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_7710344
_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         'C78 H126 La3 P7, C7 H8'
_chemical_formula_sum            'C85 H134 La3 P7'
_chemical_formula_weight         1789.43
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_audit_creation_date             2018-03-30
_audit_creation_method
;
Olex2 1.2
(compiled 2016.11.07 svn.r3352 for OlexSys, GUI svn.r5261)
;
_audit_update_record
;
2022-03-25 deposited with the CCDC.	2022-05-25 downloaded from the CCDC.
;
_cell_angle_alpha                74.861(3)
_cell_angle_beta                 81.924(2)
_cell_angle_gamma                68.345(3)
_cell_formula_units_Z            2
_cell_length_a                   14.7718(3)
_cell_length_b                   14.8165(5)
_cell_length_c                   22.3328(8)
_cell_measurement_reflns_used    16935
_cell_measurement_temperature    150.00(10)
_cell_measurement_theta_max      72.8550
_cell_measurement_theta_min      4.2600
_cell_volume                     4380.0(3)
_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      150.00(10)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 8.0243
_diffrn_detector_type            EosS2
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.979
_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    -94.00 -58.00   1.00    4.79    --  -37.03 -19.00  60.00   36
  2  \w   -106.00 -57.00   1.00    4.79    --  -37.03 -19.00 -30.00   49
  3  \w    -63.00   5.00   1.00    4.79    --  -37.03  77.00 -90.00   68
  4  \w    -37.00  -9.00   1.00    4.79    --  -37.03 -19.00  60.00   28
  5  \w    -34.00  -8.00   1.00    4.79    --  -37.03 -19.00 -30.00   26
  6  \w     48.00  75.00   1.00    4.79    --   37.03-126.00-180.00   27
  7  \w     26.00  89.00   1.00    4.79    --   37.03-126.00-150.00   63
  8  \w     74.00 103.00   1.00    4.79    --   37.03   0.00 -90.00   29
  9  \w      1.00  70.00   1.00    4.79    --   37.03 -99.00 -30.00   69
 10  \w     18.00  49.00   1.00    4.79    --   37.03  19.00  60.00   31
 11  \w     31.00  56.00   1.00    4.79    --   37.03-126.00 -90.00   25
 12  \w    -32.00  54.00   1.00    4.79    --   37.03   0.00 -90.00   86
 13  \w     34.00  61.00   1.00    4.79    --   37.03-126.00 -30.00   27
 14  \w     27.00  56.00   1.00    4.79    --   37.03 -38.00 -60.00   29
 15  \w    -33.00  13.00   1.00    4.79    --   37.03 -19.00-120.00   46
 16  \w     39.00  75.00   1.00    4.79    --   37.03 -99.00  30.00   36
 17  \w     72.00  97.00   1.00    4.79    --   37.03  19.00  60.00   25
 18  \w      9.00  53.00   1.00    4.79    --   37.03 -57.00   0.00   44
 19  \w    -18.00  27.00   1.00    4.79    --   37.03 -57.00-150.00   45
 20  \w     18.00  78.00   1.00    4.79    --   37.03  38.00 150.00   60
 21  \w     63.00  90.00   1.00    4.79    --   37.03-126.00 -30.00   27
 22  \w     43.00 122.00   1.00   19.19    --  110.47 -45.00 -60.00   79
 23  \w     86.00 138.00   1.00   19.19    --  110.47 178.00   0.00   52
 24  \w     60.00 106.00   1.00   19.19    --  110.47 -95.00  30.00   46
 25  \w     73.00 116.00   1.00   19.19    --  110.47-112.00-150.00   43
 26  \w    101.00 131.00   1.00   19.19    --  110.47 -30.00 -90.00   30
 27  \w     89.00 155.00   1.00   19.19    --  110.47  30.00 -90.00   66
 28  \w     77.00 109.00   1.00   19.19    --  110.47 -95.00 120.00   32
 29  \w     99.00 178.00   1.00   19.19    --  110.47  45.00   0.00   79
 30  \w     42.00  68.00   1.00   19.19    --  110.47 -30.00 -90.00   26
 31  \w    130.00 171.00   1.00   19.19    --  110.47  45.00  90.00   41
 32  \w     62.00 108.00   1.00   19.19    --  110.47 -95.00  60.00   46
 33  \w     83.00 109.00   1.00   19.19    --  110.47 -95.00-120.00   26
 34  \w     83.00 109.00   1.00   19.19    --  110.47 -95.00 -60.00   26
 35  \w    115.00 169.00   1.00   19.19    --  110.47 112.00 -60.00   54
 36  \w     73.00 128.00   1.00   19.19    --  110.47 -61.00  30.00   55
 37  \w    105.00 176.00   1.00   19.19    --  110.47 112.00  90.00   71
 38  \w     92.00 177.00   1.00   19.19    --  110.47  61.00 -30.00   85
 39  \w    101.00 178.00   1.00   19.19    --  110.47  77.00-150.00   77
 40  \w     44.00 129.00   1.00   19.19    --  110.47 -61.00-180.00   85
 41  \w     54.00 114.00   1.00   19.19    --  110.47 -30.00  30.00   60
;
