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_7054855
_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         'C52 H84 Ce2 I2'
_chemical_formula_sum            'C52 H84 Ce2 I2'
_chemical_formula_weight         1243.23
_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             2015-04-27
_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                90.523(3)
_cell_angle_beta                 98.515(3)
_cell_angle_gamma                104.372(3)
_cell_formula_units_Z            2
_cell_length_a                   10.5085(5)
_cell_length_b                   11.3227(4)
_cell_length_c                   23.7712(8)
_cell_measurement_reflns_used    6965
_cell_measurement_temperature    150.01(10)
_cell_measurement_theta_max      28.3030
_cell_measurement_theta_min      3.6910
_cell_volume                     2706.58(19)
_computing_cell_refinement
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.32 (release 02-08-2013 CrysAlis171 .NET)
(compiled Aug  2 2013,16:46:58)
;
_computing_data_collection
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.32 (release 02-08-2013 CrysAlis171 .NET)
(compiled Aug  2 2013,16:46:58)
;
_computing_data_reduction
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.32 (release 02-08-2013 CrysAlis171 .NET)
(compiled Aug  2 2013,16:46:58)
;
_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      150.01(10)
_diffrn_detector_area_resol_mean 8.0714
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measurement_details
;
  1 omega  -26.00    3.00   1.0000    1.0400
omega____ theta____ kappa____ phi______ frames
    -      -22.9725  -57.0000   90.0000 29

  2 omega   -5.00   26.00   1.0000    1.0400
omega____ theta____ kappa____ phi______ frames
    -      -22.9725  -99.0000   60.0000 31

  3 omega  -85.00  -40.00   1.0000    1.0400
omega____ theta____ kappa____ phi______ frames
    -      -22.9725  -57.0000   90.0000 45

  4 omega -102.00   51.00   1.0000    1.0400
omega____ theta____ kappa____ phi______ frames
    -      -22.9725  -19.0000  120.0000 153

  5 omega -101.00  -43.00   1.0000    1.0400
omega____ theta____ kappa____ phi______ frames
    -      -22.9725 -178.0000  -60.0000 58

  6 omega -107.00  -72.00   1.0000    1.0400
omega____ theta____ kappa____ phi______ frames
    -      -22.9725 -178.0000  120.0000 35

  7 omega   41.00  109.00   1.0000    1.0400
omega____ theta____ kappa____ phi______ frames
    -       24.0662  178.0000   60.0000 68

  8 omega   39.00   64.00   1.0000    1.0400
omega____ theta____ kappa____ phi______ frames
    -       24.0662  178.0000   30.0000 25
;
_diffrn_measurement_device_type  'SuperNova, Single source at offset, Eos'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_UB_11      -0.0660687000
_diffrn_orient_matrix_UB_12      -0.0029289000
_diffrn_orient_matrix_UB_13      -0.0129626000
_diffrn_orient_matrix_UB_21      -0.0238799000
_diffrn_orient_matrix_UB_22      -0.0507241000
_diffrn_orient_matrix_UB_23      0.0162428000
_diffrn_orient_matrix_UB_31      -0.0062910000
_diffrn_orient_matrix_UB_32      0.0401250000
_diffrn_orient_matrix_UB_33      0.0219211000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0409
_diffrn_reflns_av_unetI/netI     0.0682
_diffrn_reflns_laue_measured_fraction_full 0.997
_diffrn_reflns_laue_measured_fraction_max 0.997
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       27
_diffrn_reflns_limit_l_min       -28
_diffrn_reflns_number            17833
_diffrn_reflns_point_group_measured_fraction_full 0.997
_diffrn_reflns_point_group_measured_fraction_max 0.997
_diffrn_reflns_theta_full        26.000
_diffrn_reflns_theta_max         25.350
_diffrn_reflns_theta_min         3.270
_diffrn_source                   'SuperNova (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    2.831
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.419
_exptl_absorpt_correction_type   gaussian
_exptl_absorpt_process_details
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.32 (release 02-08-2013 CrysAlis171 .NET)
(compiled Aug  2 2013,16:46:58)
Numerical absorption correction based on gaussian integration over
            a multifaceted crystal model
;
_exptl_crystal_colour            orange
_exptl_crystal_density_diffrn    1.525
_exptl_crystal_description       block
_exptl_crystal_F_000             1236
_exptl_crystal_size_max          0.6874
_exptl_crystal_size_mid          0.3757
_exptl_crystal_size_min          0.2838
_refine_diff_density_max         0.739
_refine_diff_density_min         -0.841
_refine_diff_density_rms         0.134
_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     529
_refine_ls_number_reflns         9896
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.025
_refine_ls_R_factor_all          0.0561
_refine_ls_R_factor_gt           0.0393
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0037P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0641
_refine_ls_wR_factor_ref         0.0728
_reflns_Friedel_coverage         0.000
_reflns_number_gt                7547
_reflns_number_total             9896
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c5nj00761e2.cif
_cod_data_source_block           3
_cod_depositor_comments
'Adding full bibliography for 7054851--7054858.cif.'
_cod_original_cell_volume        2706.58(18)
_cod_database_code               7054855
_manchester_internal_coll_name   adpm86
_manchester_internal_coll_client FO/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   FO
_manchester_internal_coll_date   21/10/2014
_manchester_internal_process_user FO
_manchester_internal_process_date 23/10/2014
_manchester_internal_solution_user FO
_manchester_internal_solution_date 23/10/2014
_manchester_internal_refinement_user FO
_manchester_internal_refinement_date 27/10/2014
_shelxl_version_number           2014/6
_chemical_oxdiff_formula         'C26 H42 I Ce'
_reflns_odcompleteness_completeness 99.71
_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.a Aromatic/amide H refined with riding coordinates:
 C2(H2), C4(H4), C5(H5), C15(H15), C17(H17), C18(H18), C28(H28), C30(H30),
 C31(H31), C41(H41), C43(H43), C44(H44)
2.b Idealised Me refined as rotating group:
 C7(H7A,H7B,H7C), C8(H8A,H8B,H8C), C9(H9A,H9B,H9C), C11(H11A,H11B,H11C),
 C12(H12A,H12B,H12C), C13(H13A,H13B,H13C), C20(H20A,H20B,H20C), C21(H21A,H21B,
 H21C), C22(H22A,H22B,H22C), C24(H24A,H24B,H24C), C25(H25A,H25B,H25C), C26(H26A,
 H26B,H26C), C33(H33A,H33B,H33C), C34(H34A,H34B,H34C), C35(H35A,H35B,H35C),
 C37(H37A,H37B,H37C), C38(H38A,H38B,H38C), C39(H39A,H39B,H39C), C46(H46A,H46B,
 H46C), C47(H47A,H47B,H47C), C48(H48A,H48B,H48C), C50(H50A,H50B,H50C), C51(H51A,
 H51B,H51C), C52(H52A,H52B,H52C)
;
_olex2_submission_special_instructions 'No special instructions were received'