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_7054852
_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         'C44 H84 I2 La2 Si8'
_chemical_formula_sum            'C44 H84 I2 La2 Si8'
_chemical_formula_weight         1369.45
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   geom
_audit_creation_date             2015-04-23
_audit_creation_method
;
Olex2 1.2
(compiled 2015.01.26 svn.r3150 for OlexSys, GUI svn.r4998)
;
_audit_update_record
;
2015-05-01 deposited with the CCDC.
2015-05-12 downloaded from the CCDC.
;
_cell_angle_alpha                72.517(19)
_cell_angle_beta                 83.217(15)
_cell_angle_gamma                79.146(17)
_cell_formula_units_Z            1
_cell_length_a                   10.7116(19)
_cell_length_b                   11.485(3)
_cell_length_c                   13.285(3)
_cell_measurement_reflns_used    1002
_cell_measurement_temperature    100.03(11)
_cell_measurement_theta_max      21.0550
_cell_measurement_theta_min      3.4910
_cell_volume                     1527.7(6)
_computing_cell_refinement
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.28 (release 01-02-2013 CrysAlis171 .NET)
(compiled Feb  1 2013,16:14:44)
;
_computing_data_collection
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.28 (release 01-02-2013 CrysAlis171 .NET)
(compiled Feb  1 2013,16:14:44)
;
_computing_data_reduction
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.28 (release 01-02-2013 CrysAlis171 .NET)
(compiled Feb  1 2013,16:14:44)
;
_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      100.03(11)
_diffrn_detector_area_resol_mean 8.0714
_diffrn_measured_fraction_theta_full 0.995
_diffrn_measured_fraction_theta_max 0.995
_diffrn_measurement_details
;
  1 omega  -65.00   53.50   1.5000   20.0000
omega____ theta____ kappa____ phi______ frames
    -      -25.5504   77.0000  150.0000 79

  2 omega  -65.00   53.50   1.5000   20.0000
omega____ theta____ kappa____ phi______ frames
    -      -25.5504   77.0000   30.0000 79

  3 omega  -14.00  104.50   1.5000   20.0000
omega____ theta____ kappa____ phi______ frames
    -       26.0192   77.0000  -90.0000 79
;
_diffrn_measurement_device_type  'SuperNova, Single source at offset, Eos'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_UB_11      -0.0607794000
_diffrn_orient_matrix_UB_12      0.0089501000
_diffrn_orient_matrix_UB_13      -0.0198587000
_diffrn_orient_matrix_UB_21      0.0003780000
_diffrn_orient_matrix_UB_22      -0.0648063000
_diffrn_orient_matrix_UB_23      0.0172618000
_diffrn_orient_matrix_UB_31      -0.0295197000
_diffrn_orient_matrix_UB_32      0.0049762000
_diffrn_orient_matrix_UB_33      0.0495440000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0751
_diffrn_reflns_av_unetI/netI     0.2067
_diffrn_reflns_laue_measured_fraction_full 0.995
_diffrn_reflns_laue_measured_fraction_max 0.995
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       8
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_number            7661
_diffrn_reflns_point_group_measured_fraction_full 0.995
_diffrn_reflns_point_group_measured_fraction_max 0.995
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         25.347
_diffrn_reflns_theta_min         3.222
_diffrn_source                   'SuperNova (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    2.572
_exptl_absorpt_correction_T_max  0.283
_exptl_absorpt_correction_T_min  0.093
_exptl_absorpt_correction_type   analytical
_exptl_absorpt_process_details
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.28 (release 01-02-2013 CrysAlis171 .NET)
(compiled Feb  1 2013,16:14:44)
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    1.489
_exptl_crystal_description       block
_exptl_crystal_F_000             680
_exptl_crystal_size_max          0.3836
_exptl_crystal_size_mid          0.2433
_exptl_crystal_size_min          0.1386
_refine_diff_density_max         2.610
_refine_diff_density_min         -1.617
_refine_diff_density_rms         0.240
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.060
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     265
_refine_ls_number_reflns         5556
_refine_ls_number_restraints     36
_refine_ls_restrained_S_all      1.060
_refine_ls_R_factor_all          0.1663
_refine_ls_R_factor_gt           0.0976
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0502P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1642
_refine_ls_wR_factor_ref         0.2255
_reflns_Friedel_coverage         0.000
_reflns_number_gt                2891
_reflns_number_total             5556
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c5nj00761e2.cif
_cod_data_source_block           2a
_cod_depositor_comments
'Adding full bibliography for 7054851--7054858.cif.'
_cod_database_code               7054852
_manchester_internal_coll_name   adpm14
_manchester_internal_coll_client AF/JF/DPM
_manchester_internal_coll_type   custom
_manchester_internal_coll_frame_time 1s
_manchester_internal_coll_frame_width 1
_manchester_internal_coll_frame_method '\w scans'
_manchester_internal_coll_user   AF
_manchester_internal_coll_date   10/02/2013
_manchester_internal_process_user AF
_manchester_internal_process_date 10/02/2013
_manchester_internal_solution_user FO
_manchester_internal_solution_date 18/03/2014
_manchester_internal_refinement_user FO
_manchester_internal_refinement_date 23/04/2015
_chemical_oxdiff_formula         C44H84I21La2Si8
_chemical_oxdiff_usercomment     'Fomblin film on micromount'
_reflns_odcompleteness_completeness 98.93
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     26.32
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Uiso/Uaniso restraints and constraints
C8 \\sim Si1 \\sim C6 \\sim C7: within 2A with sigma of 0.004 and sigma for
terminal atoms of 0.008
C21 \\sim Si4 \\sim C22 \\sim C20: within 2A with sigma of 0.004 and sigma for
terminal atoms of 0.008
3.a Aromatic/amide H refined with riding coordinates:
 C2(H2), C4(H4), C5(H5), C13(H13), C14(H14), C16(H16)
3.b 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)
;
_shelx_res_checksum              43944
_shelx_shelxl_version_number     2014/7
_olex2_submission_special_instructions 'No special instructions were received'