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_7710349
_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         'C36 H61 Ce O2'
_chemical_formula_sum            'C36 H61 Ce O2'
_chemical_formula_weight         665.96
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2ybc'
_space_group_name_H-M_alt        'P 1 21/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     iterative
_audit_creation_date             2022-05-13
_audit_creation_method
;
Olex2 1.2
(compiled 2017.08.10 svn.r3458 for OlexSys, GUI svn.r5381)
;
_audit_update_record
;
2022-05-14 deposited with the CCDC.	2022-05-25 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 107.3342(16)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   11.36744(17)
_cell_length_b                   17.5348(3)
_cell_length_c                   18.2956(3)
_cell_measurement_reflns_used    18941
_cell_measurement_temperature    180.01(10)
_cell_measurement_theta_max      29.2220
_cell_measurement_theta_min      3.9190
_cell_volume                     3481.16(10)
_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
;
Superflip (Palatinus & Chapuis, 2007;Palatinus & van der Lee, 2008;
Palatinus et al., 2012)
;
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      180.01(10)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 8.0243
_diffrn_detector_type            EosS2
_diffrn_measured_fraction_theta_full 0.998
_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    -35.00  53.00   1.00    4.20    --  -16.50  38.00  30.00   88
  2  \w    -13.00  88.00   1.00    4.20    --   16.50  19.00 120.00  101
  3  \w    -10.00  84.00   1.00    4.20    --   16.50  77.00  30.00   94
  4  \w    -20.00  55.00   1.00    4.20    --   16.50 -99.00-120.00   75
  5  \w    -20.00  51.00   1.00    4.20    --   16.50 -99.00 120.00   71
  6  \w     -2.00  86.00   1.00    4.20    --   16.50  38.00 -60.00   88
;
_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      -0.0116953000
_diffrn_orient_matrix_UB_12      0.0369240000
_diffrn_orient_matrix_UB_13      -0.0163939000
_diffrn_orient_matrix_UB_21      -0.0364542000
_diffrn_orient_matrix_UB_22      -0.0162511000
_diffrn_orient_matrix_UB_23      -0.0349107000
_diffrn_orient_matrix_UB_31      -0.0529668000
_diffrn_orient_matrix_UB_32      0.0030184000
_diffrn_orient_matrix_UB_33      0.0127274000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0324
_diffrn_reflns_av_unetI/netI     0.0247
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       21
_diffrn_reflns_limit_k_min       -21
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_number            36097
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         26.370
_diffrn_reflns_theta_min         3.293
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    1.335
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.85922
_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 yellowish yellow'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   yellowish
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    1.271
_exptl_crystal_description       block
_exptl_crystal_F_000             1404
_exptl_crystal_size_max          0.2
_exptl_crystal_size_mid          0.2
_exptl_crystal_size_min          0.2
_refine_diff_density_max         0.558
_refine_diff_density_min         -0.359
_refine_diff_density_rms         0.063
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.073
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     395
_refine_ls_number_reflns         7100
_refine_ls_number_restraints     57
_refine_ls_restrained_S_all      1.079
_refine_ls_R_factor_all          0.0316
_refine_ls_R_factor_gt           0.0265
_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^)+(0.0253P)^2^+2.6002P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0604
_refine_ls_wR_factor_ref         0.0631
_reflns_Friedel_coverage         0.000
_reflns_number_gt                6361
_reflns_number_total             7100
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d2dt00996j2.cif
_cod_data_source_block           compound6
_cod_depositor_comments
'Adding full bibliography for 7710344--7710352.cif.'
_cod_database_code               7710349
_shelx_shelxl_version_number     2018/1
_chemical_oxdiff_formula         'C1 H1 N1 O1 Ce1'
_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, All C(H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Restrained distances
 C9-C12A \\sim C9-C12 \\sim C9-C10A \\sim C9-C10 \\sim C9-C11 \\sim C9-C11A
 with sigma of 0.001
3. Uiso/Uaniso restraints and constraints
C11A \\sim C11 \\sim C12A \\sim C12 \\sim C10A \\sim C10: within 1.7A with
sigma of 0.0001 and sigma for terminal atoms of 0.0002
Uanis(C11) \\sim Ueq, Uanis(C11A) \\sim Ueq, Uanis(C10) \\sim Ueq, Uanis(C10A)
\\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
4. Others
 Sof(C10A)=Sof(H10D)=Sof(H10E)=Sof(H10F)=Sof(C11A)=Sof(H11D)=Sof(H11E)=
 Sof(H11F)=Sof(C12A)=Sof(H12D)=Sof(H12E)=Sof(H12F)=1-FVAR(1)
 Sof(C11)=Sof(H11A)=Sof(H11B)=Sof(H11C)=Sof(C12)=Sof(H12A)=Sof(H12B)=Sof(H12C)=
 Sof(C10)=Sof(H10A)=Sof(H10B)=Sof(H10C)=FVAR(1)
5.a Ternary CH refined with riding coordinates:
 C1(H1)
5.b Secondary CH2 refined with riding coordinates:
 C33(H33A,H33B), C2(H2A,H2B), C5(H5A,H5B), C3(H3A,H3B), C4(H4A,H4B), C36(H36A,
 H36B), C34(H34A,H34B), C6(H6A,H6B), C35(H35A,H35B)
5.c Aromatic/amide H refined with riding coordinates:
 C20(H20), C14(H14), C7(H7), C13(H13), C27(H27), C26(H26)
5.d Idealised Me refined as rotating group:
 C17(H17A,H17B,H17C), C24(H24A,H24B,H24C), C19(H19A,H19B,H19C), C32(H32A,H32B,
 H32C), C30(H30A,H30B,H30C), C23(H23A,H23B,H23C), C25(H25A,H25B,H25C), C31(H31A,
 H31B,H31C), C18(H18A,H18B,H18C), C11(H11A,H11B,H11C), C12(H12A,H12B,H12C),
 C10(H10A,H10B,H10C), C10A(H10D,H10E,H10F), C11A(H11D,H11E,H11F), C12A(H12D,
 H12E,H12F)
;
_olex2_date_sample_data_collection 2022-05-12
_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 1.185
_oxdiff_exptl_absorpt_empirical_full_min 0.825