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_7710352
_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         'C52 H84 Cl2 La2'
_chemical_formula_sum            'C52 H84 Cl2 La2'
_chemical_formula_weight         1057.91
_space_group_crystal_system      orthorhombic
_space_group_IT_number           56
_space_group_name_Hall           '-P 2ab 2ac'
_space_group_name_H-M_alt        'P c c n'
_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                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   12.9548(3)
_cell_length_b                   16.8937(3)
_cell_length_c                   24.5878(5)
_cell_measurement_reflns_used    22311
_cell_measurement_temperature    180.00(10)
_cell_measurement_theta_max      29.2230
_cell_measurement_theta_min      3.7370
_cell_volume                     5381.15(19)
_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 0.996
_diffrn_measured_fraction_theta_max 0.996
_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      0.00  84.00   1.00   11.01    --   16.35  57.00  60.00   84
  2  \w    -10.00  84.00   1.00   11.01    --   16.35  77.00-150.00   94
  3  \w    -35.00  53.00   1.00   11.01    --  -16.50  38.00-150.00   88
  4  \w    -20.00   5.00   1.00   11.01    --   16.35 -99.00  60.00   25
  5  \w     12.00  54.00   1.00   11.01    --   16.35 -99.00 120.00   42
  6  \w    -30.00  47.00   1.00   11.01    --   16.35   0.00  30.00   77
  7  \w    -56.00   9.00   1.00   11.01    --  -16.50 -77.00 -60.00   65
  8  \w     34.00  81.00   1.00   11.01    --   16.35-178.00 120.00   47
  9  \w    -51.00  33.00   1.00   11.01    --   16.35 -57.00 -90.00   84
;
_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      0.0481042000
_diffrn_orient_matrix_UB_12      0.0199584000
_diffrn_orient_matrix_UB_13      0.0016674000
_diffrn_orient_matrix_UB_21      -0.0259668000
_diffrn_orient_matrix_UB_22      0.0368869000
_diffrn_orient_matrix_UB_23      -0.0011898000
_diffrn_orient_matrix_UB_31      -0.0039007000
_diffrn_orient_matrix_UB_32      0.0003672000
_diffrn_orient_matrix_UB_33      0.0287776000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0368
_diffrn_reflns_av_unetI/netI     0.0167
_diffrn_reflns_Laue_measured_fraction_full 0.996
_diffrn_reflns_Laue_measured_fraction_max 0.996
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       21
_diffrn_reflns_limit_k_min       -21
_diffrn_reflns_limit_l_max       29
_diffrn_reflns_limit_l_min       -30
_diffrn_reflns_number            62442
_diffrn_reflns_point_group_measured_fraction_full 0.996
_diffrn_reflns_point_group_measured_fraction_max 0.996
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         26.372
_diffrn_reflns_theta_min         3.322
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    1.695
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.62704
_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 light colourless'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   light
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.306
_exptl_crystal_description       plate
_exptl_crystal_F_000             2176
_exptl_crystal_size_max          0.2
_exptl_crystal_size_mid          0.2
_exptl_crystal_size_min          0.05
_refine_diff_density_max         0.655
_refine_diff_density_min         -0.683
_refine_diff_density_rms         0.065
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.276
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     266
_refine_ls_number_reflns         5501
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.276
_refine_ls_R_factor_all          0.0439
_refine_ls_R_factor_gt           0.0345
_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^)+(0.0063P)^2^+9.1855P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0563
_refine_ls_wR_factor_ref         0.0594
_reflns_Friedel_coverage         0.000
_reflns_number_gt                4625
_reflns_number_total             5501
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d2dt00996j2.cif
_cod_data_source_block           compound7
_cod_depositor_comments
'Adding full bibliography for 7710344--7710352.cif.'
_cod_original_cell_volume        5381.16(18)
_cod_database_code               7710352
_shelx_shelxl_version_number     2018/1
_chemical_oxdiff_formula         'C1 H1 Ce1 Cl1'
_reflns_odcompleteness_completeness 99.62
_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.a Aromatic/amide H refined with riding coordinates:
 C8(H8), C1(H1), C7(H7), C20(H20), C21(H21), C14(H14)
2.b Idealised Me refined as rotating group:
 C5(H5A,H5B,H5C), C11(H11A,H11B,H11C), C12(H12A,H12B,H12C), C4(H4A,H4B,H4C),
 C24(H24A,H24B,H24C), C26(H26A,H26B,H26C), C13(H13A,H13B,H13C), C19(H19A,H19B,
 H19C), C6(H6A,H6B,H6C), C25(H25A,H25B,H25C), C18(H18A,H18B,H18C), C17(H17A,
 H17B,H17C)
;
_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 1.811
_oxdiff_exptl_absorpt_empirical_full_min 0.464