Synthesis and reactivity of a tris(carbene) zinc chloride complex
Sherbow, Tobias J.; Li, Keyan; Zakharov, Lev N.; Pluth, Michael D.; Dalton Transactions  (2022) –; doi:10.1039/D2DT02809C

data_7711210
_publ_section_title
;
 Synthesis and reactivity of a tris(carbene) zinc chloride complex
;
_journal_name_full               'Dalton Transactions'
_journal_paper_doi               10.1039/D2DT02809C
_journal_year                    2022
_chemical_formula_sum            'C32 H49 B N6 O1.25 S4 Zn'
_chemical_formula_weight         742.19
_space_group_crystal_system      orthorhombic
_space_group_IT_number           61
_space_group_name_Hall           '-P 2ac 2ab'
_space_group_name_H-M_alt        'P b c a'
_atom_sites_solution_hydrogens   geom
_audit_creation_method           SHELXL-2014/7
_audit_update_record
;
2022-08-28 deposited with the CCDC.	2022-08-30 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            16
_cell_length_a                   18.5324(14)
_cell_length_b                   19.6563(15)
_cell_length_c                   41.276(3)
_cell_measurement_reflns_used    1685
_cell_measurement_temperature    173(2)
_cell_measurement_theta_max      39.18
_cell_measurement_theta_min      3.20
_cell_volume                     15036.0(19)
_computing_cell_refinement       'Bruker SAINT'
_computing_data_collection       'Bruker APEX2'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_structure_solution    'SHELXS-97 (Sheldrick 2008)'
_diffrn_ambient_temperature      173(2)
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device_type  'Bruker Apex II CCD'
_diffrn_measurement_method       '\w and \f scans'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54178
_diffrn_reflns_av_R_equivalents  0.1566
_diffrn_reflns_av_unetI/netI     0.1295
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       38
_diffrn_reflns_limit_l_min       -40
_diffrn_reflns_number            42179
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_theta_full        49.811
_diffrn_reflns_theta_max         49.811
_diffrn_reflns_theta_min         2.141
_diffrn_source                   'Incoatec I\mS'
_exptl_absorpt_coefficient_mu    3.250
_exptl_absorpt_correction_T_max  0.7498
_exptl_absorpt_correction_T_min  0.6483
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   SADABS
_exptl_crystal_colour            'light yellow'
_exptl_crystal_density_diffrn    1.311
_exptl_crystal_description       cut-block
_exptl_crystal_F_000             6272
_exptl_crystal_size_max          0.020
_exptl_crystal_size_mid          0.010
_exptl_crystal_size_min          0.010
_platon_squeeze_details
;
Solvent THF molecule (C4H8O, 40 electron) is highly disordered 
aound an inversion center and was treated by SQUEEZE.
;
_refine_diff_density_max         0.592
_refine_diff_density_min         -0.470
_refine_diff_density_rms         0.086
_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     740
_refine_ls_number_reflns         7645
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.023
_refine_ls_R_factor_all          0.1304
_refine_ls_R_factor_gt           0.0759
_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^)+(0.0998P)^2^+26.0928P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1827
_refine_ls_wR_factor_ref         0.2145
_reflns_Friedel_coverage         0.000
_reflns_number_gt                4642
_reflns_number_total             7645
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d2dt02809c2.cif
_cod_data_source_block           cu_tjs49_0m_a_sq
_cod_original_cell_volume        15035.8(19)
_cod_database_code               7711210
_shelx_shelxl_version_number     2014/7
_shelx_estimated_absorpt_t_min   0.938
_shelx_estimated_absorpt_t_max   0.968
_platon_squeeze_void_probe_radius 1.20
_shelx_res_checksum              37340
_shelx_fab_checksum              68808