Reactivity studies on lanthanum and cerium hydrido metallocenes.
Yi, Chengkun; Wu, Lingfeng; Chen, Liang; Ren, Wenshan; Dalton transactions (Cambridge, England : 2003) 51 (2022) 9241–9246; doi:10.1039/d2dt00996j

data_7710351
_publ_section_title
;
 Reactivity studies on lanthanum and cerium hydrido metallocenes.
;
_journal_issue                   24
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              9241
_journal_page_last               9246
_journal_paper_doi               10.1039/d2dt00996j
_journal_volume                  51
_journal_year                    2022
_chemical_formula_moiety         'C64 H92 La2 N2'
_chemical_formula_sum            'C64 H92 La2 N2'
_chemical_formula_weight         1167.21
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_audit_creation_date             2022-05-01
_audit_creation_method
;
Olex2 1.2
(compiled 2017.08.10 svn.r3458 for OlexSys, GUI svn.r5381)
;
_audit_update_record
;
2022-05-03 deposited with the CCDC.	2022-05-25 downloaded from the CCDC.
;
_cell_angle_alpha                78.604(2)
_cell_angle_beta                 76.732(3)
_cell_angle_gamma                70.957(2)
_cell_formula_units_Z            1
_cell_length_a                   10.2919(3)
_cell_length_b                   11.7807(2)
_cell_length_c                   14.5718(5)
_cell_measurement_reflns_used    16254
_cell_measurement_temperature    180.00(10)
_cell_measurement_theta_max      27.8900
_cell_measurement_theta_min      3.6730
_cell_volume                     1610.98(8)
_computing_cell_refinement       'CrysAlisPro 1.171.39.46e (Rigaku OD, 2018)'
_computing_data_collection       'CrysAlisPro 1.171.39.46e (Rigaku OD, 2018)'
_computing_data_reduction        'CrysAlisPro 1.171.39.46e (Rigaku OD, 2018)'
_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    'ShelXT (Sheldrick, 2015)'
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      180.00(10)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 8.0243
_diffrn_detector_type            EosS2
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_details
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  t~exp~   \w     \q     \k     \f   Frames
  1  \w    -53.00  86.00   1.00    4.97    --   16.35   0.00  90.00  139
  2  \w    -20.00  55.00   1.00    4.97    --   16.35 -99.00-150.00   75
  3  \w      0.00  84.00   1.00    4.97    --   16.35  57.00 -60.00   84
  4  \w    -84.00   0.00   1.00    4.97    --  -16.50 -57.00 -90.00   84
  5  \w    -84.00  10.00   1.00    4.97    --  -16.50 -77.00  60.00   94
  6  \w    -70.00 -23.00   1.00    4.97    --  -16.50 125.00 -13.00   47
  7  \w    -13.00  88.00   1.00    4.97    --   16.35  19.00-120.00  101
  8  \w     35.00  89.00   1.00    4.97    --   16.35 178.00-180.00   54
  9  \w    -51.00  33.00   1.00    4.97    --   16.35 -57.00 -90.00   84
 10  \w     35.00  89.00   1.00    4.97    --   16.35 178.00  30.00   54
 11  \w    -84.00   0.00   1.00    4.97    --  -16.50 -57.00 150.00   84
 12  \w    -20.00  28.00   1.00    4.97    --   16.35 -99.00  90.00   48
 13  \w    -20.00  55.00   1.00    4.97    --   16.35 -99.00 -30.00   75
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at home/near, EosS2'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      -0.0644237000
_diffrn_orient_matrix_UB_12      0.0015139000
_diffrn_orient_matrix_UB_13      0.0311269000
_diffrn_orient_matrix_UB_21      -0.0349902000
_diffrn_orient_matrix_UB_22      0.0184141000
_diffrn_orient_matrix_UB_23      -0.0395136000
_diffrn_orient_matrix_UB_31      0.0107260000
_diffrn_orient_matrix_UB_32      -0.0615558000
_diffrn_orient_matrix_UB_33      -0.0040280000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0457
_diffrn_reflns_av_unetI/netI     0.0366
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            32522
_diffrn_reflns_point_group_measured_fraction_full 0.997
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         26.371
_diffrn_reflns_theta_min         3.459
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    1.343
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.82875
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.39.46e (Rigaku Oxford Diffraction, 2018)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            'clear orangish orange'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   orangish
_exptl_crystal_colour_primary    orange
_exptl_crystal_density_diffrn    1.203
_exptl_crystal_description       plate
_exptl_crystal_F_000             604
_exptl_crystal_size_max          0.2
_exptl_crystal_size_mid          0.2
_exptl_crystal_size_min          0.1
_refine_diff_density_max         1.684
_refine_diff_density_min         -0.981
_refine_diff_density_rms         0.118
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.189
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     422
_refine_ls_number_reflns         6565
_refine_ls_number_restraints     242
_refine_ls_restrained_S_all      1.177
_refine_ls_R_factor_all          0.0624
_refine_ls_R_factor_gt           0.0597
_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^)+(0.0480P)^2^+7.5730P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1456
_refine_ls_wR_factor_ref         0.1471
_reflns_Friedel_coverage         0.000
_reflns_number_gt                6252
_reflns_number_total             6565
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d2dt00996j2.cif
_cod_data_source_block           compound9
_cod_depositor_comments
'Adding full bibliography for 7710344--7710352.cif.'
