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_7710346
_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         'C38 H64 B La O2'
_chemical_formula_sum            'C38 H64 B La O2'
_chemical_formula_weight         702.61
_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'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_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                90
_cell_angle_beta                 93.1475(14)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   10.53775(16)
_cell_length_b                   19.3733(3)
_cell_length_c                   18.2349(3)
_cell_measurement_reflns_used    14970
_cell_measurement_temperature    150.00(10)
_cell_measurement_theta_max      29.1580
_cell_measurement_theta_min      3.7320
_cell_volume                     3717.06(10)
_computing_cell_refinement       'CrysAlisPro 1.171.39.38a (Rigaku OD, 2017)'
_computing_data_collection       'CrysAlisPro 1.171.39.38a (Rigaku OD, 2017)'
_computing_data_reduction        'CrysAlisPro 1.171.39.38a (Rigaku OD, 2017)'
_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    'SIR2004 (Burla et al., 2007)'
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      150.00(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    -10.00  84.00   1.00   19.75    --   16.35  77.00 -60.00   94
  2  \w    -20.00  55.00   1.00   19.75    --   16.35 -99.00  90.00   75
  3  \w      0.00  84.00   1.00   19.75    --   16.35  57.00-180.00   84
  4  \w      0.00  84.00   1.00   19.75    --   16.35  57.00-150.00   84
  5  \w    -51.00  20.00   1.00   19.75    --   16.35 -77.00-150.00   71
;
_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      0.0055500000
_diffrn_orient_matrix_UB_12      -0.0321033000
_diffrn_orient_matrix_UB_13      -0.0182552000
_diffrn_orient_matrix_UB_21      -0.0509394000
_diffrn_orient_matrix_UB_22      -0.0133659000
_diffrn_orient_matrix_UB_23      0.0195533000
_diffrn_orient_matrix_UB_31      -0.0438171000
_diffrn_orient_matrix_UB_32      0.0114492000
_diffrn_orient_matrix_UB_33      -0.0283145000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0321
_diffrn_reflns_av_unetI/netI     0.0323
_diffrn_reflns_Laue_measured_fraction_full 0.998
_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       24
_diffrn_reflns_limit_k_min       -24
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            30964
_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         26.371
_diffrn_reflns_theta_min         3.347
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    1.178
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.88344
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.39.38a (Rigaku Oxford Diffraction, 2017)
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    1.256
_exptl_crystal_description       plate
_exptl_crystal_F_000             1480
_exptl_crystal_size_max          0.2
_exptl_crystal_size_mid          0.2
_exptl_crystal_size_min          0.05
_refine_diff_density_max         0.683
_refine_diff_density_min         -0.402
_refine_diff_density_rms         0.067
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.052
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     401
_refine_ls_number_reflns         7592
_refine_ls_number_restraints     8
_refine_ls_restrained_S_all      1.051
_refine_ls_R_factor_all          0.0340
_refine_ls_R_factor_gt           0.0256
_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^)+(0.0227P)^2^+2.2365P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0554
_refine_ls_wR_factor_ref         0.0581
_reflns_Friedel_coverage         0.000
_reflns_number_gt                6474
_reflns_number_total             7592
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d2dt00996j2.cif
_cod_data_source_block           compound3
_cod_depositor_comments
'Adding full bibliography for 7710344--7710352.cif.'
_cod_original_cell_volume        3717.05(10)
_cod_database_code               7710346
_shelx_shelxl_version_number     2018/1
_chemical_oxdiff_formula         'C1 H1 B1 O1 La1'
_reflns_odcompleteness_completeness 99.72
_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, All C(H,H,H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Restrained distances
 C7A-C6 \\sim C7-C6
 with sigma of 0.001
 C8-C7A \\sim C8-C7
 with sigma of 0.001
3. Uiso/Uaniso restraints and constraints
C7A \\sim C7: within 1.7A with sigma of 0.001 and sigma for terminal atoms of
0.002
4. Others
 Sof(H6BC)=Sof(H6BD)=Sof(H8BC)=Sof(H8BD)=Sof(C7A)=Sof(H7AA)=Sof(H7AB)=1-FVAR(1)
 Sof(H6AA)=Sof(H6AB)=Sof(H8AA)=Sof(H8AB)=Sof(C7)=Sof(H7A)=Sof(H7B)=FVAR(1)
5.a Ternary CH refined with riding coordinates:
 C1(H1), C5(H5)
5.b Secondary CH2 refined with riding coordinates:
 C11(H11A,H11B), C10(H10A,H10B), C12(H12A,H12B), C4(H4A,H4B), C9(H9A,H9B),
 C3(H3A,H3B), C2(H2A,H2B), C6(H6AA,H6AB), C6(H6BC,H6BD), C8(H8AA,H8AB), C8(H8BC,
 H8BD), C7(H7A,H7B), C7A(H7AA,H7AB)
5.c Aromatic/amide H refined with riding coordinates:
 C24(H24), C32(H32), C38(H38), C18(H18), C31(H31), C25(H25)
5.d Idealised Me refined as rotating group:
 C35(H35A,H35B,H35C), C21(H21A,H21B,H21C), C16(H16A,H16B,H16C), C22(H22A,H22B,
 H22C), C15(H15A,H15B,H15C), C23(H23A,H23B,H23C), C37(H37A,H37B,H37C), C14(H14A,
 H14B,H14C), C36(H36A,H36B,H36C), C28(H28A,H28B,H28C), C26(H26A,H26B,H26C),
 C27(H27A,H27B,H27C)
;
_olex2_date_sample_data_collection 2018-02-08
_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 1.202
_oxdiff_exptl_absorpt_empirical_full_min 0.814