Synthesis of a homoleptic Sm(ii) bis(phosphinimino)methanide
Hill, Michael S.; Hitchcock, Peter B.; Dalton Transactions  (2003) 4570–; doi:10.1039/b313034g

data_7013715
_publ_section_title
;
 Synthesis of a homoleptic Sm(ii) bis(phosphinimino)methanide
;
_journal_issue                   24
_journal_name_full               'Dalton Transactions'
_journal_page_first              4570
_journal_paper_doi               10.1039/b313034g
_journal_year                    2003
_chemical_compound_source        'synthesis as described'
_chemical_formula_moiety         '(C86 H86 N4 P4 Sm1) 2.5(C7 H8)'
_chemical_formula_sum            'C103.5 H106 N4 P4 Sm'
_chemical_formula_weight         1680.15
_chemical_name_common            '(Sm(MesNPPh2CHPPh2NMes)) 2.5(toluene)'
_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_conform_dict_location     ftp://ftp.iucr.org/pub/cif_core.dic
_audit_conform_dict_name         cif_core.dic
_audit_conform_dict_version      2.2
_audit_creation_date             2003-04-09T09:36:42-00:00
_audit_creation_method           'WinGX routine CIF_UPDATE'
_cell_angle_alpha                68.814(1)
_cell_angle_beta                 75.887(1)
_cell_angle_gamma                75.659(1)
_cell_formula_units_Z            2
_cell_length_a                   15.1670(1)
_cell_length_b                   15.8289(2)
_cell_length_c                   22.0330(3)
_cell_measurement_reflns_used    77755
_cell_measurement_temperature    173(2)
_cell_measurement_theta_max      27.485
_cell_measurement_theta_min      3.705
_cell_measurement_wavelength     0.71073
_cell_volume                     4708.17(10)
_computing_cell_refinement       'HKL Scalepack (Otwinowski & Minor 1997)'
_computing_data_collection       'Collect (Nonius BV, 1997-2000)'
_computing_data_reduction
'HKL Denzo and Scalepack (Otwinowski & Minor 1997)'
_computing_molecular_graphics    'Ortep-3 for Windows (Farrugia, 1997)'
_computing_publication_material  'WinGX publication routines (Farrugia, 1999)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1997)'
_diffrn_ambient_temperature      173(2)
_diffrn_detector                 'CCD plate'
_diffrn_measured_fraction_theta_full 0.986
_diffrn_measured_fraction_theta_max 0.986
_diffrn_measurement_device       '95mm CCD camera on \k-goniostat'
_diffrn_measurement_device_type  KappaCCD
_diffrn_measurement_method       'CCD rotation images, thick slices'
_diffrn_orient_matrix_type       'by Nonius Collect from scalepack cell'
_diffrn_orient_matrix_UB_11      0.465947E-1
_diffrn_orient_matrix_UB_12      0.285717E-1
_diffrn_orient_matrix_UB_13      -0.379524E-1
_diffrn_orient_matrix_UB_21      -0.174043E-1
_diffrn_orient_matrix_UB_22      0.577064E-1
_diffrn_orient_matrix_UB_23      0.122122E-1
_diffrn_orient_matrix_UB_31      0.479215E-1
_diffrn_orient_matrix_UB_32      -0.243298E-1
_diffrn_orient_matrix_UB_33      0.291737E-1
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0735
_diffrn_reflns_av_unetI/netI     0.0667
_diffrn_reflns_limit_h_max       19
_diffrn_reflns_limit_h_min       -19
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       28
_diffrn_reflns_limit_l_min       -27
_diffrn_reflns_number            61602
_diffrn_reflns_theta_full        27.49
_diffrn_reflns_theta_max         27.49
_diffrn_reflns_theta_min         3.71
_diffrn_source                   'Enraf Nonius FR590'
_exptl_absorpt_coefficient_mu    0.738
_exptl_absorpt_correction_T_max  0.9939
_exptl_absorpt_correction_T_min  0.8223
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
[c.f. r.h. blessing, acta cryst. (1995), a51, 33-38]
;
_exptl_crystal_colour            black
_exptl_crystal_density_diffrn    1.185
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             1754
_exptl_crystal_size_max          0.3
_exptl_crystal_size_mid          0.2
_exptl_crystal_size_min          0.05
_refine_diff_density_max         1.928
_refine_diff_density_min         -1.191
_refine_diff_density_rms         0.108
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.067
_refine_ls_hydrogen_treatment    riding
_refine_ls_matrix_type           full
_refine_ls_number_parameters     952
_refine_ls_number_reflns         21366
_refine_ls_number_restraints     231
_refine_ls_restrained_S_all      1.12
_refine_ls_R_factor_all          0.0866
_refine_ls_R_factor_gt           0.0635
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0824P)^2^+9.1638P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1609
_refine_ls_wR_factor_ref         0.1749
_reflns_number_gt                16861
_reflns_number_total             21366
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            b313034g.txt
_cod_data_source_block           apr803
_cod_original_cell_volume        4708.17(9)
_cod_original_sg_symbol_H-M      P-1
_cod_database_code               7013715