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_7054858
_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 H65 Ce N2 Si7'
_chemical_formula_sum            'C26 H65 Ce N2 Si7'
_chemical_formula_weight         742.55
_space_group_crystal_system      monoclinic
_space_group_IT_number           15
_space_group_name_Hall           '-C 2yc'
_space_group_name_H-M_alt        'C 1 2/c 1'
_symmetry_space_group_name_Hall  '-C 2yc'
_symmetry_space_group_name_H-M   'C 1 2/c 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                90
_cell_angle_beta                 109.755(3)
_cell_angle_gamma                90
_cell_formula_units_Z            16
_cell_length_a                   38.4377(14)
_cell_length_b                   17.9044(5)
_cell_length_c                   25.5605(7)
_cell_measurement_reflns_used    10204
_cell_measurement_temperature    150.02(10)
_cell_measurement_theta_max      28.4350
_cell_measurement_theta_min      3.6580
_cell_volume                     16555.6(9)
_computing_cell_refinement
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.35 (release 13-08-2014 CrysAlis171 .NET)
(compiled Aug 13 2014,18:06:01)
;
_computing_data_collection
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.35 (release 13-08-2014 CrysAlis171 .NET)
(compiled Aug 13 2014,18:06:01)
;
_computing_data_reduction
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.35 (release 13-08-2014 CrysAlis171 .NET)
(compiled Aug 13 2014,18:06:01)
;
_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_environment      N~2~
_diffrn_ambient_temperature      150.02(10)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 8.0714
_diffrn_detector_type            Eos
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measurement_details
;
  1 omega  -77.00  -41.00   0.3000   25.0000
omega____ theta____ kappa____ phi______ frames
    -      -17.7663 -178.0000 -120.0000 120

  2 omega  -54.00   45.00   0.3000   25.0000
omega____ theta____ kappa____ phi______ frames
    -       18.8601  -37.0000  120.0000 330

  3 omega  -22.20   63.30   0.3000   25.0000
omega____ theta____ kappa____ phi______ frames
    -       18.8601  -19.0000 -180.0000 285
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'SuperNova, Single source at offset, Eos'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_UB_11      -0.0033026000
_diffrn_orient_matrix_UB_12      -0.0286957000
_diffrn_orient_matrix_UB_13      -0.0133298000
_diffrn_orient_matrix_UB_21      0.0262993500
_diffrn_orient_matrix_UB_22      0.0088208500
_diffrn_orient_matrix_UB_23      -0.0013753500
_diffrn_orient_matrix_UB_31      0.0126312500
_diffrn_orient_matrix_UB_32      -0.0258473500
_diffrn_orient_matrix_UB_33      0.0143491500
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.1159
_diffrn_reflns_av_unetI/netI     0.1352
_diffrn_reflns_laue_measured_fraction_full 0.997
_diffrn_reflns_laue_measured_fraction_max 0.997
_diffrn_reflns_limit_h_max       43
_diffrn_reflns_limit_h_min       -46
_diffrn_reflns_limit_k_max       21
_diffrn_reflns_limit_k_min       -21
_diffrn_reflns_limit_l_max       30
_diffrn_reflns_limit_l_min       -30
_diffrn_reflns_number            15128
_diffrn_reflns_point_group_measured_fraction_full 0.997
_diffrn_reflns_point_group_measured_fraction_max 0.997
_diffrn_reflns_theta_full        25.350
_diffrn_reflns_theta_max         25.350
_diffrn_reflns_theta_min         3.227
_diffrn_source                   'SuperNova (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    1.319
_exptl_absorpt_correction_T_max  0.991
_exptl_absorpt_correction_T_min  0.986
_exptl_absorpt_correction_type   gaussian
_exptl_absorpt_process_details
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.35 (release 13-08-2014 CrysAlis171 .NET)
(compiled Aug 13 2014,18:06:01)
Numerical absorption correction based on gaussian integration over
            a multifaceted crystal model
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            'clear dark red'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   dark
_exptl_crystal_colour_primary    red
_exptl_crystal_density_diffrn    1.192
_exptl_crystal_description       block
_exptl_crystal_F_000             6256
_exptl_crystal_size_max          0.2429
_exptl_crystal_size_mid          0.1477
_exptl_crystal_size_min          0.1329
_refine_diff_density_max         5.318
_refine_diff_density_min         -4.257
_refine_diff_density_rms         0.335
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.025
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     691
_refine_ls_number_reflns         15128
_refine_ls_number_restraints     88
_refine_ls_restrained_S_all      1.023
_refine_ls_R_factor_all          0.1311
_refine_ls_R_factor_gt           0.0957
_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^)+(0.1701P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2443
_refine_ls_wR_factor_ref         0.2851
_reflns_Friedel_coverage         0.000
_reflns_number_gt                9642
_reflns_number_total             15128
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c5nj00761e2.cif
_cod_data_source_block           6
_cod_depositor_comments
'Adding full bibliography for 7054851--7054858.cif.'
