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_4318296
_publ_section_title
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 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            'C8 H20 I6 N2 Zr2'
_chemical_formula_weight         1088.10
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_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
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.323(2)
_cell_angle_beta                 106.820(2)
_cell_angle_gamma                108.206(2)
_cell_formula_units_Z            1
_cell_length_a                   7.1219(8)
_cell_length_b                   7.6193(8)
_cell_length_c                   11.7175(12)
_cell_measurement_reflns_used    2364
_cell_measurement_temperature    223(2)
_cell_measurement_theta_max      23.28
_cell_measurement_theta_min      2.83
_cell_volume                     574.93(11)
_computing_cell_refinement       'Siemens SAINT software (Siemens, 1996)'
_computing_data_collection       'Siemens SMART software (Siemens, 1996)'
_computing_data_reduction        'Siemens SAINT software (Siemens, 1996)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      223(2)
_diffrn_detector_area_resol_mean 1K
_diffrn_measured_fraction_theta_full 0.989
_diffrn_measured_fraction_theta_max 0.989
_diffrn_measurement_device_type  'Siemens SMART CCD'
_diffrn_measurement_method       CCD
_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  0.0340
_diffrn_reflns_av_sigmaI/netI    0.0313
_diffrn_reflns_limit_h_max       7
_diffrn_reflns_limit_h_min       -7
_diffrn_reflns_limit_k_max       8
_diffrn_reflns_limit_k_min       -8
_diffrn_reflns_limit_l_max       13
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_number            2609
_diffrn_reflns_theta_full        23.28
_diffrn_reflns_theta_max         23.28
_diffrn_reflns_theta_min         2.83
_diffrn_standards_decay_%        0.0
_exptl_absorpt_coefficient_mu    8.951
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.3849
_exptl_absorpt_correction_type   empirical
_exptl_crystal_colour            Orange
_exptl_crystal_density_diffrn    3.143
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       'Thin plate'
_exptl_crystal_F_000             480
_exptl_crystal_size_max          0.30
_exptl_crystal_size_mid          0.18
_exptl_crystal_size_min          0.06
_refine_diff_density_max         1.242
_refine_diff_density_min         -0.818
_refine_diff_density_rms         0.182
_refine_ls_extinction_coef       0.0040(5)
_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   1.126
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     83
_refine_ls_number_reflns         1640
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.126
_refine_ls_R_factor_all          0.0293
_refine_ls_R_factor_gt           0.0273
_refine_ls_shift/su_max          0.010
_refine_ls_shift/su_mean         0.003
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0382P)^2^+2.8208P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0743
_refine_ls_wR_factor_ref         0.0765
_reflns_number_gt                1554
_reflns_number_total             1641
_reflns_threshold_expression     >4sigma(I)
_cod_data_source_file            ic025630b_s1_3.cif
_cod_data_source_block           k417[Zr(NEt2)I3]2
_cod_depositor_comments
;
The following automatic conversions were performed:

'_symmetry_cell_setting' value 'Triclinic' changed to 'triclinic'
according to the built-in table from CIF Core dictionary named
'cif_core.dic' version 2.4.1 from
2010-06-29.

'_exptl_absorpt_correction_type' value 'Empirical'
changed to 'empirical' according to the built-in table from CIF Core
dictionary named 'cif_core.dic' version 2.4.1 from 2010-06-29.

Automatic conversion script
Id: cif_fix_values 1646 2011-03-28 12:23:43Z adriana 
;
_cod_database_code               4318296