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_7710347
_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 Ce3 P7, C7 H8'
_chemical_formula_sum            'C85 H134 Ce3 P7'
_chemical_formula_weight         1793.06
_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             2022-03-23
_audit_creation_method
;
Olex2 1.2
(compiled 2017.08.10 svn.r3458 for OlexSys, GUI svn.r5381)
;
_audit_update_record
;
2022-03-25 deposited with the CCDC.	2022-05-25 downloaded from the CCDC.
;
_cell_angle_alpha                74.202(4)
_cell_angle_beta                 81.751(3)
_cell_angle_gamma                68.303(3)
_cell_formula_units_Z            2
_cell_length_a                   14.7799(5)
_cell_length_b                   14.8493(5)
_cell_length_c                   22.4110(9)
_cell_measurement_reflns_used    11020
_cell_measurement_temperature    180.01(10)
_cell_measurement_theta_max      71.5320
_cell_measurement_theta_min      4.2730
_cell_volume                     4392.4(3)
_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      180.01(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 0.974
_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    -39.00   9.00   1.00    8.07    --  -35.97  57.00-120.00   48
  2  \w   -102.00 -35.00   1.00    8.07    --  -35.97 -38.00   0.00   67
  3  \w   -103.00  33.00   1.00    8.07    --  -35.97   0.00-150.00  136
  4  \w     28.00  54.00   1.00    8.07    --   35.97-126.00-180.00   26
  5  \w      9.00  75.00   1.00    8.07    --   35.97 -99.00   0.00   66
  6  \w     24.00  73.00   1.00    8.07    --   35.97-126.00 -30.00   49
  7  \w      7.00  69.00   1.00    8.07    --   35.97 -99.00 120.00   62
  8  \w      7.00  74.00   1.00    8.07    --   35.97 -99.00-150.00   67
  9  \w     42.00 104.00   1.00   32.31    --  107.97 -61.00  60.00   62
 10  \w     44.00  71.00   1.00   32.31    --  107.97 -45.00-150.00   27
 11  \w     45.00 109.00   1.00   32.31    --  107.97 -95.00-180.00   64
 12  \w     48.00  88.00   1.00   32.31    --  107.97 -95.00   0.00   40
 13  \w     91.00 129.00   1.00   32.31    --  107.97 -30.00  30.00   38
 14  \w     39.00  85.00   1.00   32.31    --  107.97 -95.00  60.00   46
 15  \w     57.00 123.00   1.00   32.31    --  107.97 -45.00 -30.00   66
 16  \w     74.00 112.00   1.00   32.31    --  107.97-112.00 120.00   38
 17  \w     38.00  79.00   1.00   32.31    --  107.97 -30.00 -60.00   41
 18  \w     87.00 112.00   1.00   32.31    --  107.97-112.00   0.00   25
 19  \w     47.00  74.00   1.00   32.31    --  107.97-112.00   0.00   27
 20  \w    103.00 163.00   1.00   32.31    --  107.97 112.00  60.00   60
 21  \w     43.00  86.00   1.00   32.31    --  107.97 -77.00-150.00   43
 22  \w     73.00 178.00   1.00   32.31    --  107.97  15.00  60.00  105
 23  \w     63.00 105.00   1.00   32.31    --  107.97 -95.00 -90.00   42
 24  \w     87.00 115.00   1.00   32.31    --  107.97 -45.00-150.00   28
 25  \w     38.00 119.00   1.00   32.31    --  107.97 -30.00 120.00   81
 26  \w     91.00 176.00   1.00   32.31    --  107.97  45.00 120.00   85
;
_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      0.0714788000
_diffrn_orient_matrix_UB_12      -0.1018480000
_diffrn_orient_matrix_UB_13      0.0324902000
_diffrn_orient_matrix_UB_21      -0.0521378000
_diffrn_orient_matrix_UB_22      0.0144801000
_diffrn_orient_matrix_UB_23      0.0631520000
_diffrn_orient_matrix_UB_31      -0.0691810000
_diffrn_orient_matrix_UB_32      -0.0513389000
_diffrn_orient_matrix_UB_33      -0.0084617000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0292
_diffrn_reflns_av_unetI/netI     0.0467
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.974
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -27
_diffrn_reflns_number            29866
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.974
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         71.900
_diffrn_reflns_theta_min         3.444
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    13.295
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.31418
_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 brownish brown'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   brownish
_exptl_crystal_colour_primary    brown
_exptl_crystal_density_diffrn    1.356
_exptl_crystal_description       plate
_exptl_crystal_F_000             1846
_exptl_crystal_size_max          0.1
_exptl_crystal_size_mid          0.08
_exptl_crystal_size_min          0.03
_refine_diff_density_max         1.252
_refine_diff_density_min         -1.119
_refine_diff_density_rms         0.095
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.033
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     961
_refine_ls_number_reflns         16825
_refine_ls_number_restraints     279
_refine_ls_restrained_S_all      1.031
_refine_ls_R_factor_all          0.0582
_refine_ls_R_factor_gt           0.0496
_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^)+(0.0720P)^2^+5.5350P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1301
_refine_ls_wR_factor_ref         0.1371
_reflns_Friedel_coverage         0.000
_reflns_number_gt                14436
_reflns_number_total             16825
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d2dt00996j2.cif
_cod_data_source_block           compound12
_cod_depositor_comments
'Adding full bibliography for 7710344--7710352.cif.'
