Synthesis and Characterisation of Lanthanide N-Trimethylsilyl and -Mesityl Functionalised Bis(iminophosphorano)methanides and -Methanediides
Marshall, G.; Wooles, A.J.; Mills, D.P.; Lewis, W.; Blake, A.J.; Liddle, S.T.; Inorganics 1 (2013) 46–69; doi:10.3390/inorganics1010046

data_1556460
_publ_section_title
;
 Synthesis and Characterisation of Lanthanide N-Trimethylsilyl and
 -Mesityl Functionalised Bis(iminophosphorano)methanides and
 -Methanediides
;
_journal_name_full               Inorganics
_journal_page_first              46
_journal_page_last               69
_journal_paper_doi               10.3390/inorganics1010046
_journal_volume                  1
_journal_year                    2013
_chemical_formula_moiety         'C86 H85 La N4 P4, 3(C7 H8)'
_chemical_formula_sum            'C107 H109 La N4 P4'
_chemical_formula_weight         1713.77
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_symmetry_cell_setting           triclinic
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   'geom, Me from difmap'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_cell_angle_alpha                71.398(13)
_cell_angle_beta                 75.826(8)
_cell_angle_gamma                77.368(10)
_cell_formula_units_Z            2
_cell_length_a                   14.9196(11)
_cell_length_b                   15.179(3)
_cell_length_c                   21.622(2)
_cell_measurement_reflns_used    19004
_cell_measurement_temperature    90(2)
_cell_measurement_theta_max      74.54
_cell_measurement_theta_min      3.43
_cell_volume                     4446.6(11)
_computing_cell_refinement
;
CrysAlisPro, Oxford Diffraction Ltd.,
Version 1.171.34.36 (release 02-08-2010 CrysAlis171 .NET)
(compiled Nov  6 2009,16:24:50)
;
_computing_data_collection
;
CrysAlisPro, Oxford Diffraction Ltd.,
Version 1.171.34.36 (release 02-08-2010 CrysAlis171 .NET)
(compiled Nov  6 2009,16:24:50)
;
_computing_data_reduction
;
CrysAlisPro, Oxford Diffraction Ltd.,
Version 1.171.34.36 (release 02-08-2010 CrysAlis171 .NET)
(compiled Nov  6 2009,16:24:50)
;
_computing_molecular_graphics    'SHELXTL (Sheldrick, 2008)'
_computing_publication_material
'enCIFer(Allen et al.,2004);PLATON(Spek,2003)'
_computing_structure_refinement  'SHELXL97 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXTL (Sheldrick, 2008)'
_diffrn_ambient_temperature      90(2)
_diffrn_detector_area_resol_mean 10.3613
_diffrn_measured_fraction_theta_full 0.969
_diffrn_measured_fraction_theta_max 0.969
_diffrn_measurement_device_type  'SuperNova, Single source at offset), Atlas'
_diffrn_measurement_method       '\w scans'
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_source         'SuperNova (Cu) X-ray Source'
_diffrn_radiation_type           'Cu K\a'
_diffrn_radiation_wavelength     1.5418
_diffrn_reflns_av_R_equivalents  0.056
_diffrn_reflns_av_sigmaI/netI    0.065
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_h_min       -18
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       26
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            37469
_diffrn_reflns_theta_full        75.28
_diffrn_reflns_theta_max         75.28
_diffrn_reflns_theta_min         3.44
_diffrn_standards_decay_%        0
_diffrn_standards_interval_count .
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    4.777
_exptl_absorpt_correction_T_max  0.71
_exptl_absorpt_correction_T_min  0.29
_exptl_absorpt_correction_type   analytical
_exptl_absorpt_process_details
;
CrysAlisPro, Oxford Diffraction Ltd., 
Version 1.171.34.36 (release 02-08-2010 CrysAlis171 .NET) 
(compiled Jan  5 2010,16:28:46) 
Analytical numeric absorption correction using a multifaceted crystal 
model based on expressions derived by R.C. Clark & J.S. Reid. 
(Clark, R. C. & Reid, J. S. (1995). Acta Cryst. A51, 887-897) 
;
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.280
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             1792
_exptl_crystal_size_max          0.4571
_exptl_crystal_size_mid          0.2816
_exptl_crystal_size_min          0.0989
_refine_diff_density_max         1.89
_refine_diff_density_min         -1.58
_refine_diff_density_rms         0.11
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.06
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     972
_refine_ls_number_reflns         17807
_refine_ls_number_restraints     114
_refine_ls_restrained_S_all      1.06
_refine_ls_R_factor_all          0.0655
_refine_ls_R_factor_gt           0.0599
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.083P)^2^+8.838P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.153
_refine_ls_wR_factor_ref         0.157
_reflns_number_gt                15935
_reflns_number_total             17807
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            inorganics-01-00046-s001.cif
_cod_data_source_block           7a
_cod_original_cell_volume        4446.5(10)
_cod_database_code               1556460