Simple entry into N-tert-butyl-iminophosphonamide rare-earth metal alkyl and chlorido complexes.
Rufanov, Konstantin A.; Pruß, Noa K; Sundermeyer, Jörg; Dalton transactions (Cambridge, England : 2003) 45 (2016) 1525–1538; doi:10.1039/c5dt03721b

data_7037453
_publ_section_title
;
 Simple entry into N-tert-butyl-iminophosphonamide rare-earth metal alkyl
 and chlorido complexes.
;
_journal_issue                   4
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              1525
_journal_page_last               1538
_journal_paper_doi               10.1039/c5dt03721b
_journal_volume                  45
_journal_year                    2016
_chemical_formula_moiety         'C60 H84 Cl4 N6 O P3 Sc3, 3(C6 D6)'
_chemical_formula_sum            'C78 H84 Cl4 D18 N6 O P3 Sc3'
_chemical_formula_weight         1527.35
_chemical_name_systematic
;

tris-((tert-butyl(N-(tert-butyl)-P,P-diphenylphosphorimidoyl)amino)-(mu2-chlorido)scandium)mu3-oxo-mu3-chloride

;
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   geom
_audit_creation_method           SHELXL-2014/7
_audit_update_record
;
2015-11-13 deposited with the CCDC.
2015-11-24 downloaded from the CCDC.
;
_cell_angle_alpha                80.619(3)
_cell_angle_beta                 79.875(3)
_cell_angle_gamma                70.044(3)
_cell_formula_units_Z            2
_cell_length_a                   12.8438(4)
_cell_length_b                   14.0230(5)
_cell_length_c                   24.5137(8)
_cell_measurement_reflns_used    24108
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      27.195
_cell_measurement_theta_min      1.555
_cell_volume                     4060.0(2)
_computing_cell_refinement       'STOE WinCell (X-Area)'
_computing_data_collection       'STOE WinXpose (X-Area)'
_computing_data_reduction        'STOE WinIntegrate (X-Area)'
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_structure_solution    'Sir-97 (Giacovazzo et al., 1997)'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measurement_device_type  'Stoe IPDS2'
_diffrn_measurement_method       \w
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71069
_diffrn_reflns_av_R_equivalents  0.0780
_diffrn_reflns_av_unetI/netI     0.1122
_diffrn_reflns_laue_measured_fraction_full 1.000
_diffrn_reflns_laue_measured_fraction_max 0.997
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       30
_diffrn_reflns_limit_l_min       -30
_diffrn_reflns_number            59927
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.997
_diffrn_reflns_theta_full        25.240
_diffrn_reflns_theta_max         26.732
_diffrn_reflns_theta_min         1.554
_exptl_absorpt_coefficient_mu    0.479
_exptl_absorpt_correction_T_max  0.9762
_exptl_absorpt_correction_T_min  0.8798
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
'R.H. Blessing, Acta cryst. (1995), A51, 33-38'
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.249
_exptl_crystal_description       plate
_exptl_crystal_F_000             1592
_exptl_crystal_size_max          0.320
_exptl_crystal_size_mid          0.200
_exptl_crystal_size_min          0.160
_exptl_transmission_factor_max   0.9272
_exptl_transmission_factor_min   0.8617
_refine_diff_density_max         1.321
_refine_diff_density_min         -0.820
_refine_diff_density_rms         0.079
_refine_ls_extinction_coef       0.0020(3)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     'SHELXL-2014/7 (Sheldrick 2014'
_refine_ls_goodness_of_fit_ref   0.808
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     875
_refine_ls_number_reflns         17184
_refine_ls_number_restraints     84
_refine_ls_restrained_S_all      0.817
_refine_ls_R_factor_all          0.1070
_refine_ls_R_factor_gt           0.0605
_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^)+(0.0895P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1432
_refine_ls_wR_factor_ref         0.1557
_reflns_Friedel_coverage         0.000
_reflns_number_gt                8772
_reflns_number_total             17184
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c5dt03721b1.cif
_cod_data_source_block           a
_cod_depositor_comments
'Adding full bibliography for 7037450--7037455.cif.'
_cod_database_code               7037453
_shelx_shelxl_version_number     2014/7
_shelx_estimated_absorpt_t_min   0.862
_shelx_estimated_absorpt_t_max   0.927
_shelx_res_checksum              97631
_shelx_hkl_checksum              33294