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_4126712
_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            'C43 H68 B Cl3 Li N2 O5 Sm'
_chemical_formula_weight         967.44
_chemical_name_common            {(Boryl)Sm[C(O)]Cl2(THF)2LiCl(THF)2}
_space_group_crystal_system      orthorhombic
_space_group_IT_number           19
_space_group_name_Hall           'P 2ac 2ab'
_space_group_name_H-M_alt        'P 21 21 21'
_symmetry_space_group_name_Hall  'P 2ac 2ab'
_symmetry_space_group_name_H-M   'P 21 21 21'
_atom_sites_solution_hydrogens   geom
_audit_creation_method           SHELXL-2014/7
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   10.858(4)
_cell_length_b                   12.779(5)
_cell_length_c                   35.995(11)
_cell_measurement_reflns_used    236
_cell_measurement_temperature    173(2)
_cell_measurement_theta_max      25
_cell_measurement_theta_min      2
_cell_volume                     4994(3)
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_diffrn_ambient_temperature      173(2)
_diffrn_measured_fraction_theta_full 0.995
_diffrn_measured_fraction_theta_max 0.995
_diffrn_measurement_device_type  'Diffractometer with a CMOS area detector'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0628
_diffrn_reflns_av_unetI/netI     0.0273
_diffrn_reflns_Laue_measured_fraction_full 0.995
_diffrn_reflns_Laue_measured_fraction_max 0.995
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       42
_diffrn_reflns_limit_l_min       -42
_diffrn_reflns_number            97422
_diffrn_reflns_point_group_measured_fraction_full 0.994
_diffrn_reflns_point_group_measured_fraction_max 0.994
_diffrn_reflns_theta_full        25.071
_diffrn_reflns_theta_max         25.071
_diffrn_reflns_theta_min         1.691
_diffrn_source                   'microfocus sealed tube'
_exptl_absorpt_coefficient_mu    1.376
_exptl_absorpt_correction_T_max  0.75
_exptl_absorpt_correction_T_min  0.68
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   SADABS
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    1.287
_exptl_crystal_description       block
_exptl_crystal_F_000             2004
_exptl_crystal_size_max          0.300
_exptl_crystal_size_mid          0.200
_exptl_crystal_size_min          0.200
_refine_diff_density_max         1.263
_refine_diff_density_min         -0.844
_refine_diff_density_rms         0.063
_refine_ls_abs_structure_details
;
 Flack x determined using 3601 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   0.070(4)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.155
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     531
_refine_ls_number_reflns         8793
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.155
_refine_ls_R_factor_all          0.0320
_refine_ls_R_factor_gt           0.0308
_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^)+(0.0374P)^2^+2.9499P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0778
_refine_ls_wR_factor_ref         0.0783
_reflns_Friedel_coverage         0.784
_reflns_Friedel_fraction_full    0.993
_reflns_Friedel_fraction_max     0.993
_reflns_number_gt                8551
_reflns_number_total             8793
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ja7b10108_si_001.cif
_cod_data_source_block           3
_cod_database_code               4126712
_shelx_shelxl_version_number     2014/7
_shelx_estimated_absorpt_t_min   0.683
_shelx_estimated_absorpt_t_max   0.770
_shelx_res_checksum              95740
_shelx_hkl_checksum              23454