Monomeric 16-Electron π-Diborene Complexes of Zn(II) and Cd(II).
Wang, Sunewang R.; Arrowsmith, Merle; Braunschweig, Holger; Dewhurst, Rian D.; Dömling, Michael; Mattock, James D.; Pranckevicius, Conor; Vargas, Alfredo; Journal of the American Chemical Society 139 (2017) 10661–10664; doi:10.1021/jacs.7b06644

data_4131538
_publ_section_title
;
 Monomeric 16-Electron \p-Diborene Complexes of Zn(II) and Cd(II).
;
_journal_issue                   31
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              10661
_journal_page_last               10664
_journal_paper_doi               10.1021/jacs.7b06644
_journal_volume                  139
_journal_year                    2017
_chemical_formula_moiety         'C18 H22 B2 Cl2 N4 S2 Zn, C H2 Cl2'
_chemical_formula_sum            'C19 H24 B2 Cl4 N4 S2 Zn'
_chemical_formula_weight         601.33
_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'
_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                   9.5859(9)
_cell_length_b                   12.2845(10)
_cell_length_c                   24.092(3)
_cell_measurement_reflns_used    9492
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      23.95
_cell_measurement_theta_min      2.29
_cell_volume                     2837.0(5)
_computing_cell_refinement       'Saint+ ver. 7.68A (Bruker AXS)'
_computing_data_collection       'APEX2 ver. 2014.9 (Bruker AXS)'
_computing_data_reduction        'Saint+ ver. 7.68A (Bruker AXS)'
_computing_molecular_graphics    'ShelXLe (Huebschle et all, 2011)'
_computing_publication_material  'SHELXL-2014/6 (Sheldrick, 2014) '
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_structure_solution    'SHELXT 2014/4 (Sheldrick, 2014)'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 0.996
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measurement_device_type  'Photon Quest'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0774
_diffrn_reflns_av_unetI/netI     0.0551
_diffrn_reflns_Laue_measured_fraction_full 0.996
_diffrn_reflns_Laue_measured_fraction_max 0.997
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       30
_diffrn_reflns_limit_l_min       -27
_diffrn_reflns_number            43110
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_theta_full        26.000
_diffrn_reflns_theta_max         27.101
_diffrn_reflns_theta_min         2.825
_diffrn_source
'rotating-anode X-ray tube or sealed X-ray tube'
_exptl_absorpt_coefficient_mu    1.404
_exptl_absorpt_correction_T_max  0.7455
_exptl_absorpt_correction_T_min  0.6157
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'Sadabs 2014/4 (Bruker 2014)'
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.408
_exptl_crystal_description       block
_exptl_crystal_F_000             1224
_exptl_crystal_size_max          0.258
_exptl_crystal_size_mid          0.252
_exptl_crystal_size_min          0.206
_refine_diff_density_max         0.712
_refine_diff_density_min         -0.368
_refine_diff_density_rms         0.087
_refine_ls_abs_structure_details
;
 Flack x determined using 1989 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   0.021(7)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.064
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     480
_refine_ls_number_reflns         6249
_refine_ls_number_restraints     496
_refine_ls_restrained_S_all      1.045
_refine_ls_R_factor_all          0.0593
_refine_ls_R_factor_gt           0.0447
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0569P)^2^+2.0740P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1049
_refine_ls_wR_factor_ref         0.1112
_reflns_Friedel_coverage         0.775
_reflns_Friedel_fraction_full    1.000
_reflns_Friedel_fraction_max     1.000
_reflns_number_gt                5343
_reflns_number_total             6249
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ja7b06644_si_005.cif
_cod_data_source_block           final_a
_cod_database_code               4131538
_shelx_shelxl_version_number     2014/7
_shelx_estimated_absorpt_t_min   0.713
_shelx_estimated_absorpt_t_max   0.761
_exptl_absorpt_special_details
;The crystal was immersed in a film of perfluoropolyether oil, 
mounted on a a glass fiber and transferred to stream of cold nitrogen.
;
_shelx_res_checksum              59327
_shelx_hkl_checksum              48918