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_1556458
_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         'C49 H59 I2 La N4 P2, 3(C7 H8)'
_chemical_formula_sum            'C70 H83 I2 La N4 P2'
_chemical_formula_weight         1435.05
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_atom_sites_solution_hydrogens   'geom, Me from difmap'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_cell_angle_alpha                82.761(6)
_cell_angle_beta                 74.997(7)
_cell_angle_gamma                87.043(7)
_cell_formula_units_Z            2
_cell_length_a                   13.0112(11)
_cell_length_b                   15.2310(11)
_cell_length_c                   17.0292(12)
_cell_measurement_reflns_used    8937
_cell_measurement_temperature    90(2)
_cell_measurement_theta_max      75.3947
_cell_measurement_theta_min      3.5146
_cell_volume                     3233.1(4)
_computing_cell_refinement
;
CrysAlisPro, Agilent Technologies,
Version 1.171.35.19 (release 27-10-2011 CrysAlis171 .NET)
(compiled Oct 27 2011,15:02:11)
;
_computing_data_collection
;
CrysAlisPro, Agilent Technologies,
Version 1.171.35.19 (release 27-10-2011 CrysAlis171 .NET)
(compiled Oct 27 2011,15:02:11)
;
_computing_data_reduction
;
CrysAlisPro, Agilent Technologies,
Version 1.171.35.19 (release 27-10-2011 CrysAlis171 .NET)
(compiled Oct 27 2011,15:02:11)
;
_computing_molecular_graphics
;
O. V. Dolomanov, L. J. Bourhis, R. J. Gildea, J. A. K. Howard and H. Puschmann,
OLEX2: a complete structure solution, refinement and analysis program.
J. Appl. Cryst. (2009). 42, 339-341.
;
_computing_publication_material
;
O. V. Dolomanov, L. J. Bourhis, R. J. Gildea, J. A. K. Howard and H. Puschmann,
OLEX2: a complete structure solution, refinement and analysis program.
J. Appl. Cryst. (2009). 42, 339-341.
;
_computing_structure_refinement
;
SHELXL, G.M. Sheldrick, Acta Cryst.
(2008). A64, 112-122
;
_diffrn_ambient_temperature      90(2)
_diffrn_detector_area_resol_mean 10.3613
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.958
_diffrn_measurement_details
;
  1 omega  -69.00   25.00   1.0000   12.0000
omega____ theta____ kappa____ phi______ frames
    -      -43.7877   57.0000  -90.0000 94

  2 omega -112.00  -20.00   1.0000   12.0000
omega____ theta____ kappa____ phi______ frames
    -      -43.7877  -57.0000  120.0000 92

  3 omega   38.00   73.00   1.0000   12.0000
omega____ theta____ kappa____ phi______ frames
    -       43.7877  -77.0000    0.0000 35

  4 omega  -19.00   57.00   1.0000   12.0000
omega____ theta____ kappa____ phi______ frames
    -       43.7877  -57.0000  -30.0000 76

  5 omega   23.00   63.00   1.0000   12.0000
omega____ theta____ kappa____ phi______ frames
    -       43.7877  -38.0000 -150.0000 40

  6 omega   43.00   91.00   1.0000   48.0000
omega____ theta____ kappa____ phi______ frames
    -      105.8472  -95.0000  -30.0000 48

  7 omega   33.00   63.00   1.0000   48.0000
omega____ theta____ kappa____ phi______ frames
    -      105.8472  -30.0000   60.0000 30

  8 omega   33.00   69.00   1.0000   48.0000
omega____ theta____ kappa____ phi______ frames
    -      105.8472  -30.0000 -120.0000 36

  9 omega   83.00  133.00   1.0000   48.0000
omega____ theta____ kappa____ phi______ frames
    -      105.8472   15.0000 -180.0000 50

 10 omega   44.00   69.00   1.0000   48.0000
omega____ theta____ kappa____ phi______ frames
    -      105.8472  -45.0000  -60.0000 25

 11 omega   43.00  110.00   1.0000   48.0000
omega____ theta____ kappa____ phi______ frames
    -      105.8472  -95.0000  120.0000 67

 12 omega   33.00   69.00   1.0000   48.0000
omega____ theta____ kappa____ phi______ frames
    -      105.8472  -30.0000  150.0000 36

 13 omega   34.00   66.00   1.0000   48.0000
omega____ theta____ kappa____ phi______ frames
    -      105.8472  -30.0000  -90.0000 32

 14 omega   37.00   76.00   1.0000   48.0000
omega____ theta____ kappa____ phi______ frames
    -      105.8472  -45.0000   30.0000 39

 15 omega   36.00   65.00   1.0000   48.0000
omega____ theta____ kappa____ phi______ frames
    -      105.8472  -45.0000 -120.0000 29

 16 omega   39.00   71.00   1.0000   48.0000
omega____ theta____ kappa____ phi______ frames
    -      105.8472  -45.0000 -150.0000 32

 17 omega   38.00   66.00   1.0000   48.0000
omega____ theta____ kappa____ phi______ frames
    -      105.8472  -30.0000  120.0000 28

 18 omega   35.00   61.00   1.0000   48.0000
omega____ theta____ kappa____ phi______ frames
    -      105.8472  -30.0000 -180.0000 26