_cod_original_cell_volume        1610.97(8)
_cod_database_code               7710351
_shelx_shelxl_version_number     2018/1
_chemical_oxdiff_formula         'C1 H1 N1 Ce1 O1'
_reflns_odcompleteness_completeness 99.77
_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. Restrained distances
 C23A-C25A
 2.174 with sigma of 0.001
 C9A-C10A \\sim C9-C12
 with sigma of 0.001
3. Uiso/Uaniso restraints and constraints
C16 \\sim C17 \\sim C19 \\sim C18: within 1.7A with sigma of 0.001 and sigma
for terminal atoms of 0.002
C14A \\sim C7 \\sim C15 \\sim C7A \\sim C8 \\sim C13 \\sim C14 \\sim C13A:
within 1.7A with sigma of 0.001 and sigma for terminal atoms of 0.002
C9A \\sim C9 \\sim C10 \\sim C11 \\sim C12 \\sim C10A \\sim C11A: within 1.7A
with sigma of 0.001 and sigma for terminal atoms of 0.002
C25A \\sim C25 \\sim C23 \\sim C23A \\sim C24: within 1.7A with sigma of 0.001
and sigma for terminal atoms of 0.002
C25A \\sim C25 \\sim C22 \\sim C23A \\sim C23 \\sim C24A \\sim C24: within 1.7A
with sigma of 0.001 and sigma for terminal atoms of 0.002
C29 \\sim C32 \\sim C31 \\sim C30: within 1.7A with sigma of 0.001 and sigma
for terminal atoms of 0.002
Uanis(C12A) \\sim Ueq: with sigma of 0.001 and sigma for terminal atoms of 0.001
4. Others
 Sof(C7A)=Sof(H7A)=1-FVAR(1)
 Sof(C7)=Sof(H7)=FVAR(1)
 Sof(C13A)=Sof(H13A)=1-FVAR(2)
 Sof(C13)=Sof(H13)=FVAR(2)
 Sof(C14A)=Sof(H14A)=1-FVAR(3)
 Sof(C14)=Sof(H14)=FVAR(3)
 Sof(C10A)=Sof(H10D)=Sof(H10E)=Sof(H10F)=Sof(C9A)=Sof(C11A)=Sof(H11D)=
 Sof(H11E)=Sof(H11F)=Sof(C12A)=Sof(H12D)=Sof(H12E)=Sof(H12F)=1-FVAR(4)
 Sof(C10)=Sof(H10A)=Sof(H10B)=Sof(H10C)=Sof(C9)=Sof(C12)=Sof(H12A)=Sof(H12B)=
 Sof(H12C)=Sof(C11)=Sof(H11A)=Sof(H11B)=Sof(H11C)=FVAR(4)
 Sof(C23A)=Sof(H23D)=Sof(H23E)=Sof(H23F)=1-FVAR(5)
 Sof(C23)=Sof(H23A)=Sof(H23B)=Sof(H23C)=FVAR(5)
 Sof(C25A)=Sof(H25D)=Sof(H25E)=Sof(H25F)=1-FVAR(6)
 Sof(C25)=Sof(H25A)=Sof(H25B)=Sof(H25C)=FVAR(6)
 Sof(C24A)=Sof(H24D)=Sof(H24E)=Sof(H24F)=1-FVAR(7)
 Sof(C24)=Sof(H24A)=Sof(H24B)=Sof(H24C)=FVAR(7)
5.a Ternary CH refined with riding coordinates:
 C4(H4), C7A(H7A), C13A(H13A), C14A(H14A)
5.b Aromatic/amide H refined with riding coordinates:
 C27(H27), C26(H26), C20(H20), C5(H5), C1(H1), C6(H6), C7(H7), C14(H14),
 C13(H13)
5.c Idealised Me refined as rotating group:
 C32(H32A,H32B,H32C), C30(H30A,H30B,H30C), C31(H31A,H31B,H31C), C24(H24A,H24B,
 H24C), C18(H18A,H18B,H18C), C19(H19A,H19B,H19C), C10(H10A,H10B,H10C), C25(H25A,
 H25B,H25C), C23(H23A,H23B,H23C), C17(H17A,H17B,H17C), C12(H12A,H12B,H12C),
 C11(H11A,H11B,H11C), C10A(H10D,H10E,H10F), C11A(H11D,H11E,H11F), C12A(H12D,
 H12E,H12F), C23A(H23D,H23E,H23F), C25A(H25D,H25E,H25F), C24A(H24D,H24E,H24F)
;
_olex2_date_sample_data_collection 2021-02-08
_olex2_submission_special_instructions 'No special instructions were received'
_oxdiff_exptl_absorpt_empirical_details
;
Empirical correction (ABSPACK) includes:
- Absorption correction using spherical harmonics
- Frame scaling
;
_oxdiff_exptl_absorpt_empirical_full_max 1.297
_oxdiff_exptl_absorpt_empirical_full_min 0.766