Synthesis and Structures of Zirconium Amide-Iodide Complexes
Jean-Sébastien M. Lehn; David M. Hoffman; Inorganic Chemistry 41 (2002) 4063–4067; doi:10.1021/ic025630b

data_4318295
_publ_section_title
;
 Synthesis and Structures of Zirconium Amide-Iodide Complexes
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              4063
_journal_page_last               4067
_journal_paper_doi               10.1021/ic025630b
_journal_volume                  41
_journal_year                    2002
_chemical_formula_sum            'C16 H40 I4 N4 Zr2'
_chemical_formula_weight         978.56
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 100.440(10)
_cell_angle_gamma                90.00
_cell_formula_units_Z            2
_cell_length_a                   8.149(2)
_cell_length_b                   13.480(3)
_cell_length_c                   14.420(3)
_cell_measurement_reflns_used    30
_cell_measurement_temperature    223(2)
_cell_measurement_theta_max      15.0
_cell_measurement_theta_min      7.5
_cell_volume                     1557.8(6)
_computing_cell_refinement       'Bruker XSCANS'
_computing_data_collection       'Bruker XSCANS'
_computing_data_reduction        'Bruker XSCANS'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      223(2)
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device_type  'Siemens P4'
_diffrn_measurement_method       '2\q/\w scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0203
_diffrn_reflns_av_sigmaI/netI    0.0340
_diffrn_reflns_limit_h_max       8
_diffrn_reflns_limit_h_min       -8
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_number            2310
_diffrn_reflns_theta_full        22.49
_diffrn_reflns_theta_max         22.49
_diffrn_reflns_theta_min         2.08
_diffrn_standards_decay_%        0.0
_diffrn_standards_interval_count 97
_diffrn_standards_interval_time  120
_diffrn_standards_number         3
_exptl_absorpt_coefficient_mu    4.641
_exptl_absorpt_correction_T_max  0.8533
_exptl_absorpt_correction_T_min  0.7639
_exptl_absorpt_correction_type   Semi-empirical
_exptl_crystal_colour            'Pale yellow'
_exptl_crystal_density_diffrn    2.086
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       Column
_exptl_crystal_F_000             912
_exptl_crystal_size_max          0.30
_exptl_crystal_size_mid          0.10
_exptl_crystal_size_min          0.08
_refine_diff_density_max         0.628
_refine_diff_density_min         -0.691
_refine_diff_density_rms         0.114
_refine_ls_extinction_coef       0.00026(13)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     SHELXL
_refine_ls_goodness_of_fit_ref   1.032
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     119
_refine_ls_number_reflns         2023
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.032
_refine_ls_R_factor_all          0.0380
_refine_ls_R_factor_gt           0.0268
_refine_ls_shift/su_max          0.017
_refine_ls_shift/su_mean         0.003
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0237P)^2^+7.6700P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0694
_refine_ls_wR_factor_ref         0.0729
_reflns_number_gt                1739
_reflns_number_total             2131
_reflns_threshold_expression     >4sigma(I)
_cod_data_source_file            ic025630b_s1_2.cif
_cod_data_source_block           k402[Zr(NEt2)2I2]2
_cod_database_code               4318295