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_7710350
_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 La O2'
_chemical_formula_sum            'C36 H61 La O2'
_chemical_formula_weight         664.75
_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             2022-05-01
_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                 107.0666(19)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   11.37190(18)
_cell_length_b                   17.5341(3)
_cell_length_c                   18.3300(3)
_cell_measurement_reflns_used    18344
_cell_measurement_temperature    179.99(11)
_cell_measurement_theta_max      28.9340
_cell_measurement_theta_min      3.9080
_cell_volume                     3493.98(11)
_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
;
Superflip (Palatinus & Chapuis, 2007;Palatinus & van der Lee, 2008;
Palatinus et al., 2012)
;
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      179.99(11)
_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     34.00  89.00   1.00   20.52    --   16.35-178.00  30.00   55
  2  \w    -20.00  55.00   1.00   20.52    --   16.35 -99.00-120.00   75
  3  \w     34.00  89.00   1.00   20.52    --   16.35-178.00 120.00   55
  4  \w      0.00  84.00   1.00   20.52    --   16.35  57.00-180.00   84
  5  \w    -51.00  33.00   1.00   20.52    --   16.35 -57.00-120.00   84
  6  \w    -10.00  84.00   1.00   20.52    --   16.35  77.00  90.00   94
  7  \w     -3.00  65.00   1.00   20.52    --   16.35  38.00   0.00   68
;
_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      -0.0041031000
_diffrn_orient_matrix_UB_12      -0.0374281000
_diffrn_orient_matrix_UB_13      0.0137207000
_diffrn_orient_matrix_UB_21      -0.0634646000
_diffrn_orient_matrix_UB_22      0.0056943000
_diffrn_orient_matrix_UB_23      -0.0044021000
_diffrn_orient_matrix_UB_31      -0.0145776000
_diffrn_orient_matrix_UB_32      -0.0142345000
_diffrn_orient_matrix_UB_33      -0.0378303000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0311
_diffrn_reflns_av_unetI/netI     0.0253
_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            36244
_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         26.372
_diffrn_reflns_theta_min         3.388
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    1.250
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.81798
_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 light colourless'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   light
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.264
_exptl_crystal_description       block
_exptl_crystal_F_000             1400
_exptl_crystal_size_max          0.2
_exptl_crystal_size_mid          0.15
_exptl_crystal_size_min          0.15
_refine_diff_density_max         0.721
_refine_diff_density_min         -0.843
_refine_diff_density_rms         0.075
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.163
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     386
_refine_ls_number_reflns         7122
_refine_ls_number_restraints     44
_refine_ls_restrained_S_all      1.164
_refine_ls_R_factor_all          0.0415
_refine_ls_R_factor_gt           0.0367
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0272P)^2^+6.0586P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0839
_refine_ls_wR_factor_ref         0.0861
_reflns_Friedel_coverage         0.000
_reflns_number_gt                6474
_reflns_number_total             7122
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d2dt00996j2.cif
_cod_data_source_block           compound5
_cod_depositor_comments
'Adding full bibliography for 7710344--7710352.cif.'
_cod_database_code               7710350
_shelx_shelxl_version_number     2018/1
_chemical_oxdiff_formula         'C1 H1 O1 La1'
_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
 C16-C19 \\sim C16-C19A
 with sigma of 0.001
 C16-C18 \\sim C16-C18A
 with sigma of 0.001
3. Uiso/Uaniso restraints and constraints
C16 \\sim C19 \\sim C19A \\sim C18 \\sim C18A: within 1.7A with sigma of 0.001
and sigma for terminal atoms of 0.002
4. Others
 Sof(C19A)=Sof(H19D)=Sof(H19E)=Sof(H19F)=1-FVAR(1)
 Sof(C19)=Sof(H19A)=Sof(H19B)=Sof(H19C)=FVAR(1)
 Sof(C18A)=Sof(H18D)=Sof(H18E)=Sof(H18F)=1-FVAR(2)
 Sof(C18)=Sof(H18A)=Sof(H18B)=Sof(H18C)=FVAR(2)
5.a Ternary CH refined with riding coordinates:
 C1(H1)
5.b Secondary CH2 refined with riding coordinates:
 C4(H4A,H4B), C6(H6A,H6B), C36(H36A,H36B), C34(H34A,H34B), C35(H35A,H35B),
 C33(H33A,H33B), C3(H3A,H3B), C2(H2A,H2B), C5(H5A,H5B)
5.c Aromatic/amide H refined with riding coordinates:
 C20(H20), C27(H27), C13(H13), C14(H14), C7(H7), C26(H26)
5.d Idealised Me refined as rotating group:
 C17(H17A,H17B,H17C), C32(H32A,H32B,H32C), C24(H24A,H24B,H24C), C31(H31A,H31B,
 H31C), C10(H10A,H10B,H10C), C25(H25A,H25B,H25C), C30(H30A,H30B,H30C), C11(H11A,
 H11B,H11C), C23(H23A,H23B,H23C), C12(H12A,H12B,H12C), C18(H18A,H18B,H18C),
 C19(H19A,H19B,H19C), C19A(H19D,H19E,H19F), C18A(H18D,H18E,H18F)
;
_olex2_date_sample_data_collection 2020-06-10
_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 1.224
_oxdiff_exptl_absorpt_empirical_full_min 0.776