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_7054851
_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         'C15 H29 K O Si2, C4 H8 O'
_chemical_formula_sum            'C19 H37 K O2 Si2'
_chemical_formula_weight         392.76
_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             2015-04-24
_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                 93.491(4)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   10.0903(5)
_cell_length_b                   10.8463(5)
_cell_length_c                   21.9151(11)
_cell_measurement_reflns_used    2467
_cell_measurement_temperature    150.01(10)
_cell_measurement_theta_max      22.3550
_cell_measurement_theta_min      3.6420
_cell_volume                     2394.0(2)
_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      150.01(10)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 8.0714
_diffrn_detector_type            Eos
_diffrn_measured_fraction_theta_full 0.996
_diffrn_measured_fraction_theta_max 0.996
_diffrn_measurement_details
;
  1 omega  -10.00   63.00   1.0000   15.0000
omega____ theta____ kappa____ phi______ frames
    -        6.1663   77.0000 -150.0000 73

  2 omega  -16.00   79.00   1.0000   15.0000
omega____ theta____ kappa____ phi______ frames
    -        6.1663   77.0000   90.0000 95

  3 omega  -46.00   -6.00   1.0000   15.0000
omega____ theta____ kappa____ phi______ frames
    -       -5.6194   90.0000  -30.0000 40
;
_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      0.0689712000
_diffrn_orient_matrix_UB_12      0.0131117000
_diffrn_orient_matrix_UB_13      0.0009713000
_diffrn_orient_matrix_UB_21      0.0037848000
_diffrn_orient_matrix_UB_22      -0.0259668000
_diffrn_orient_matrix_UB_23      -0.0295499000
_diffrn_orient_matrix_UB_31      -0.0137025000
_diffrn_orient_matrix_UB_32      0.0585153000
_diffrn_orient_matrix_UB_33      -0.0133785000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0420
_diffrn_reflns_av_unetI/netI     0.0440
_diffrn_reflns_laue_measured_fraction_full 0.996
_diffrn_reflns_laue_measured_fraction_max 0.996
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_h_min       -8
_diffrn_reflns_limit_k_max       9
_diffrn_reflns_limit_k_min       -9
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_number            5817
_diffrn_reflns_point_group_measured_fraction_full 0.996
_diffrn_reflns_point_group_measured_fraction_max 0.996
_diffrn_reflns_theta_full        18.844
_diffrn_reflns_theta_max         18.844
_diffrn_reflns_theta_min         3.260
_diffrn_source                   'SuperNova (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    0.330
_exptl_absorpt_correction_T_max  0.832
_exptl_absorpt_correction_T_min  0.513
_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            'metallic light colourless'
_exptl_crystal_colour_lustre     metallic
_exptl_crystal_colour_modifier   light
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.090
_exptl_crystal_description       irregular
_exptl_crystal_F_000             856
_exptl_crystal_size_max          0.9281
_exptl_crystal_size_mid          0.1995
_exptl_crystal_size_min          0.1639
_refine_diff_density_max         0.413
_refine_diff_density_min         -0.381
_refine_diff_density_rms         0.062
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.053
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     269
_refine_ls_number_reflns         1872
_refine_ls_number_restraints     162
_refine_ls_restrained_S_all      1.029
_refine_ls_R_factor_all          0.0642
_refine_ls_R_factor_gt           0.0549
_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^)+(0.0654P)^2^+6.1071P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1377
_refine_ls_wR_factor_ref         0.1456
_reflns_Friedel_coverage         0.000
_reflns_number_gt                1595
_reflns_number_total             1872
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c5nj00761e2.cif
_cod_data_source_block           1
_cod_depositor_comments
'Adding full bibliography for 7054851--7054858.cif.'
_cod_database_code               7054851
_manchester_internal_coll_name   adpm42
_manchester_internal_coll_client FO/DPM
_manchester_internal_coll_type   custom
_manchester_internal_coll_frame_time 15s
_manchester_internal_coll_frame_width 1
_manchester_internal_coll_frame_method '\w scans'
_manchester_internal_coll_user   FO/CAPG
_manchester_internal_coll_date   28/04/2015
_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 24/04/2015
_chemical_oxdiff_formula         'K C14 Si3 H24'
_reflns_odcompleteness_completeness 70.26
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     23.29
_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
 C16A-O2A = O2-C16 = C16A-C17A = O2-C19
 1.44 with sigma of 0.008
 C18-C16
 2.5 with sigma of 0.008
 C19-C17
 2.5 with sigma of 0.008
 C18A-C17A = C17-C16 = C19A-O2A = C18-C19
 1.55 with sigma of 0.008
 C17-C18 = C19A-C18A
 1.57 with sigma of 0.008
3. Uiso/Uaniso restraints and constraints
O2 \\sim C16 \\sim C17 \\sim C18 \\sim C19 \\sim O2A \\sim C16A \\sim C17A
\\sim C18A \\sim C19A: within 2A with sigma of 0.004 and sigma for terminal
atoms of 0.008
4. Others
 Sof(O2A)=Sof(C16A)=Sof(H16C)=Sof(H16D)=Sof(C17A)=Sof(H17C)=Sof(H17D)=
 Sof(C18A)=Sof(H18C)=Sof(H18D)=Sof(C19A)=Sof(H19C)=Sof(H19D)=1-FVAR(1)
 Sof(O2)=Sof(C16)=Sof(H16A)=Sof(H16B)=Sof(C17)=Sof(H17A)=Sof(H17B)=Sof(C18)=
 Sof(H18A)=Sof(H18B)=Sof(C19)=Sof(H19A)=Sof(H19B)=FVAR(1)
5.a Secondary CH2 refined with riding coordinates:
 C12(H12A,H12B), C13(H13A,H13B), C14(H14A,H14B), C15(H15A,H15B), C16(H16A,
 H16B), C17(H17A,H17B), C18(H18A,H18B), C19(H19A,H19B), C16A(H16C,H16D),
 C17A(H17C,H17D), C18A(H18C,H18D), C19A(H19C,H19D)
5.b Aromatic/amide H refined with riding coordinates:
 C2(H2), C4(H4), C5(H5)
5.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)
;
_shelx_res_checksum              29913
_shelx_shelxl_version_number     2014/7
_olex2_submission_special_instructions 'No special instructions were received'