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_7710348
_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 Ce2 N2, 2(C6 H14)'
_chemical_formula_sum            'C76 H120 Ce2 N2'
_chemical_formula_weight         1341.97
_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                64.338(2)
_cell_angle_beta                 73.743(2)
_cell_angle_gamma                77.473(2)
_cell_formula_units_Z            1
_cell_length_a                   10.5325(2)
_cell_length_b                   13.8019(3)
_cell_length_c                   14.5653(3)
_cell_measurement_reflns_used    16079
_cell_measurement_temperature    180.00(10)
_cell_measurement_theta_max      28.2470
_cell_measurement_theta_min      3.9950
_cell_volume                     1820.95(7)
_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    -51.00  43.00   1.00    3.57    --   16.35 -77.00 150.00   94
  2  \w    -10.00  84.00   1.00    3.57    --   16.35  77.00   0.00   94
  3  \w     -3.00  85.00   1.00    3.57    --   16.35  38.00 -60.00   88
  4  \w      0.00  84.00   1.00    3.57    --   16.35  57.00 -90.00   84
  5  \w    -10.00  84.00   1.00    3.57    --   16.35  77.00 120.00   94
  6  \w    -33.00  51.00   1.00    3.57    --  -16.50  57.00  30.00   84
  7  \w     34.00  89.00   1.00    3.57    --   16.35-178.00   0.00   55
  8  \w    -20.00  55.00   1.00    3.57    --   16.35 -99.00 -30.00   75
  9  \w    -20.00  21.00   1.00    3.57    --   16.35 -99.00  90.00   41
 10  \w    -43.00  51.00   1.00    3.57    --  -16.50  77.00-120.00   94
;
_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      -0.0189156000
_diffrn_orient_matrix_UB_12      0.0558174000
_diffrn_orient_matrix_UB_13      -0.0110403000
_diffrn_orient_matrix_UB_21      -0.0511810000
_diffrn_orient_matrix_UB_22      -0.0131612000
_diffrn_orient_matrix_UB_23      0.0456686000
_diffrn_orient_matrix_UB_31      0.0447709000
_diffrn_orient_matrix_UB_32      -0.0014614000
_diffrn_orient_matrix_UB_33      0.0291197000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0313
_diffrn_reflns_av_unetI/netI     0.0310
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            29781
_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         3.295
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    1.273
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.89462
_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            'metallic brownish brown'
_exptl_crystal_colour_lustre     metallic
_exptl_crystal_colour_modifier   brownish
_exptl_crystal_colour_primary    brown
_exptl_crystal_density_diffrn    1.224
_exptl_crystal_description       block
_exptl_crystal_F_000             706
_exptl_crystal_size_max          0.2
_exptl_crystal_size_mid          0.2
_exptl_crystal_size_min          0.15
_refine_diff_density_max         1.294
_refine_diff_density_min         -0.627
_refine_diff_density_rms         0.090
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.076
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     385
_refine_ls_number_reflns         7428
_refine_ls_number_restraints     35
_refine_ls_restrained_S_all      1.076
_refine_ls_R_factor_all          0.0442
_refine_ls_R_factor_gt           0.0393
_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^)+(0.0580P)^2^+2.3220P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1046
_refine_ls_wR_factor_ref         0.1081
_reflns_Friedel_coverage         0.000
_reflns_number_gt                6783
_reflns_number_total             7428
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d2dt00996j2.cif
_cod_data_source_block           compound10
_cod_depositor_comments
'Adding full bibliography for 7710344--7710352.cif.'
_cod_database_code               7710348
_shelx_shelxl_version_number     2018/1
_shelx_estimated_absorpt_t_max   0.832
_shelx_estimated_absorpt_t_min   0.785
_reflns_odcompleteness_completeness 99.76
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     26.32
_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
 C38-C37
 1.52 with sigma of 0.001
 C37-C36
 1.52 with sigma of 0.001
 C36-C35
 1.52 with sigma of 0.001
 C35-C34
 1.52 with sigma of 0.001
 C34-C33
 1.52 with sigma of 0.001
3. Uiso/Uaniso restraints and constraints
C37 \\sim C38 \\sim C36 \\sim C35 \\sim C34 \\sim C33: within 1.7A with sigma
of 0.001 and sigma for terminal atoms of 0.002
4. Others
 Sof(Ce1A)=1-FVAR(1)
 Sof(Ce1)=FVAR(1)
5.a Secondary CH2 refined with riding coordinates:
 C36(H36A,H36B), C35(H35A,H35B), C34(H34A,H34B), C37(H37A,H37B)
5.b Aromatic/amide H refined with riding coordinates:
 C20(H20), C26(H26), C1(H1), C27(H27), C6(H6), C4(H4), C7(H7), C5(H5), C8(H8),
 C14(H14)
5.c Idealised Me refined as rotating group:
 C19(H19A,H19B,H19C), C12(H12A,H12B,H12C), C30(H30A,H30B,H30C), C24(H24A,H24B,
 H24C), C23(H23A,H23B,H23C), C11(H11A,H11B,H11C), C25(H25A,H25B,H25C), C32(H32A,
 H32B,H32C), C18(H18A,H18B,H18C), C31(H31A,H31B,H31C), C13(H13A,H13B,H13C),
 C17(H17A,H17B,H17C), C33(H33A,H33B,H33C), C38(H38A,H38B,H38C)
;
_olex2_date_sample_data_collection 2021-03-09
_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 1.218
_oxdiff_exptl_absorpt_empirical_full_min 0.848