Cooperative Trimerization of Carbon Monoxide by Lithium and Samarium Boryls.
Wang, Baoli; Luo, Gen; Nishiura, Masayoshi; Luo, Yi; Hou, Zhaomin; Journal of the American Chemical Society  (2017) –; doi:10.1021/jacs.7b10108

data_4126714
_publ_section_title
;
 Cooperative Trimerization of Carbon Monoxide by Lithium and Samarium
 Boryls.
;
_journal_name_full               'Journal of the American Chemical Society'
_journal_paper_doi               10.1021/jacs.7b10108
_journal_year                    2017
_chemical_formula_sum            'C84 H128 B2 Li2 N4 O11'
_chemical_formula_weight         1405.40
_chemical_name_common            {[(Boryl)2(C4O4)]Li2(THF)4}
_space_group_crystal_system      monoclinic
_space_group_IT_number           9
_space_group_name_Hall           'C -2yc'
_space_group_name_H-M_alt        'C 1 c 1'
_symmetry_space_group_name_Hall  'C -2yc'
_symmetry_space_group_name_H-M   'C 1 c 1'
_atom_sites_solution_hydrogens   geom
_audit_creation_method           SHELXL-2014/7
_cell_angle_alpha                90
_cell_angle_beta                 103.137(5)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   10.5952(5)
_cell_length_b                   38.7321(17)
_cell_length_c                   20.7110(11)
_cell_measurement_reflns_used    268
_cell_measurement_temperature    173(2)
_cell_measurement_theta_max      25
_cell_measurement_theta_min      2
_cell_volume                     8276.8(7)
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_diffrn_ambient_temperature      173(2)
_diffrn_measured_fraction_theta_full 0.985
_diffrn_measured_fraction_theta_max 0.985
_diffrn_measurement_device_type  'RIGAKU XtaLAB-P200'
_diffrn_measurement_method       'phi and omega scan'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0441
_diffrn_reflns_av_unetI/netI     0.0744
_diffrn_reflns_Laue_measured_fraction_full 0.985
_diffrn_reflns_Laue_measured_fraction_max 0.985
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       36
_diffrn_reflns_limit_k_min       -46
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_limit_l_min       -24
_diffrn_reflns_number            22792
_diffrn_reflns_point_group_measured_fraction_full 0.823
_diffrn_reflns_point_group_measured_fraction_max 0.823
_diffrn_reflns_theta_full        25.028
_diffrn_reflns_theta_max         25.028
_diffrn_reflns_theta_min         2.043
_exptl_absorpt_coefficient_mu    0.072
_exptl_absorpt_correction_T_max  0.978
_exptl_absorpt_correction_T_min  0.475
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_process_details   SADABS
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.128
_exptl_crystal_description       plate
_exptl_crystal_F_000             3056
_exptl_crystal_size_max          0.400
_exptl_crystal_size_mid          0.400
_exptl_crystal_size_min          0.350
_refine_diff_density_max         0.477
_refine_diff_density_min         -0.414
_refine_diff_density_rms         0.132
_refine_ls_abs_structure_details
;
 Flack x determined using 2854 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   0.2(8)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.040
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     906
_refine_ls_number_reflns         12040
_refine_ls_number_restraints     5
_refine_ls_restrained_S_all      1.041
_refine_ls_R_factor_all          0.1252
_refine_ls_R_factor_gt           0.0883
_refine_ls_shift/su_max          0.009
_refine_ls_shift/su_mean         0.001
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.1847P)^2^+3.0074P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2407
_refine_ls_wR_factor_ref         0.2720
_reflns_Friedel_coverage         0.669
_reflns_Friedel_fraction_full    0.660
_reflns_Friedel_fraction_max     0.660
_reflns_number_gt                8344
_reflns_number_total             12040
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ja7b10108_si_001.cif
_cod_data_source_block           5
_cod_database_code               4126714
_shelx_shelxl_version_number     2014/7
_shelx_estimated_absorpt_t_min   0.972
_shelx_estimated_absorpt_t_max   0.975
_shelx_res_checksum              58587
_shelx_hkl_checksum              9708