_cod_database_code               7710347
_shelx_shelxl_version_number     2018/1
_chemical_oxdiff_formula         'C1 H1 P1 Ce1'
_shelx_estimated_absorpt_t_max   0.691
_shelx_estimated_absorpt_t_min   0.350
_reflns_odcompleteness_completeness 99.96
_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, All C(H,H,H,H,H,H) groups
2. Restrained distances
 C32-C34 \\sim C32A-C34 \\sim C32A-C35 \\sim C32-C28 \\sim C32A-C28 \\sim
C33A-C32A
 with sigma of 0.001
3. Uiso/Uaniso restraints and constraints
C32 \\sim C27: within 1.7A with sigma of 0.001 and sigma for terminal atoms of
0.002
C29A \\sim C30A \\sim C31 \\sim C27 \\sim C28 \\sim C27A \\sim C29 \\sim C30:
within 1.7A with sigma of 0.001 and sigma for terminal atoms of 0.002
C79 \\sim C85 \\sim C84 \\sim C83 \\sim C82 \\sim C81 \\sim C80: within 1.7A
with sigma of 0.001 and sigma for terminal atoms of 0.001
C32 \\sim C32A \\sim C33 \\sim C35 \\sim C34 \\sim C33A: within 1.7A with sigma
of 0.001 and sigma for terminal atoms of 0.002
C57 \\sim C55 \\sim C56 \\sim C58: within 1.7A with sigma of 0.001 and sigma
for terminal atoms of 0.002
C49 \\sim C52 \\sim C50 \\sim C51: within 1.7A with sigma of 0.001 and sigma
for terminal atoms of 0.002
C45 \\sim C42 \\sim C44 \\sim C43: within 1.7A with sigma of 0.001 and sigma
for terminal atoms of 0.002
Uanis(C81) \\sim Ueq, Uanis(C80) \\sim Ueq, Uanis(C79) \\sim Ueq, Uanis(C85)
\\sim Ueq, Uanis(C82) \\sim Ueq, Uanis(C83) \\sim Ueq, Uanis(C84) \\sim Ueq:
with sigma of 0.01 and sigma for terminal atoms of 0.01
4. Others
 Sof(C29A)=Sof(H29A)=Sof(C30A)=Sof(H30A)=1-FVAR(1)
 Sof(C30)=Sof(H30)=Sof(C29)=Sof(H29)=FVAR(1)
 Sof(C27A)=Sof(H27A)=1-FVAR(2)
 Sof(C27)=Sof(H27)=FVAR(2)
 Sof(C33A)=Sof(H33D)=Sof(H33E)=Sof(H33F)=1-FVAR(3)
 Sof(C33)=Sof(H33A)=Sof(H33B)=Sof(H33C)=FVAR(3)
 Sof(H35D)=Sof(H35E)=Sof(H35F)=Sof(H34D)=Sof(H34E)=Sof(H34F)=Sof(C32A)=1-FVAR(4)
 Sof(H35A)=Sof(H35B)=Sof(H35C)=Sof(H34A)=Sof(H34B)=Sof(H34C)=Sof(C32)=FVAR(4)
 Sof(Ce1A)=1-FVAR(5)
 Sof(Ce1)=FVAR(5)
 Sof(Ce2A)=1-FVAR(6)
 Sof(Ce2)=FVAR(6)
 Sof(Ce3A)=1-FVAR(7)
 Sof(Ce3)=FVAR(7)
5.a Ternary CH refined with riding coordinates:
 C29A(H29A), C30A(H30A), C27A(H27A)
5.b Aromatic/amide H refined with riding coordinates:
 C66(H66), C14(H14), C73(H73), C40(H40), C72(H72), C53(H53), C59(H59),
 C60(H60), C21(H21), C27(H27), C20(H20), C47(H47), C7(H7), C1(H1), C8(H8),
 C46(H46), C30(H30), C29(H29), C83(H83), C84(H84), C80(H80), C81(H81), C82(H82)
5.c Fitted hexagon refined as free rotating group:
 C83(C84,C79,C80,C81,C82)
5.d Idealised Me refined as rotating group:
 C24(H24A,H24B,H24C), C26(H26A,H26B,H26C), C5(H5A,H5B,H5C), C71(H71A,H71B,
 H71C), C18(H18A,H18B,H18C), C25(H25A,H25B,H25C), C37(H37A,H37B,H37C), C58(H58A,
 H58B,H58C), C69(H69A,H69B,H69C), C39(H39A,H39B,H39C), C76(H76A,H76B,H76C),
 C70(H70A,H70B,H70C), C35(H35A,H35B,H35C), C35(H35D,H35E,H35F), C65(H65A,H65B,
 H65C), C11(H11A,H11B,H11C), C6(H6A,H6B,H6C), C34(H34A,H34B,H34C), C34(H34D,
 H34E,H34F), C19(H19A,H19B,H19C), C63(H63A,H63B,H63C), C43(H43A,H43B,H43C),
 C78(H78A,H78B,H78C), C64(H64A,H64B,H64C), C38(H38A,H38B,H38C), C50(H50A,H50B,
 H50C), C77(H77A,H77B,H77C), C51(H51A,H51B,H51C), C12(H12A,H12B,H12C), C17(H17A,
 H17B,H17C), C56(H56A,H56B,H56C), C52(H52A,H52B,H52C), C44(H44A,H44B,H44C),
 C4(H4A,H4B,H4C), C45(H45A,H45B,H45C), C57(H57A,H57B,H57C), C13(H13A,H13B,H13C),
  C33(H33A,H33B,H33C), C85(H85A,H85B,H85C), C33A(H33D,H33E,H33F)
;
_olex2_date_sample_data_collection 2022-03-18
_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 2.465
_oxdiff_exptl_absorpt_empirical_full_min 0.586