A structural investigation of heteroleptic lanthanide substituted cyclopentadienyl complexes
Ortu, Fabrizio; Fowler, Jonathan M.; Burton, Matthew; Formanuik, Alasdair; Mills, David P.; New J. Chem. 39 (2015) 7633–; doi:10.1039/C5NJ00761E

data_7054854
_publ_section_title
;
 A structural investigation of heteroleptic lanthanide substituted
 cyclopentadienyl complexes
;
_journal_issue                   10
_journal_name_full               'New J. Chem.'
_journal_page_first              7633
_journal_paper_doi               10.1039/C5NJ00761E
_journal_volume                  39
_journal_year                    2015
_chemical_formula_moiety         'C26 H50 I La O Si4'
_chemical_formula_sum            'C26 H50 I La O Si4'
_chemical_formula_weight         756.83
_space_group_crystal_system      orthorhombic
_space_group_IT_number           19
_space_group_name_Hall           'P 2ac 2ab'
_space_group_name_H-M_alt        'P 21 21 21'
_symmetry_space_group_name_Hall  'P 2ac 2ab'
_symmetry_space_group_name_H-M   'P 21 21 21'
_atom_sites_solution_hydrogens   geom
_audit_creation_date             2015-05-05
_audit_creation_method
;
Olex2 1.2
(compiled 2015.01.26 svn.r3150 for OlexSys, GUI svn.r4998)
;
_audit_update_record
;
2015-05-06 deposited with the CCDC.
2015-05-12 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   11.0319(4)
_cell_length_b                   16.0851(11)
_cell_length_c                   20.1692(7)
_cell_measurement_reflns_used    9466
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      26.8000
_cell_measurement_theta_min      3.0140
_cell_volume                     3579.0(3)
_computing_cell_refinement
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.28a (release 18-03-2013 CrysAlis171 .NET)
(compiled Mar 18 2013,11:47:30)
;
_computing_data_collection
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.28a (release 18-03-2013 CrysAlis171 .NET)
(compiled Mar 18 2013,11:47:30)
;
_computing_data_reduction
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.28a (release 18-03-2013 CrysAlis171 .NET)
(compiled Mar 18 2013,11:47:30)
;
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_computing_structure_solution    'ShelXS (Sheldrick, 2008)'
_diffrn_ambient_temperature      100(2)
_diffrn_detector_area_resol_mean 8.3367
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_details
;
  1 omega   35.00   79.00   1.0000   30.0000
omega____ theta____ kappa____ phi______ frames
    -      -21.2308  179.0000 -150.0000 44

  2 omega   77.00  104.00   1.0000   30.0000
omega____ theta____ kappa____ phi______ frames
    -       22.5590 -179.0000    0.0000 27

  3 omega  -17.00   69.00   1.0000   30.0000
omega____ theta____ kappa____ phi______ frames
    -       22.5590  -99.0000   30.0000 86

  4 omega   -7.00   76.00   1.0000   30.0000
omega____ theta____ kappa____ phi______ frames
    -       22.5590   37.0000  -90.0000 83

  5 omega   45.00  120.00   1.0000   30.0000
omega____ theta____ kappa____ phi______ frames
    -       22.5590 -179.0000  -90.0000 75

  6 omega  -61.00   46.00   1.0000   30.0000
omega____ theta____ kappa____ phi______ frames
    -       22.5590  -37.0000 -120.0000 107

