Thorium(iv) alkyl and allyl complexes of a rigid NON-donor pincer ligand with flanking 1-adamantyl substituents.
Andreychuk, Nicholas R.; Dickie, Tara; Emslie, David J. H.; Jenkins, Hilary A.; Dalton transactions (Cambridge, England : 2003) 47 (2018) 4866–4876; doi:10.1039/c8dt00421h

data_7045863
_publ_section_title
;
 Thorium(iv) alkyl and allyl complexes of a rigid NON-donor pincer ligand
 with flanking 1-adamantyl substituents.
;
_journal_issue                   14
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              4866
_journal_page_last               4876
_journal_paper_doi               10.1039/c8dt00421h
_journal_volume                  47
_journal_year                    2018
_chemical_formula_moiety         'C67 H106 K2 N2 O7'
_chemical_formula_sum            'C67 H106 K2 N2 O7'
_chemical_formula_weight         1129.73
_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'
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_audit_creation_date             2018-01-31
_audit_creation_method
;
Olex2 1.2
(compiled 2017.08.10 svn.r3458 for OlexSys, GUI svn.r5381)
;
_audit_update_record
;
2018-01-31 deposited with the CCDC.
2018-03-06 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 100.230(2)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   17.088(2)
_cell_length_b                   17.455(2)
_cell_length_c                   21.803(3)
_cell_measurement_reflns_used    9895
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      2.33
_cell_measurement_theta_min      26.20
_cell_volume                     6399.8(14)
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'XL (Sheldrick, 2008)'
_computing_structure_solution    'ShelXT (Sheldrick, 2015)'
_diffrn_ambient_temperature      100.15
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.995
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.1092
_diffrn_reflns_av_unetI/netI     0.0880
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.995
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_h_min       -21
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -21
_diffrn_reflns_limit_l_max       27
_diffrn_reflns_limit_l_min       -27
_diffrn_reflns_number            70975
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.995
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         26.533
_diffrn_reflns_theta_min         1.681
_exptl_absorpt_coefficient_mu    0.200
_exptl_absorpt_correction_T_max  0.9588
_exptl_absorpt_correction_T_min  0.9292
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   SADABS
_exptl_crystal_colour            colourless
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.172
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             2464
_exptl_crystal_size_max          0.372
_exptl_crystal_size_mid          0.33
_exptl_crystal_size_min          0.212
_refine_diff_density_max         0.414
_refine_diff_density_min         -0.496
_refine_diff_density_rms         0.068
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.023
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     703
_refine_ls_number_reflns         13246
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.023
_refine_ls_R_factor_all          0.1193
_refine_ls_R_factor_gt           0.0605
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0686P)^2^+2.2718P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1363
_refine_ls_wR_factor_ref         0.1629
_reflns_Friedel_coverage         0.000
_reflns_number_gt                7808
_reflns_number_total             13246
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c8dt00421h2.cif
_cod_data_source_block           nra_5
_cod_depositor_comments
'Adding full bibliography for 7045861--7045863.cif.'
_cod_original_cell_volume        6400.1(15)
_cod_database_code               7045863
_shelx_shelxl_version_number     2016/6
_shelx_estimated_absorpt_t_max   0.959
_shelx_estimated_absorpt_t_min   0.929
_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.a Ternary CH refined with riding coordinates:
 C42(H42), C30(H30), C32(H32), C28(H28), C38(H38), C40(H40)
2.b Secondary CH2 refined with riding coordinates:
 C25(H25A,H25B), C35(H35A,H35B), C27(H27A,H27B), C37(H37A,H37B), C26(H26A,
 H26B), C29(H29A,H29B), C33(H33A,H33B), C36(H36A,H36B), C43(H43A,H43B),
 C39(H39A,H39B), C31(H31A,H31B), C50(H50A,H50B), C41(H41A,H41B), C64(H64A,H64B),
  C49(H49A,H49B), C54(H54A,H54B), C67(H67A,H67B), C52(H52A,H52B), C53(H53A,
 H53B), C57(H57A,H57B), C48(H48A,H48B), C51(H51A,H51B), C60(H60A,H60B),
 C46(H46A,H46B), C65(H65A,H65B), C55(H55A,H55B), C63(H63A,H63B), C56(H56A,H56B),
  C59(H59A,H59B), C45(H45A,H45B), C58(H58A,H58B), C47(H47A,H47B), C62(H62A,
 H62B), C44(H44A,H44B), C61(H61A,H61B), C66(H66A,H66B)
2.c Me refined with riding coordinates:
 C19(H19A,H19B,H19C), C23(H23A,H23B,H23C), C21(H21A,H21B,H21C), C17(H17A,H17B,
 H17C), C18(H18A,H18B,H18C), C14(H14A,H14B,H14C), C22(H22A,H22B,H22C), C15(H15A,
 H15B,H15C)
2.d Aromatic/amide H refined with riding coordinates:
 C6(H6), C3(H3), C1(H1), C8(H8)
;
_shelx_res_checksum              3783
_olex2_submission_special_instructions 'No special instructions were received'