Isolation and Structural Characterization of Geminal Di(iodozincio)methane Complexes Stabilized with Nitrogen Ligands.
Nishida, Yusuke; Hosokawa, Naoki; Murai, Masahito; Takai, Kazuhiko; Journal of the American Chemical Society 137 (2015) 114–117; doi:10.1021/ja5114535

data_4123326
_publ_section_title
;
 Isolation and Structural Characterization of Geminal
 Di(iodozincio)methane Complexes Stabilized with Nitrogen Ligands.
;
_journal_issue                   1
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              114
_journal_page_last               117
_journal_paper_doi               10.1021/ja5114535
_journal_volume                  137
_journal_year                    2015
_chemical_formula_moiety         'C40 H40 Cl2 I2 N4 Zn2'
_chemical_formula_sum            'C40 H40 Cl2 I2 N4 Zn2'
_chemical_formula_weight         1032.26
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_symmetry_Int_Tables_number      2
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_cell_angle_alpha                105.017(4)
_cell_angle_beta                 93.698(4)
_cell_angle_gamma                90.313(3)
_cell_formula_units_Z            2
_cell_length_a                   11.879(3)
_cell_length_b                   13.183(3)
_cell_length_c                   13.847(4)
_cell_measurement_reflns_used    6397
_cell_measurement_temperature    113
_cell_measurement_theta_max      27.50
_cell_measurement_theta_min      3.10
_cell_volume                     2089.5(9)
_computing_cell_refinement       'CrystalClear-SM Expert 2.0 r16'
_computing_data_collection
'CrystalClear-SM Expert 2.0 r16 (Rigaku, 2014)'
_computing_data_reduction        'CrystalClear-SM Expert 2.0 r16'
_computing_molecular_graphics    'CrystalStructure 4.0'
_computing_publication_material  'CrystalStructure 4.0 (Rigaku, 2010)'
_computing_structure_refinement  'SHELXL97 (Sheldrick, 2008)'
_computing_structure_solution    'SIR92 (Altomare, et al., 1994)'
_diffrn_ambient_temperature      113
_diffrn_detector_area_resol_mean 7.111
_diffrn_measured_fraction_theta_full 0.992
_diffrn_measured_fraction_theta_max 0.992
_diffrn_measurement_device_type  'Rigaku Saturn724'
_diffrn_measurement_method       \w
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71075
_diffrn_reflns_av_R_equivalents  0.0349
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            32881
_diffrn_reflns_theta_full        27.48
_diffrn_reflns_theta_max         27.48
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    2.786
_exptl_absorpt_correction_T_max  0.716
_exptl_absorpt_correction_T_min  0.644
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'REQAB (Rigaku, 1998)'
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.641
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             1016.00
_exptl_crystal_size_max          0.150
_exptl_crystal_size_mid          0.150
_exptl_crystal_size_min          0.120
_refine_diff_density_max         1.510
_refine_diff_density_min         -1.560
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.086
_refine_ls_hydrogen_treatment    constr
_refine_ls_number_parameters     453
_refine_ls_number_reflns         9503
_refine_ls_number_restraints     0
_refine_ls_R_factor_gt           0.0470
_refine_ls_shift/su_max          0.001
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w = 1/[\s^2^(Fo^2^)+(0.0760P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_ref         0.1291
_reflns_number_gt                8027
_reflns_number_total             9503
_reflns_threshold_expression     F^2^>2.0\s(F^2^)
_cod_data_source_file            ja5114535_si_003.cif
_cod_data_source_block           1
_cod_original_cell_volume        2089.5(10)
_cod_database_code               4123326