  7 omega  -12.00  114.00   1.0000   30.0000
omega____ theta____ kappa____ phi______ frames
    -       22.5590   77.0000  120.0000 126
;
_diffrn_measurement_device_type  'Xcalibur, Sapphire2, large Be window'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_UB_11      0.0057267000
_diffrn_orient_matrix_UB_12      -0.0370716000
_diffrn_orient_matrix_UB_13      0.0188444000
_diffrn_orient_matrix_UB_21      -0.0569844000
_diffrn_orient_matrix_UB_22      0.0078804000
_diffrn_orient_matrix_UB_23      0.0149883000
_diffrn_orient_matrix_UB_31      -0.0291456000
_diffrn_orient_matrix_UB_32      -0.0226422000
_diffrn_orient_matrix_UB_33      -0.0256011000
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0694
_diffrn_reflns_av_unetI/netI     0.0604
_diffrn_reflns_laue_measured_fraction_full 0.998
_diffrn_reflns_laue_measured_fraction_max 0.998
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_limit_l_min       -24
_diffrn_reflns_number            30648
_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         25.348
_diffrn_reflns_theta_min         3.016
_diffrn_source                   'Enhance (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    2.205
_exptl_absorpt_correction_T_max  0.334
_exptl_absorpt_correction_T_min  0.059
_exptl_absorpt_correction_type   analytical
_exptl_absorpt_process_details
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.28a (release 18-03-2013 CrysAlis171 .NET)
(compiled Mar 18 2013,11:47:30)
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            'metallic light colourless'
_exptl_crystal_colour_lustre     metallic
_exptl_crystal_colour_modifier   light
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.405
_exptl_crystal_description       block
_exptl_crystal_F_000             1520
_exptl_crystal_size_max          0.4232
_exptl_crystal_size_mid          0.3496
_exptl_crystal_size_min          0.3496
_refine_diff_density_max         0.837
_refine_diff_density_min         -0.963
_refine_diff_density_rms         0.109
_refine_ls_abs_structure_details
;
 Flack x determined using 2341 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   0.003(12)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.097
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     360
_refine_ls_number_reflns         6552
_refine_ls_number_restraints     168
_refine_ls_restrained_S_all      1.105
_refine_ls_R_factor_all          0.0527
_refine_ls_R_factor_gt           0.0453
_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^)+11.3477P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0810
_refine_ls_wR_factor_ref         0.0846
_reflns_Friedel_coverage         0.784
_reflns_friedel_fraction_full    0.928
_reflns_friedel_fraction_max     1.000
_reflns_number_gt                5957
_reflns_number_total             6552
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c5nj00761e2.cif
_cod_data_source_block           2aTHF
_cod_depositor_comments
'Adding full bibliography for 7054851--7054858.cif.'
_cod_database_code               7054854
_manchester_internal_coll_name   odpm10
_manchester_internal_coll_client FO/DPM
_manchester_internal_coll_type   custom
_manchester_internal_coll_frame_time 30s
_manchester_internal_coll_frame_width 1
_manchester_internal_coll_frame_method '\w scans'
_manchester_internal_coll_user   FO
_manchester_internal_coll_date   04/03/2014
_manchester_internal_process_user FO
_manchester_internal_process_date 04/03/2014
_manchester_internal_solution_user FO
_manchester_internal_solution_date 04/03/2014
_manchester_internal_refinement_user FO
_manchester_internal_refinement_date 05/05/2015
_shelxl_version_number           2014/6
_chemical_oxdiff_formula         'C44 H84 La2 I2 Si4'
_reflns_odcompleteness_completeness 99.72
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     26.32
_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
 O1A-C26A \\sim O1A-C23A \\sim O1-C23 \\sim O1-C26
 with sigma of 0.02
 C26A-C25A \\sim C26-C25 \\sim C24-C23 \\sim C24A-C23A
 with sigma of 0.02
 C25A-C24A \\sim C25-C24
 with sigma of 0.02
 La1-I1A \\sim La1-I1
 with sigma of 0.02
3. Rigid bond restraints
 C26, C26A, C25, C25A, C24A, C24, C23, C23A
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.008
4. Uiso/Uaniso restraints and constraints
C26A \\sim C25A \\sim C23A \\sim C24 \\sim C25 \\sim C26 \\sim C24A \\sim C23:
within 2A with sigma of 0.004 and sigma for terminal atoms of 0.008
Si1 \\sim C7 \\sim C6 \\sim C8: within 2A with sigma of 0.005 and sigma for
terminal atoms of 0.01
C19 \\sim Si3 \\sim C18 \\sim C17: within 2A with sigma of 0.004 and sigma for
terminal atoms of 0.008
Uanis(I1A) = Uanis(I1)
5. Others
 Sof(O1A)=Sof(C26A)=Sof(H26C)=Sof(H26D)=Sof(C25A)=Sof(H25C)=Sof(H25D)=
 Sof(C24A)=Sof(H24C)=Sof(H24D)=Sof(C23A)=Sof(H23C)=Sof(H23D)=1-FVAR(1)
 Sof(O1)=Sof(C23)=Sof(H23A)=Sof(H23B)=Sof(C24)=Sof(H24A)=Sof(H24B)=Sof(C25)=
 Sof(H25A)=Sof(H25B)=Sof(C26)=Sof(H26A)=Sof(H26B)=FVAR(1)
 Sof(I1A)=1-FVAR(2)
 Sof(I1)=FVAR(2)
6.a Secondary CH2 refined with riding coordinates:
 C23(H23A,H23B), C24(H24A,H24B), C25(H25A,H25B), C26(H26A,H26B), C26A(H26C,
 H26D), C25A(H25C,H25D), C24A(H24C,H24D), C23A(H23C,H23D)
6.b Aromatic/amide H refined with riding coordinates:
 C2(H2), C4(H4), C5(H5), C13(H13), C15(H15), C16(H16)
6.c Idealised Me refined as rotating group:
 C6(H6A,H6B,H6C), C7(H7A,H7B,H7C), C8(H8A,H8B,H8C), C9(H9A,H9B,H9C), C10(H10A,
 H10B,H10C), C11(H11A,H11B,H11C), C17(H17A,H17B,H17C), C18(H18A,H18B,H18C),
 C19(H19A,H19B,H19C), C20(H20A,H20B,H20C), C21(H21A,H21B,H21C), C22(H22A,H22B,
 H22C)
;
_olex2_submission_special_instructions 'No special instructions were received'