An ion pair scandium hydride supported by a dianionic (NNNN)-type macrocycle ligand
Peng Cui; Thomas P. Spaniol; Laurent Maron; Jun Okuda; Chem.Commun. 50 (2014) 424–; doi:10.1039/c3cc47805j

data_7110214
_publ_section_title
;
 An ion pair scandium hydride supported by a dianionic (NNNN)-type
 macrocycle ligand
;
_journal_name_full               Chem.Commun.
_journal_page_first              424
_journal_paper_doi               10.1039/c3cc47805j
_journal_volume                  50
_journal_year                    2014
_chemical_formula_moiety         '3(C30 H68 N12 Sc3), 3(C6 H5 S), 3(C4 H8 O)'
_chemical_formula_sum            'C120 H243 N36 O3 S3 Sc9'
_chemical_formula_weight         2739.32
_chemical_name_systematic
;
 ?
;
_space_group_IT_number           173
_symmetry_cell_setting           trigonal
_symmetry_space_group_name_Hall  'P 6c'
_symmetry_space_group_name_H-M   'P 63'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                120.00
_cell_formula_units_Z            2
_cell_length_a                   19.2442(17)
_cell_length_b                   19.2442(17)
_cell_length_c                   21.4089(19)
_cell_measurement_reflns_used    9856
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      26.46
_cell_measurement_theta_min      2.26
_cell_volume                     6866.3(11)
_computing_cell_refinement       'Bruker SAINT'
_computing_data_collection       'Bruker APEX'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    'ORTEP-III (Farrugia, 1999)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SIR-92 (Altomare 1992)'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device_type  'Bruker APEX-I CCD'
_diffrn_measurement_method       '\w scans'
_diffrn_radiation_monochromator  'multilayer optics'
_diffrn_radiation_source         microsource
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0599
_diffrn_reflns_av_sigmaI/netI    0.0529
_diffrn_reflns_limit_h_max       24
_diffrn_reflns_limit_h_min       -24
_diffrn_reflns_limit_k_max       24
_diffrn_reflns_limit_k_min       -24
_diffrn_reflns_limit_l_max       26
_diffrn_reflns_limit_l_min       -26
_diffrn_reflns_number            82918
_diffrn_reflns_theta_full        26.46
_diffrn_reflns_theta_max         26.46
_diffrn_reflns_theta_min         1.90
_exptl_absorpt_coefficient_mu    0.523
_exptl_absorpt_correction_T_max  0.8935
_exptl_absorpt_correction_T_min  0.8380
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'Sadabs Bruker'
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.325
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             2952
_exptl_crystal_size_max          0.35
_exptl_crystal_size_mid          0.25
_exptl_crystal_size_min          0.22
_refine_diff_density_max         1.901
_refine_diff_density_min         -0.633
_refine_diff_density_rms         0.095
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   0.13(4)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.041
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     492
_refine_ls_number_reflns         9437
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.041
_refine_ls_R_factor_all          0.0743
_refine_ls_R_factor_gt           0.0665
_refine_ls_shift/su_max          0.015
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.1071P)^2^+6.2341P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1758
_refine_ls_wR_factor_ref         0.1845
_reflns_number_gt                8291
_reflns_number_total             9437
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c3cc47805j.txt
_cod_data_source_block           4
_cod_database_code               7110214