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_1556454
_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         'C51 H59 Gd I2 N2 O2 P2, 3(C7 H8)'
_chemical_formula_sum            'C72 H83 Gd I2 N2 O2 P2'
_chemical_formula_weight         1481.39
_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                85.091(2)
_cell_angle_beta                 76.608(2)
_cell_angle_gamma                87.266(2)
_cell_formula_units_Z            2
_cell_length_a                   12.7851(6)
_cell_length_b                   15.1220(8)
_cell_length_c                   17.2635(9)
_cell_measurement_reflns_used    19750
_cell_measurement_temperature    90(2)
_cell_measurement_theta_max      27.39
_cell_measurement_theta_min      2.34
_cell_volume                     3233.7(3)
_computing_cell_refinement       'Bruker SAINT version 6.36A (Bruker, 2000)'
_computing_data_collection       'Bruker SMART version 5.625 (Bruker, 2001)'
_computing_data_reduction        'Bruker SAINT; SHELXTL (Sheldrick, 2008)'
_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 8.366
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.987
_diffrn_measurement_device_type  'Bruker SMART APEX CCD area detector'
_diffrn_measurement_method       \w
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.034
_diffrn_reflns_av_unetI/netI     0.036
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.987
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_number            40617
_diffrn_reflns_point_group_measured_fraction_full 0.997
_diffrn_reflns_point_group_measured_fraction_max 0.987
_diffrn_reflns_theta_full        25.000
_diffrn_reflns_theta_max         27.428
_diffrn_reflns_theta_min         1.887
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    2.076
_exptl_absorpt_correction_T_max  0.4305
_exptl_absorpt_correction_T_min  0.3505
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2007/2 (Bruker,2007) was used for absorption correction.
wR2(int) was 0.0615 before and 0.0445 after correction.
The Ratio of minimum to maximum transmission is 0.8142.
The \l/2 correction factor is 0.0015.
;
_exptl_crystal_colour            COLOURLESS
_exptl_crystal_density_diffrn    1.521
_exptl_crystal_description       BLOCK
_exptl_crystal_F_000             1490
_exptl_crystal_size_max          0.15
_exptl_crystal_size_mid          0.09
_exptl_crystal_size_min          0.09
_refine_diff_density_max         2.25
_refine_diff_density_min         -1.26
_refine_diff_density_rms         0.14
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.05
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     663
_refine_ls_number_reflns         14563
_refine_ls_number_restraints     45
_refine_ls_restrained_S_all      1.14
_refine_ls_R_factor_all          0.0475
_refine_ls_R_factor_gt           0.0419
_refine_ls_shift/su_max          0.003
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0646P)^2^+6.3799P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.109
_refine_ls_wR_factor_ref         0.114
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                12925
_reflns_number_total             14563
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            inorganics-01-00046-s001.cif
_cod_data_source_block           3
_cod_database_code               1556454
_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. Restrained distances
 C59-C60
 1.51 with sigma of 0.005
 C60-C65
 1.38 with sigma of 0.02
 C65-C64
 1.38 with sigma of 0.02
 C64-C63
 1.38 with sigma of 0.02
 C63-C62
 1.38 with sigma of 0.02
 C62-C61
 1.38 with sigma of 0.02
 C61-C60
 1.38 with sigma of 0.02
 C61-C59
 2.5 with sigma of 0.02
 C65-C59
 2.5 with sigma of 0.02
 C67-C68
 1.38 with sigma of 0.02
 C68-C69
 1.38 with sigma of 0.02
 C69-C70
 1.38 with sigma of 0.02
 C70-C71
 1.38 with sigma of 0.02
 C71-C72
 1.38 with sigma of 0.02
 C72-C67
 1.38 with sigma of 0.02
 C66-C67
 1.55 with sigma of 0.02
 C68-C66
 2.5 with sigma of 0.01
 C66-C72
 2.5 with sigma of 0.01
 C85-C86 = C86-C81 = C83-C81 = C84-C85
 1.38 with sigma of 0.02
 C82-C81
 1.55 with sigma of 0.02
 C80-C86
 2.5 with sigma of 0.02
 C80-C82
 2.5 with sigma of 0.02
 C80-C81
 1.55 with sigma of 0.02
 C83-C84
 1.38 with sigma of 0.02
 C82-C81
 1.38 with sigma of 0.02
 C82-C83
 1.38 with sigma of 0.02
3. Restrained planarity
 C59, C60, C65, C64, C63, C62, C61
 with sigma of 0.1
 C66, C67, C68, C69, C70, C71, C72
 with sigma of 0.1
 C66, C67, C68, C69, C70, C71, C72
 with sigma of 0.1
 C81, C86, C85, C84, C83, C82, C80
 with sigma of 0.1
4. Others
 Sof(C80)=Sof(H80A)=Sof(H80B)=Sof(H80C)=Sof(C81)=Sof(C86)=Sof(H86)=Sof(C85)=
 Sof(H85)=Sof(C84)=Sof(H84)=Sof(C83)=Sof(H83)=Sof(C82)=Sof(H82)=1-FVAR(1)
 Sof(C59)=Sof(H59A)=Sof(H59B)=Sof(H59C)=Sof(C60)=Sof(C65)=Sof(H65)=Sof(C64)=
 Sof(H64)=Sof(C63)=Sof(H63)=Sof(C62)=Sof(H62)=Sof(C61)=Sof(H61)=FVAR(1)
5.a Ternary CH refined with riding coordinates:
 C1(H1)
5.b Secondary CH2 refined with riding coordinates:
 C44(H44A,H44B), C45(H45A,H45B), C46(H46A,H46B), C47(H47A,H47B), C48(H48A,
 H48B), C49(H49A,H49B), C50(H50A,H50B), C51(H51A,H51B)
5.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),
 C54(H54), C55(H55), C56(H56), C57(H57), C58(H58), C65(H65), C64(H64), C63(H63),
  C62(H62), C61(H61), C68(H68), C69(H69), C70(H70), C71(H71), C72(H72),
 C86(H86), C85(H85), C84(H84), C83(H83), C82(H82)
5.d Fitted hexagon refined as free rotating group:
 C60(C65,C64,C63,C62,C61), C67(C68,C69,C70,C71,C72), C81(C86,C85,C84,C83,C82)
5.e 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), C52(H52A,H52B,H52C), C59(H59A,
 H59B,H59C), C66(H66A,H66B,H66C), C80(H80A,H80B,H80C)
;
_shelxl_version_number           2013-4