Differences in the cyclometalation reactivity of bisphosphinimine-supported organo-rare earth complexes.
Zamora, Matthew T.; Johnson, Kevin R. D.; Hänninen, Mikko M; Hayes, Paul G.; Dalton transactions (Cambridge, England : 2003) 43 (2014) 10739–10750; doi:10.1039/c4dt00863d

data_7030938
_publ_section_title
;
 Differences in the cyclometalation reactivity of
 bisphosphinimine-supported organo-rare earth complexes.
;
_journal_issue                   28
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              10739
_journal_page_last               10750
_journal_paper_doi               10.1039/c4dt00863d
_journal_volume                  43
_journal_year                    2014
_chemical_formula_moiety         'C100 H100 N6 O2 P4 Sm2, 2(C6 H6)'
_chemical_formula_sum            'C112 H112 N6 O2 P4 Sm2'
_chemical_formula_weight         1998.65
_chemical_name_systematic
;
 ?
;
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2yn'
_space_group_name_H-M_alt        'P 1 21/n 1'
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 1'
_atom_sites_solution_hydrogens   geom
_audit_creation_date             2014-02-26
_audit_creation_method
;
Olex2 1.2
(compiled 2014.02.17 svn.r2891 for OlexSys, GUI svn.r4779)
;
_cell_angle_alpha                90
_cell_angle_beta                 109.2030(10)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   15.9755(13)
_cell_length_b                   17.8486(15)
_cell_length_c                   17.3855(14)
_cell_measurement_reflns_used    9210
_cell_measurement_temperature    173(2)
_cell_measurement_theta_max      27.51
_cell_measurement_theta_min      2.40
_cell_volume                     4681.5(7)
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2008)'
_diffrn_ambient_temperature      173.15
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0219
_diffrn_reflns_av_unetI/netI     0.0155
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_limit_h_max       19
_diffrn_reflns_limit_h_min       -19
_diffrn_reflns_limit_k_max       22
_diffrn_reflns_limit_k_min       -22
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            48294
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_theta_full        26.000
_diffrn_reflns_theta_max         25.999
_diffrn_reflns_theta_min         1.685
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    1.366
_exptl_absorpt_correction_T_max  0.864
_exptl_absorpt_correction_T_min  0.681
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
'SADABS-2012/1 (Bruker,2012) was used for absorption correction.'
_exptl_crystal_colour            yellow
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    1.418
_exptl_crystal_description       prism
_exptl_crystal_F_000             2052
_exptl_crystal_size_max          0.305
_exptl_crystal_size_mid          0.173
_exptl_crystal_size_min          0.11
_refine_diff_density_max         0.549
_refine_diff_density_min         -0.305
_refine_diff_density_rms         0.057
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.033
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     587
_refine_ls_number_reflns         9183
_refine_ls_number_restraints     48
_refine_ls_restrained_S_all      1.061
_refine_ls_R_factor_all          0.0244
_refine_ls_R_factor_gt           0.0199
_refine_ls_shift/su_max          0.005
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0212P)^2^+4.1613P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0473
_refine_ls_wR_factor_ref         0.0499
_reflns_Friedel_coverage         0.000
_reflns_number_gt                8272
_reflns_number_total             9183
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c4dt00863d1.cif
_cod_data_source_block           3_ph13002
_cod_depositor_comments
'Adding full bibliography for 7030936--7030940.cif.'
_cod_database_code               7030938
_shelxl_version_number           2013-4
_shelx_estimated_absorpt_t_max   0.864
_shelx_estimated_absorpt_t_min   0.681
_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
 C5S-C4S = C6S-C5S = C6S-C1S = C1S-C2S = C2S-C3S = C3S-C4S
 1.39 with sigma of 0.003
3. Uiso/Uaniso restraints and constraints
C1S \\sim C2S \\sim C3S \\sim C4S \\sim C5S \\sim C6S: within 1.7A with sigma
of 0.007 and sigma for terminal atoms of 0.01
Uanis(C17) \\sim Ueq: with sigma of 0.001 and sigma for terminal atoms of 0.002
4. Others
 Sof(C17B)=Sof(C18B)=Sof(H18B)=Sof(C19B)=Sof(H19B)=Sof(C20B)=Sof(C21B)=
 Sof(H21B)=Sof(C22B)=Sof(H22B)=Sof(C23B)=Sof(H23B)=Sof(C24B)=Sof(H24D)=
 Sof(H24E)=Sof(H24F)=Sof(C25B)=Sof(H25D)=Sof(H25E)=Sof(H25F)=1-FVAR(1)
 Sof(C17)=Sof(C18)=Sof(H18)=Sof(C19)=Sof(H19)=Sof(C20)=Sof(C21)=Sof(H21)=
 Sof(C22)=Sof(H22)=Sof(C23)=Sof(H23)=Sof(C24)=Sof(H24A)=Sof(H24B)=Sof(H24C)=
 Sof(C25)=Sof(H25A)=Sof(H25B)=Sof(H25C)=FVAR(1)
5.a Ternary CH refined with riding coordinates:
 C44(H44), C23(H23), C23B(H23B)
5.b Secondary CH2 refined with riding coordinates:
 C50(H50A,H50B), C48(H48A,H48B), C47(H47A,H47B), C49(H49A,H49B)
5.c Aromatic/amide H refined with riding coordinates:
 C18B(H18B), C19B(H19B), C21B(H21B), C22B(H22B), C18(H18), C19(H19), C21(H21),
 C22(H22), C16(H16), C12(H12), C13(H13), C6(H6), C14(H14), C10(H10), C7(H7),
 C8(H8), C9(H9), C15(H15), C3(H3), C2(H2), C37(H37), C33(H33), C34(H34),
 C31(H31), C28(H28), C30(H30), C29(H29), C35(H35), C36(H36), C43(H43), C40(H40),
  C42(H42), C1S(H1S), C2S(H2S), C5S(H5S), C6S(H6S), C4S(H4S), C3S(H3S)
5.d Fitted hexagon refined as free rotating group:
 C17B(C18B,C19B,C20B,C21B,C22B), C17(C18,C19,C20,C21,C22)
5.e Idealised Me refined as rotating group:
 C46(H46A,H46B,H46C), C45(H45A,H45B,H45C), C24(H24A,H24B,H24C), C25(H25A,H25B,
 H25C), C24B(H24D,H24E,H24F), C25B(H25D,H25E,H25F)
;