Crystal structure of tris(dimethylamido-κ<i>N</i>)bis(dimethylamine-κ<i>N</i>)zirconium(IV) iodide
Clark, Wesley D.; Akurathi, Gopalakrishna; Valle, Henry U.; Hollis, T. Keith; Acta Crystallographica Section E 72 (2016) 73–75; doi:10.1107/S2056989015023919

data_2241438
_publ_section_title
;
 Crystal structure of
 tris(dimethylamido-\k<i>N</i>)bis(dimethylamine-\k<i>N</i>)zirconium(IV)
 iodide
;
_journal_coeditor_code           PK2563
_journal_issue                   1
_journal_name_full               'Acta Crystallographica Section E'
_journal_page_first              73
_journal_page_last               75
_journal_paper_doi               10.1107/S2056989015023919
_journal_volume                  72
_journal_year                    2016
_chemical_formula_iupac          '[Zr (C2 H6 N)3 (C2 H7 N)2] I'
_chemical_formula_moiety         'C10 H32 N5 Zr, I'
_chemical_formula_sum            'C10 H32 I N5 Zr'
_chemical_formula_weight         440.52
_chemical_name_systematic
;
Tris(dimethylamido-\k<i>N</i>)bis(dimethylamine-\k<i>N</i>)zirconium(IV) iodide
;
_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'
_symmetry_space_group_name_Hall  '-P 2ac 2ab'
_symmetry_space_group_name_H-M   'P b c a'
_atom_sites_solution_hydrogens   geom
_audit_creation_method
;
Olex2 1.2
(compiled 2015.01.26 svn.r3150 for OlexSys, GUI svn.r4998)
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   14.2425(3)
_cell_length_b                   15.4113(3)
_cell_length_c                   16.8537(3)
_cell_measurement_reflns_used    9970
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      26.029
_cell_measurement_theta_min      2.292
_cell_volume                     3699.31(12)
_computing_cell_refinement
;
SAINT (Bruker, 2013)
;
_computing_data_collection
;
APEX2 (Bruker, 2013)
;
_computing_data_reduction
;
SAINT (Bruker, 2013)
;
_computing_molecular_graphics
;
<i>OLEX2</i> (Dolomanov <i>et al.</i>, 2009) and Mercury
(Macrae <i>et al.</i>, 2006)
;
_computing_publication_material
;
publCIF (Westrip, 2010)
;
_computing_structure_refinement
;
SHELXL (Sheldrick, 2008)
;
_computing_structure_solution
;
SHELXS (Sheldrick, 2008)
;
_diffrn_ambient_temperature      100.01
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.995
_diffrn_measurement_device_type  'Bruker APEXII CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0265
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            29665
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         26.029
_diffrn_reflns_theta_min         2.292
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    2.256
_exptl_absorpt_correction_T_max  0.7453
_exptl_absorpt_correction_T_min  0.6563
_exptl_absorpt_correction_type   numerical
_exptl_absorpt_process_details
;
(SADABS; Bruker, 2014)
;
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.582
_exptl_crystal_description       tablet
_exptl_crystal_F_000             1760
_exptl_crystal_size_max          0.2
_exptl_crystal_size_mid          0.1
_exptl_crystal_size_min          0.1
_refine_diff_density_max         0.333
_refine_diff_density_min         -0.339
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.067
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     154
_refine_ls_number_reflns         3620
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.067
_refine_ls_R_factor_all          0.0173
_refine_ls_R_factor_gt           0.0146
_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^)+(0.0158P)^2^+1.6295P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0351
_refine_ls_wR_factor_ref         0.0363
_reflns_number_gt                3319
_reflns_number_total             3620
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            pk2563sup1.cif
_cod_data_source_block           I
_cod_depositor_comments
;Adding full bibliography for 2241438.cif.

 Adding full bibliography for 2241438.cif.
;
_cod_database_code               2241438
_cod_database_fobs_code          2241438