Primary and secondary coordination of crown ethers to scandium(iii). Synthesis, properties and structures of the reaction products of ScCl3(thf)3, ScCl3·6H2O and Sc(NO3)3·5H2O with crown ethers
Brown, Michael D.; Levason, William; Murray, David C.; Popham, Michael C.; Reid, Gillian; Webster, Michael; Dalton Transactions  (2003) 857–; doi:10.1039/b210458j

data_7012362
_publ_section_title
;
 Primary and secondary coordination of crown ethers to scandium(iii).
 Synthesis, properties and structures of the reaction products of
 ScCl3(thf)3, ScCl3&#x00B7;6H2O and Sc(NO3)3&#x00B7;5H2O with crown
 ethers
;
_journal_issue                   5
_journal_name_full               'Dalton Transactions'
_journal_page_first              857
_journal_paper_doi               10.1039/b210458j
_journal_year                    2003
_chemical_formula_moiety         'C12 H24 CL2 O6 Sc 1+, Cl4 Fe 1-'
_chemical_formula_sum            'C12 H24 Cl6 Fe O6 Sc'
_chemical_formula_weight         577.82
_chemical_name_systematic
; 
dichloro(1,4,7,10,13,16-hexaoxacyclooctadecane)scandium(III)
tetrachloroiron(III) 
;
_space_group_IT_number           33
_symmetry_cell_setting           orthorhombic
_symmetry_Int_Tables_number      33
_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           'SHELXL-97 + template + hand edit'
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                90.00
_cell_formula_units_Z            8
_cell_length_a                   19.2026(15)
_cell_length_b                   11.2156(10)
_cell_length_c                   21.0990(15)
_cell_measurement_reflns_used    22453
_cell_measurement_temperature    120(2)
_cell_measurement_theta_max      27.48
_cell_measurement_theta_min      2.91
_cell_volume                     4544.1(6)
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1997)'
_diffrn_ambient_temperature      120(2)
_diffrn_measured_fraction_theta_full 0.994
_diffrn_measured_fraction_theta_max 0.994
_diffrn_measurement_device_type  'area detector, Nonius Kappa ccd'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'Nonius rotating anode'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0599
_diffrn_reflns_av_sigmaI/netI    0.0708
_diffrn_reflns_limit_h_max       24
_diffrn_reflns_limit_h_min       -22
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       26
_diffrn_reflns_limit_l_min       -27
_diffrn_reflns_number            33479
_diffrn_reflns_theta_full        27.49
_diffrn_reflns_theta_max         27.49
_diffrn_reflns_theta_min         2.95
_exptl_absorpt_coefficient_mu    1.667
_exptl_absorpt_correction_T_max  0.8875
_exptl_absorpt_correction_T_min  0.8157
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
'SORTAV, R H Blessing, J. Appl. Cryst., 1997, 30, 421-426.'
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.689
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             2344
_exptl_crystal_size_max          0.26
_exptl_crystal_size_mid          0.26
_exptl_crystal_size_min          0.20
_refine_diff_density_max         0.437
_refine_diff_density_min         -0.558
_refine_diff_density_rms         0.093
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   0.095(14)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.992
_refine_ls_hydrogen_treatment    refU
_refine_ls_matrix_type           full
_refine_ls_number_parameters     470
_refine_ls_number_reflns         10116
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      0.992
_refine_ls_R_factor_all          0.0650
_refine_ls_R_factor_gt           0.0392
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0288P)^2^+0.00P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0716
_refine_ls_wR_factor_ref         0.0799
_reflns_number_gt                7859
_reflns_number_total             10116
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            b210458j.txt
_cod_data_source_block           d052
_cod_database_code               7012362