838.83
_chemical_name_common            'Bis Tp* samarium pyridinolate'
_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                76.63(1)
_cell_angle_beta                 75.98(1)
_cell_angle_gamma                59.97(1)
_cell_formula_units_Z            2
_cell_length_a                   10.881(4)
_cell_length_b                   10.927(3)
_cell_length_c                   19.737(4)
_cell_measurement_reflns_used    25
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      14.1
_cell_measurement_theta_min      7.8
_cell_volume                     1954.2(10)
_computing_cell_refinement       'CAD4 software(Enraf-Nonius,1989)'
_computing_data_collection       'CAD4 software(Enraf-Nonius,1989)'
_computing_data_reduction        process-MolEN(Fair,1990)
_computing_molecular_graphics    ORTEP(Johnson,1976)
_computing_structure_refinement  'SHELXL-93 (Sheldrick, 1993)'
_computing_structure_solution    'SHELXS-86 (Sheldrick, 1990)'
_diffrn_ambient_temperature      293(2)
_diffrn_measurement_device       CAD4-Enraf-Nonius
_diffrn_measurement_method       \w/2\qscans
_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  0.0171
_diffrn_reflns_av_sigmaI/netI    0.0409
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       0
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -10
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            6524
_diffrn_reflns_theta_max         24.03
_diffrn_reflns_theta_min         2.15
_diffrn_standards_decay_%        0.5
_diffrn_standards_interval_time  60
_diffrn_standards_number         3
_exptl_absorpt_coefficient_mu    1.549
_exptl_absorpt_correction_T_max  0.9997
_exptl_absorpt_correction_T_min  0.9336
_exptl_absorpt_correction_type   'empirical via \y-scan North et al(1968)'
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.426
_exptl_crystal_density_meas      ?
_exptl_crystal_description       plate
_exptl_crystal_F_000             858
_exptl_crystal_size_max          0.45
_exptl_crystal_size_mid          0.22
_exptl_crystal_size_min          0.18
_refine_diff_density_max         0.476
_refine_diff_density_min         -0.437
_refine_diff_density_rms         0.083
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_all   1.105
_refine_ls_goodness_of_fit_obs   1.073
_refine_ls_hydrogen_treatment    riding
_refine_ls_matrix_type           full
_refine_ls_number_parameters     469
_refine_ls_number_reflns         6158
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.114
_refine_ls_restrained_S_obs      1.073
_refine_ls_R_factor_all          0.0481
_refine_ls_R_factor_obs          0.0350
_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^)+(0.0342P)^2^+1.9493P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.0821
_refine_ls_wR_factor_obs         0.0728
_reflns_number_observed          5288
_reflns_number_total             6160
_reflns_observed_criterion       >2sigma(I)
_cod_data_source_file            ic001056x_3.cif
_cod_data_source_block           smopy
_cod_depositor_comments
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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^)+(0.0342P)^2^+1.9493P] 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^)+(0.0342P)^2^+1.9493P] 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               4319397