Reversible addition and hydrogenation of 1,1-diphenylethylene with a barium complex.
Shi, Xianghui; Cheng, Jianhua; Dalton transactions (Cambridge, England : 2003) 48 (2019) 8565–8568; doi:10.1039/c9dt01874c

data_7700076
_publ_section_title
;
 Reversible addition and hydrogenation of 1,1-diphenylethylene with a
 barium complex.
;
_journal_issue                   24
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              8565
_journal_page_last               8568
_journal_paper_doi               10.1039/c9dt01874c
_journal_volume                  48
_journal_year                    2019
_chemical_formula_sum            'C62 H83 B Ba N6'
_chemical_formula_weight         1060.49
_chemical_name_common            '[TpBa(CH3Ph2)]'
_chemical_properties_physical    Air-sensitive,Moisture-sensitive
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   mixed
_audit_creation_method           SHELXL-2018/3
_audit_update_record
;
2018-08-21 deposited with the CCDC.    2019-05-24 downloaded from the CCDC.
;
_cell_angle_alpha                90.219(2)
_cell_angle_beta                 101.569(2)
_cell_angle_gamma                104.232(3)
_cell_formula_units_Z            2
_cell_length_a                   12.3228(19)
_cell_length_b                   15.352(3)
_cell_length_c                   17.272(3)
_cell_measurement_reflns_used    3914
_cell_measurement_temperature    193(2)
_cell_measurement_theta_max      23.13
_cell_measurement_theta_min      2.32
_cell_volume                     3098.0(9)
_computing_structure_refinement  'SHELXL-2018/3 (Sheldrick, 2018)'
_diffrn_ambient_temperature      193(2)
_diffrn_measured_fraction_theta_full 0.970
_diffrn_measured_fraction_theta_max 0.970
_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  0.0436
_diffrn_reflns_av_unetI/netI     0.0949
_diffrn_reflns_Laue_measured_fraction_full 0.970
_diffrn_reflns_Laue_measured_fraction_max 0.970
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       10
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            15398
_diffrn_reflns_point_group_measured_fraction_full 0.970
_diffrn_reflns_point_group_measured_fraction_max 0.970
_diffrn_reflns_theta_full        25.000
_diffrn_reflns_theta_max         25.000
_diffrn_reflns_theta_min         1.774
_exptl_absorpt_coefficient_mu    0.680
_exptl_absorpt_correction_T_max  1
_exptl_absorpt_correction_T_min  0.6447
_exptl_absorpt_correction_type   empirical
_exptl_crystal_colour            Red
_exptl_crystal_density_diffrn    1.137
_exptl_crystal_description       Block
_exptl_crystal_F_000             1116
_exptl_crystal_recrystallization_method
'Re-crystallisation from solvent: Hexane'
_exptl_crystal_size_max          0.230
_exptl_crystal_size_mid          0.170
_exptl_crystal_size_min          0.120
_platon_squeeze_details
;
One disorder hexane molecule per formual unit of [TpBa(CH3Ph2)]
was not modelled and the disordered density was taken into account
using the SQUEEZE/PLATON procedure.(Sluis, P. van der; Spek, A. L. Acta Crystallogr.
1990, A46, 194?01) as implemented in PLATON (Spek, A.L. Acta
Crystallogr. 1990, A46, C34; Spek, A.L. J. Appl. Cryst. 2003, 36, 7?3.
PLATON - a multipurpose crystallographic tool.  Utrecht University,
Utrecht, The Netherlands). 
;
_refine_diff_density_max         2.044
_refine_diff_density_min         -1.048
_refine_diff_density_rms         0.124
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.953
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     607
_refine_ls_number_reflns         10595
_refine_ls_number_restraints     102
_refine_ls_restrained_S_all      0.956
_refine_ls_R_factor_all          0.0989
_refine_ls_R_factor_gt           0.0709
_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^)+(0.1205P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1711
_refine_ls_wR_factor_ref         0.1873
_reflns_Friedel_coverage         0.000
_reflns_number_gt                7535
_reflns_number_total             10595
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c9dt01874c2.cif
_cod_data_source_block           C121
_cod_depositor_comments
'Adding full bibliography for 7700075--7700076.cif.'
_cod_original_cell_volume        3098.0(8)
_cod_database_code               7700076
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_min   0.859
_shelx_estimated_absorpt_t_max   0.923
_shelx_res_checksum              37733