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_7710345
_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 Ce O2'
_chemical_formula_sum            'C38 H64 B Ce O2'
_chemical_formula_weight         703.82
_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     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                 93.152(2)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   10.5206(3)
_cell_length_b                   19.3399(5)
_cell_length_c                   18.2318(5)
_cell_measurement_reflns_used    14549
_cell_measurement_temperature    150.01(10)
_cell_measurement_theta_max      29.0450
_cell_measurement_theta_min      3.7710
_cell_volume                     3703.96(18)
_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    'ShelXT (Sheldrick, 2015)'
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      150.01(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    -55.00  46.00   1.00   24.64    --   16.35 -19.00 -90.00  101
  2  \w    -51.00  33.00   1.00   24.64    --   16.35 -57.00  30.00   84
  3  \w    -71.00 -25.00   1.00   24.64    --  -16.50 127.00  -3.00   46
  4  \w    -84.00  10.00   1.00   24.64    --  -16.50 -77.00 -90.00   94
  5  \w    -55.00  37.00   1.00   24.64    --   16.35 -19.00 150.00   92
;
_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      -0.0156922000
_diffrn_orient_matrix_UB_12      0.0274526000
_diffrn_orient_matrix_UB_13      0.0236609000
_diffrn_orient_matrix_UB_21      -0.0239327000
_diffrn_orient_matrix_UB_22      -0.0241973000
_diffrn_orient_matrix_UB_23      0.0250221000
_diffrn_orient_matrix_UB_31      0.0611519000
_diffrn_orient_matrix_UB_32      -0.0024392000
_diffrn_orient_matrix_UB_33      0.0182329000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0370
_diffrn_reflns_av_unetI/netI     0.0344
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       24
_diffrn_reflns_limit_k_min       -23
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_number            30589
_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         26.372
_diffrn_reflns_theta_min         3.519
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    1.258
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.71591
_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    1.262
_exptl_crystal_description       plate
_exptl_crystal_F_000             1484
_exptl_crystal_size_max          0.2
_exptl_crystal_size_mid          0.2
_exptl_crystal_size_min          0.02
_refine_diff_density_max         1.187
_refine_diff_density_min         -0.755
_refine_diff_density_rms         0.088
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.099
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     391
_refine_ls_number_reflns         7563
_refine_ls_number_restraints     6
_refine_ls_restrained_S_all      1.107
_refine_ls_R_factor_all          0.0407
_refine_ls_R_factor_gt           0.0337
_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^)+(0.0230P)^2^+7.4490P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0746
_refine_ls_wR_factor_ref         0.0777
_reflns_Friedel_coverage         0.000
_reflns_number_gt                6658
_reflns_number_total             7563
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d2dt00996j2.cif
_cod_data_source_block           compound4
_cod_depositor_comments
'Adding full bibliography for 7710344--7710352.cif.'
_cod_original_cell_volume        3703.96(17)
_cod_database_code               7710345
_shelx_shelxl_version_number     2018/1
_chemical_oxdiff_formula         'C1 H1 O1 B1 Ce1'
_reflns_odcompleteness_completeness 99.69
_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. Uiso/Uaniso restraints and constraints
Uanis(C3) \\sim Ueq: with sigma of 0.005 and sigma for terminal atoms of 0.001
3.a Ternary CH refined with riding coordinates:
 C5(H5), C1(H1)
3.b Secondary CH2 refined with riding coordinates:
 C11(H11A,H11B), C12(H12A,H12B), C9(H9A,H9B), C10(H10A,H10B), C6(H6A,H6B),
 C7(H7A,H7B), C8(H8A,H8B), C2(H2A,H2B), C4(H4A,H4B), C3(H3A,H3B)
3.c Aromatic/amide H refined with riding coordinates:
 C20(H20), C26(H26), C19(H19), C33(H33), C32(H32), C13(H13)
3.d Idealised Me refined as rotating group:
 C36(H36A,H36B,H36C), C38(H38A,H38B,H38C), C31(H31A,H31B,H31C), C37(H37A,H37B,
 H37C), C29(H29A,H29B,H29C), C30(H30A,H30B,H30C), C17(H17A,H17B,H17C), C16(H16A,
 H16B,H16C), C18(H18A,H18B,H18C), C24(H24A,H24B,H24C), C23(H23A,H23B,H23C),
 C25(H25A,H25B,H25C)
;
_olex2_date_sample_data_collection 2018-05-12
_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 1.446
_oxdiff_exptl_absorpt_empirical_full_min 0.647