_cod_database_code               7054858
_manchester_internal_coll_name   adpm146
_manchester_internal_coll_client FO/DPM
_manchester_internal_coll_type   custom
_manchester_internal_coll_frame_time 25s
_manchester_internal_coll_frame_width 1
_manchester_internal_coll_frame_method '\w scans'
_manchester_internal_coll_user   FO
_manchester_internal_coll_date   05/03/2015
_manchester_internal_process_user FO
_manchester_internal_process_date 23/04/2015
_manchester_internal_solution_user FO
_manchester_internal_solution_date 23/04/2015
_manchester_internal_refinement_user FO
_manchester_internal_refinement_date 23/04/2015
_chemical_oxdiff_formula         'C48 N2 Si10 Ce'
_reflns_odcompleteness_completeness 99.59
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     26.32
_olex2_refinement_description
;
1. Twinned data refinement
 Scales: 0.861(5) 0.139(5)
2. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
 At 1.5 times of:
  All C(H,H,H) groups
3. Rigid bond restraints
 C27, C28, C29, C30, C31
 with sigma for 1-2 distances of 0.005 and sigma for 1-3 distances of 0.01
4. Uiso/Uaniso restraints and constraints
C27 \\sim C28 \\sim C29 \\sim C30 \\sim C31: within 2A with sigma of 0.005 and
sigma for terminal atoms of 0.01
Si10 \\sim C38 \\sim C39 \\sim C40: within 2A with sigma of 0.01 and sigma for
terminal atoms of 0.02
C1 \\sim C2 \\sim C3 \\sim C4 \\sim C5: within 2A with sigma of 0.005 and sigma
for terminal atoms of 0.1
5.a Me refined with riding coordinates:
 C9(H9A,H9B,H9C)
5.b Aromatic/amide H refined with riding coordinates:
 C3(H3), C5(H5), C29(H29), C31(H31)
5.c Idealised Me refined as rotating group:
 C6(H6A,H6B,H6C), C7(H7A,H7B,H7C), C8(H8A,H8B,H8C), C10(H10A,H10B,H10C),
 C11(H11A,H11B,H11C), C12(H12A,H12B,H12C), C13(H13A,H13B,H13C), C14(H14A,H14B,
 H14C), C15(H15A,H15B,H15C), C16(H16A,H16B,H16C), C17(H17A,H17B,H17C), C18(H18A,
 H18B,H18C), C19(H19A,H19B,H19C), C20(H20A,H20B,H20C), C21(H21A,H21B,H21C),
 C22(H22A,H22B,H22C), C23(H23A,H23B,H23C), C24(H24A,H24B,H24C), C25(H25A,H25B,
 H25C), C26(H26A,H26B,H26C), C32(H32A,H32B,H32C), C33(H33A,H33B,H33C), C34(H34A,
 H34B,H34C), C35(H35A,H35B,H35C), C36(H36A,H36B,H36C), C37(H37A,H37B,H37C),
 C38(H38A,H38B,H38C), C39(H39A,H39B,H39C), C40(H40A,H40B,H40C), C41(H41A,H41B,
 H41C), C42(H42A,H42B,H42C), C43(H43A,H43B,H43C), C44(H44A,H44B,H44C), C45(H45A,
 H45B,H45C), C46(H46A,H46B,H46C), C47(H47A,H47B,H47C), C48(H48A,H48B,H48C),
 C49(H49A,H49B,H49C), C50(H50A,H50B,H50C), C51(H51A,H51B,H51C), C52(H52A,H52B,
 H52C)
;
_shelx_res_checksum              83749
_shelx_shelxl_version_number     2014/7
_olex2_submission_special_instructions 'No special instructions were received'