 19 omega   47.00   74.00   1.0000   48.0000
omega____ theta____ kappa____ phi______ frames
    -      105.8472  -45.0000   90.0000 27

 20 omega   55.00  118.00   1.0000   48.0000
omega____ theta____ kappa____ phi______ frames
    -      105.8472 -125.0000 -120.0000 63

 21 omega   30.00  108.00   1.0000   48.0000
omega____ theta____ kappa____ phi______ frames
    -      105.8472  -95.0000   60.0000 78

 22 omega   62.00  117.00   1.0000   48.0000
omega____ theta____ kappa____ phi______ frames
    -      105.8472 -125.0000   60.0000 55

 23 omega   65.00  112.00   1.0000   48.0000
omega____ theta____ kappa____ phi______ frames
    -      105.8472 -125.0000  -30.0000 47

 24 omega   77.00  104.00   1.0000   48.0000
omega____ theta____ kappa____ phi______ frames
    -      105.8472   77.0000  150.0000 27

 25 omega   27.00  146.00   1.0000   48.0000
omega____ theta____ kappa____ phi______ frames
    -      105.8472  -15.0000  -60.0000 119

 26 omega   86.00  113.00   1.0000   48.0000
omega____ theta____ kappa____ phi______ frames
    -      105.8472   45.0000   30.0000 27

 27 omega   45.00   90.00   1.0000   48.0000
omega____ theta____ kappa____ phi______ frames
    -      105.8472  -95.0000 -120.0000 45
;
_diffrn_measurement_device_type  'SuperNova, Single source at offset), Atlas'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_UB_11      0.0706931000
_diffrn_orient_matrix_UB_12      -0.0547140000
_diffrn_orient_matrix_UB_13      -0.0644338000
_diffrn_orient_matrix_UB_21      -0.1001704000
_diffrn_orient_matrix_UB_22      -0.0356403000
_diffrn_orient_matrix_UB_23      -0.0164998000
_diffrn_orient_matrix_UB_31      0.0006437000
_diffrn_orient_matrix_UB_32      0.0783322000
_diffrn_orient_matrix_UB_33      -0.0668527000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_type           'Cu K\a'
_diffrn_radiation_wavelength     1.5418
_diffrn_reflns_av_R_equivalents  0.058
_diffrn_reflns_av_unetI/netI     0.060
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.958
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            25965
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.958
_diffrn_reflns_theta_full        67.500
_diffrn_reflns_theta_max         75.578
_diffrn_reflns_theta_min         3.518
_diffrn_source                   'SuperNova (Cu) X-ray Source'
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    13.393
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.18860
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro, Agilent Technologies,
Version 1.171.35.19 (release 27-10-2011 CrysAlis171 .NET)
(compiled Oct 27 2011,15:02:11)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            colourless
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.474
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       column
_exptl_crystal_F_000             1448
_exptl_crystal_size_max          0.3133
_exptl_crystal_size_mid          0.1578
_exptl_crystal_size_min          0.0865
_refine_diff_density_max         2.65
_refine_diff_density_min         -1.94
_refine_diff_density_rms         0.19
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.04
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     725
_refine_ls_number_reflns         12864
_refine_ls_number_restraints     6
_refine_ls_restrained_S_all      1.04
_refine_ls_R_factor_all          0.067
_refine_ls_R_factor_gt           0.058
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.118P)^2^+0.092P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.153
_refine_ls_wR_factor_ref         0.164
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                10928
_reflns_number_total             12864
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            inorganics-01-00046-s001.cif
_cod_data_source_block           6a
_cod_database_code               1556458
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Uiso/Uaniso restraints and constraints
Uanis(C64) \\sim Ueq: with sigma of 0.005 and sigma for terminal atoms of 0.01
3.a Ternary CH refined with riding coordinates:
 C1(H1)
3.b Secondary CH2 refined with riding coordinates:
 C46(H46A,H46B), C47(H47A,H47B)
3.c Aromatic/amide H refined with riding coordinates:
 C3(H3), C4(H4), C5(H5), C6(H6), C7(H7), C9(H9), C10(H10), C11(H11), C12(H12),
 C13(H13), C15(H15), C16(H16), C17(H17), C18(H18), C19(H19), C21(H21), C22(H22),
  C23(H23), C24(H24), C25(H25), C28(H28), C30(H30), C37(H37), C39(H39),
 C52(H52), C53(H53), C54(H54), C55(H55), C56(H56), C59(H59), C60(H60), C61(H61),
  C62(H62), C63(H63), C66(H66), C67(H67), C68(H68), C69(H69), C70(H70)
3.d Idealised Me refined as rotating group:
 C32(H32A,H32B,H32C), C33(H33A,H33B,H33C), C34(H34A,H34B,H34C), C41(H41A,H41B,
 H41C), C42(H42A,H42B,H42C), C43(H43A,H43B,H43C), C44(H44A,H44B,H44C), C45(H45A,
 H45B,H45C), C48(H48A,H48B,H48C), C49(H49A,H49B,H49C), C50(H50A,H50B,H50C),
 C57(H57A,H57B,H57C), C64(H64A,H64B,H64C)
;
_shelxl_version_number           2013-4