Synthesis, Structure, and Ion Pair Dynamics of β-Diketiminato-Supported Organoscandium Contact Ion Pairs
Hayes, Paul G.; Piers, Warren E.; Parvez, Masood; Organometallics 24 (2005) 1173–; doi:10.1021/om050007v

data_4075791
_publ_section_title
;
 Synthesis, Structure, and Ion Pair Dynamics of \b-Diketiminato-Supported
 Organoscandium Contact Ion Pairs
;
_journal_issue                   6
_journal_name_full               Organometallics
_journal_page_first              1173
_journal_paper_doi               10.1021/om050007v
_journal_volume                  24
_journal_year                    2005
_chemical_formula_sum            'C55.5 H47.5 B F20 N2 Sc'
_chemical_formula_weight         1178.22
_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
_cell_angle_alpha                82.7740(6)
_cell_angle_beta                 73.6650(6)
_cell_angle_gamma                73.6860(8)
_cell_formula_units_Z            2
_cell_length_a                   12.2225(2)
_cell_length_b                   13.9703(2)
_cell_length_c                   16.9809(3)
_cell_measurement_reflns_used    16150
_cell_measurement_temperature    170(2)
_cell_measurement_theta_max      24.0
_cell_measurement_theta_min      2.7
_cell_volume                     2667.00(8)
_computing_cell_refinement       'HKL DENZO (Otwinowski & Minor, 1997)'
_computing_data_collection       'COLLECT (Hooft, 1998)'
_computing_data_reduction        'SCALEPACK (Otwinowski & Minor, 1997)'
_computing_molecular_graphics    'ORTEPII (Johnson, 1976)'
_computing_publication_material  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SAPI91 (Fan, 1991)'
_diffrn_ambient_temperature      170(2)
_diffrn_measured_fraction_theta_full 0.996
_diffrn_measured_fraction_theta_max 0.996
_diffrn_measurement_device_type  'Nonius KappaCCD'
_diffrn_measurement_method       ' \w and \f '
_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  0.0228
_diffrn_reflns_av_sigmaI/netI    0.0394
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            16150
_diffrn_reflns_theta_full        24.00
_diffrn_reflns_theta_max         24.00
_diffrn_reflns_theta_min         2.77
_exptl_absorpt_coefficient_mu    0.248
_exptl_absorpt_correction_T_max  0.9521
_exptl_absorpt_correction_T_min  0.9294
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SORTAV: (Blessing, 1997)'
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.467
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             1201
_exptl_crystal_size_max          0.30
_exptl_crystal_size_mid          0.25
_exptl_crystal_size_min          0.20
_refine_diff_density_max         0.703
_refine_diff_density_min         -0.704
_refine_diff_density_rms         0.096
_refine_ls_extinction_coef       0.013(3)
_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   1.087
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     716
_refine_ls_number_reflns         8321
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.087
_refine_ls_R_factor_all          0.0902
_refine_ls_R_factor_gt           0.0736
_refine_ls_shift/su_max          0.008
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.1574P)^2^+3.1431P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2329
_refine_ls_wR_factor_ref         0.2517
_reflns_number_gt                6513
_reflns_number_total             8321
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            om050007vsi20050104_103951.cif
_cod_data_source_block           Compound_p5
_cod_depositor_comments
;
The following automatic conversions were performed:

'_symmetry_cell_setting' value 'Triclinic' changed to 'triclinic'
according to /home/saulius/struct/CIF-dictionaries/cif_core.dic
dictionary named 'cif_core.dic' version 2.4.1 from 2010-06-29.

Automatic conversion script
Id: cif_fix_values 1715 2011-07-08 13:25:40Z adriana 

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 
;
_cod_original_cell_volume        2667.00(7)
_cod_original_formula_sum        'C55.50 H47.50 B F20 N2 Sc'
_cod_database_code               4075791