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_7012364
_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         'H14 N2 O14 Sc2 2+, (N O3 1-)2, C8 H16 O4'
_chemical_formula_sum            'C8 H30 N4 O24 Sc2'
_chemical_formula_weight         656.28
_chemical_name_systematic
; 
di(mu-hydroxo)bis((O,O'-nitrato)triaquascandium(III)) dinitrate
(1,4,7,10-tetraoxacyclododecane)
;
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_symmetry_Int_Tables_number      2
_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-97 + template + hand edit'
_cell_angle_alpha                85.497(7)
_cell_angle_beta                 84.869(8)
_cell_angle_gamma                69.545(15)
_cell_formula_units_Z            1
_cell_length_a                   7.5712(15)
_cell_length_b                   9.2350(15)
_cell_length_c                   9.862(3)
_cell_measurement_reflns_used    18452
_cell_measurement_temperature    120(2)
_cell_measurement_theta_max      27.48
_cell_measurement_theta_min      2.91
_cell_volume                     642.7(3)
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1997)'
_diffrn_ambient_temperature      120(2)
_diffrn_measured_fraction_theta_full 0.954
_diffrn_measured_fraction_theta_max 0.954
_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  0.0851
_diffrn_reflns_av_sigmaI/netI    0.0799
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_l_max       12
_diffrn_reflns_limit_l_min       -12
_diffrn_reflns_number            8198
_diffrn_reflns_theta_full        27.45
_diffrn_reflns_theta_max         27.45
_diffrn_reflns_theta_min         3.03
_exptl_absorpt_coefficient_mu    0.636
_exptl_absorpt_correction_T_max  0.9230
_exptl_absorpt_correction_T_min  0.8746
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
'SORTAV, R H Blessing, J. Appl. Cryst., 1997, 30, 421-426.'
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.696
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             340
_exptl_crystal_size_max          0.26
_exptl_crystal_size_mid          0.20
_exptl_crystal_size_min          0.10
_refine_diff_density_max         0.340
_refine_diff_density_min         -0.470
_refine_diff_density_rms         0.081
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.027
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     191
_refine_ls_number_reflns         2801
_refine_ls_number_restraints     6
_refine_ls_restrained_S_all      1.026
_refine_ls_R_factor_all          0.0691
_refine_ls_R_factor_gt           0.0411
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0323P)^2^+0.1240P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0877
_refine_ls_wR_factor_ref         0.0983
_reflns_number_gt                2053
_reflns_number_total             2801
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            b210458j.txt
_cod_data_source_block           d062
_cod_original_cell_volume        642.7(2)
_cod_database_code               7012364