_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      0.0152718000
_diffrn_orient_matrix_UB_12      -0.0049215000
_diffrn_orient_matrix_UB_13      0.0677644000
_diffrn_orient_matrix_UB_21      0.0106861000
_diffrn_orient_matrix_UB_22      -0.1110392000
_diffrn_orient_matrix_UB_23      0.0177048000
_diffrn_orient_matrix_UB_31      0.1107876000
_diffrn_orient_matrix_UB_32      -0.0291661000
_diffrn_orient_matrix_UB_33      -0.0146215000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0325
_diffrn_reflns_av_unetI/netI     0.0448
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.979
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       25
_diffrn_reflns_limit_l_min       -27
_diffrn_reflns_number            38478
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.979
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         73.107
_diffrn_reflns_theta_min         3.464
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    12.593
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.24866
_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    1.357
_exptl_crystal_description       plate
_exptl_crystal_F_000             1840
_exptl_crystal_size_max          0.2
_exptl_crystal_size_mid          0.15
_exptl_crystal_size_min          0.03
_refine_diff_density_max         1.967
_refine_diff_density_min         -1.659
_refine_diff_density_rms         0.100
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.034
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     861
_refine_ls_number_reflns         17187
_refine_ls_number_restraints     48
_refine_ls_restrained_S_all      1.037
_refine_ls_R_factor_all          0.0621
_refine_ls_R_factor_gt           0.0487
_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^)+(0.0690P)^2^+6.8410P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1254
_refine_ls_wR_factor_ref         0.1341
_reflns_Friedel_coverage         0.000
_reflns_number_gt                13908
_reflns_number_total             17187
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d2dt00996j2.cif
_cod_data_source_block           compound11
_cod_depositor_comments
'Adding full bibliography for 7710344--7710352.cif.'
_cod_original_cell_volume        4379.9(2)
_cod_database_code               7710344
_chemical_oxdiff_formula         'C1 H1 B1 La1 P1'
_reflns_odcompleteness_completeness 99.93
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     66.97
_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. Uiso/Uaniso restraints and constraints
Uanis(C82) \\sim Ueq, Uanis(C81) \\sim Ueq, Uanis(C80) \\sim Ueq, Uanis(C85)
\\sim Ueq, Uanis(C84) \\sim Ueq, Uanis(C83) \\sim Ueq: with sigma of 0.01 and
sigma for terminal atoms of 0.01
Uanis(C79) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.01
Uanis(C5) \\sim Ueq: with sigma of 0.05 and sigma for terminal atoms of 0.01
Uanis(C81) = Uanis(C80) = Uanis(C85) = Uanis(C84) = Uanis(C83) = Uanis(C82)
3. Others
 Sof(La2A)=1-FVAR(1)
 Sof(La2)=FVAR(1)
4.a Aromatic/amide H refined with riding coordinates:
 C14(H14), C8(H8), C66(H66), C73(H73), C1(H1), C20(H20), C40(H40), C21(H21),
 C46(H46), C7(H7), C47(H47), C72(H72), C33(H33), C53(H53), C27(H27), C34(H34),
 C81(H81), C82(H82), C83(H83), C84(H84), C85(H85), C60(H60), C59(H59)
4.b Fitted hexagon refined as free rotating group:
 C81(C82,C83,C84,C85,C80)
4.c Idealised Me refined as rotating group:
 C44(H44A,H44B,H44C), C45(H45A,H45B,H45C), C30(H30A,H30B,H30C), C4(H4A,H4B,
 H4C), C43(H43A,H43B,H43C), C26(H26A,H26B,H26C), C52(H52A,H52B,H52C), C24(H24A,
 H24B,H24C), C51(H51A,H51B,H51C), C18(H18A,H18B,H18C), C11(H11A,H11B,H11C),
 C25(H25A,H25B,H25C), C63(H63A,H63B,H63C), C69(H69A,H69B,H69C), C78(H78A,H78B,
 H78C), C65(H65A,H65B,H65C), C56(H56A,H56B,H56C), C64(H64A,H64B,H64C), C17(H17A,
 H17B,H17C), C31(H31A,H31B,H31C), C38(H38A,H38B,H38C), C76(H76A,H76B,H76C),
 C6(H6A,H6B,H6C), C71(H71A,H71B,H71C), C5(H5A,H5B,H5C), C12(H12A,H12B,H12C),
 C13(H13A,H13B,H13C), C57(H57A,H57B,H57C), C77(H77A,H77B,H77C), C37(H37A,H37B,
 H37C), C70(H70A,H70B,H70C), C19(H19A,H19B,H19C), C50(H50A,H50B,H50C), C32(H32A,
 H32B,H32C), C39(H39A,H39B,H39C), C58(H58A,H58B,H58C), C79(H79A,H79B,H79C)
;
_shelx_shelxl_version_number     2017/1
_olex2_date_sample_data_collection 2018-03-22
_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 2.764
_oxdiff_exptl_absorpt_empirical_full_min 0.596