Rare Neutral Diphosphine Complexes of Scandium(III) and Yttrium(III) Halides.
Carravetta, Marina; Concistre, Maria; Levason, William; Reid, Gillian; Zhang, Wenjian; Inorganic chemistry 55 (2016) 12890–12896; doi:10.1021/acs.inorgchem.6b02268

data_4349280
_publ_section_title
;
 Rare Neutral Diphosphine Complexes of Scandium(III) and Yttrium(III)
 Halides.
;
_journal_issue                   24
_journal_name_full               'Inorganic chemistry'
_journal_page_first              12890
_journal_page_last               12896
_journal_paper_doi               10.1021/acs.inorgchem.6b02268
_journal_volume                  55
_journal_year                    2016
_chemical_formula_sum            'C20 H32 I3 P4 Sc'
_chemical_formula_weight         822.00
_space_group_IT_number           96
_space_group_name_Hall           'P 4nw 2abw'
_space_group_name_H-M_alt        'P 43 21 2'
_symmetry_cell_setting           tetragonal
_symmetry_space_group_name_Hall  'P 4nw 2abw'
_symmetry_space_group_name_H-M   'P 43 21 2'
_atom_sites_solution_hydrogens   geom
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_cell_angle_beta                 90.00
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   8.8820(10)
_cell_length_b                   8.8820(10)
_cell_length_c                   35.4690(10)
_cell_measurement_reflns_used    13120
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      31.715
_cell_measurement_theta_min      2.279
_cell_volume                     2798.1(5)
_computing_cell_refinement       'CrysAlisPro 1.171.38.41 (Rigaku OD, 2015)'
_computing_data_collection
;
CrystalClear-SM Expert 2.0 r7 (Rigaku, 2011)
;
_computing_data_reduction        'CrysAlisPro 1.171.38.41 (Rigaku OD, 2015)'
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_computing_publication_material
'PLATON (Spek, 2003), WinGX (Farrugia, 1999) and enCIFer (Allen et al., 2004).'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1997)'
_diffrn_ambient_temperature      100(2)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 28.5714
_diffrn_detector_type            'Rigaku HG Saturn724+ (2x2 bin mode)'
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 1.000
_diffrn_measurement_device       'four-circle \k diffractometer'
_diffrn_measurement_device_type  'Rigaku AFC12 (Right)'
_diffrn_measurement_method       'profile data from \w-scans'
_diffrn_measurement_specimen_support 'MiTeGen micromount'
_diffrn_radiation_collimation    'Confocal mirrors, VHF Varimax '
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71075
_diffrn_reflns_av_R_equivalents  0.0484
_diffrn_reflns_av_sigmaI/netI    0.0238
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_diffrn_reflns_limit_l_max       43
_diffrn_reflns_limit_l_min       -43
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_diffrn_reflns_theta_max         26.00
_diffrn_reflns_theta_min         2.30
_diffrn_source                   'Rotating Anode'
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_diffrn_source_power             2.475
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_exptl_absorpt_correction_T_min  0.83558
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_exptl_absorpt_process_details
;
CrysAlisPro 1.171.38.41 (Rigaku Oxford Diffraction, 2015)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.951
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       fragment
_exptl_crystal_F_000             1568
_exptl_crystal_size_max          0.03
_exptl_crystal_size_mid          0.03
_exptl_crystal_size_min          0.02
_refine_diff_density_max         0.733
_refine_diff_density_min         -0.425
_refine_diff_density_rms         0.096
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   0.00(3)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.156
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     132
_refine_ls_number_reflns         2743
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.156
_refine_ls_R_factor_all          0.0278
_refine_ls_R_factor_gt           0.0258
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0263P)^2^+2.9260P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0575
_refine_ls_wR_factor_ref         0.0581
_reflns_number_gt                2632
_reflns_number_total             2743
_reflns_threshold_expression     >2\s(I)
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_cod_data_source_block           16r413a_[ScI3{o-C6H4(PMe2)2}2]
_cod_database_code               4349280