{<i>N</i>,<i>N</i>-Bis[2-(trimethylsilylamino)ethyl]-<i>N</i>'-(trimethylsilyl)ethane-1,2-diaminato(3‒)-κ^4^<i>N</i>}methylzirconium(IV)
MacMillan, Samantha N.; Tanski, Joseph M.; Waterman, Rory; Acta Crystallographica Section E 64 (2008) m477–; doi:10.1107/S160053680800425X

data_2217784
_publ_section_title
{<i>N</i>,<i>N</i>-Bis[2-(trimethylsilylamino)ethyl]-<i>N</i>'-(trimethylsilyl)ethane-1,2-diaminato(3--)-\k^4^<i>N</i>}methylzirconium(IV)
_journal_coeditor_code           HG2378
_journal_issue                   3
_journal_name_full               'Acta Crystallographica Section E'
_journal_page_first              m477
_journal_paper_doi               10.1107/S160053680800425X
_journal_volume                  64
_journal_year                    2008
_chemical_formula_iupac          '[Zr (C H3) (C15 H39 N4 Si3)]'
_chemical_formula_moiety         'C16 H42 N4 Si3 Zr'
_chemical_formula_sum            'C16 H42 N4 Si3 Zr'
_chemical_formula_weight         466.03
_chemical_melting_point          362
_chemical_name_systematic
;
{N,N-Bis[2-(trimethylsilylamino)ethyl]-N'-(trimethylsilyl)ethane-1,2-
diaminato(3-)-\k^4^<i>N</i>}methylzirconium(IV)
;
_space_group_IT_number           61
_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_Hall  '-P 2ac 2ab'
_symmetry_space_group_name_H-M   'P b c a'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                90.00
_cell_formula_units_Z            8
_cell_length_a                   15.6018(7)
_cell_length_b                   18.0682(8)
_cell_length_c                   18.3745(8)
_cell_measurement_reflns_used    9832
_cell_measurement_temperature    125(2)
_cell_measurement_theta_max      30.21
_cell_measurement_theta_min      2.51
_cell_volume                     5179.7(4)
_computing_cell_refinement       'SAINT-Plus (Bruker, 1999)'
_computing_data_collection       'SMART (Bruker, 2001)'
_computing_data_reduction        'SAINT-Plus (Bruker, 1999)'
_computing_molecular_graphics    'SHELXTL (Sheldrick, 2008)'
_computing_publication_material  'SHELXTL (Sheldrick, 2008)'
_computing_structure_refinement  'SHELXL97 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      125(2)
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 1.000
_diffrn_measurement_device_type  'Bruker SMART CCD area-detector'
_diffrn_measurement_method       '\f and \w'
_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  0.0326
_diffrn_reflns_av_sigmaI/netI    0.0169
_diffrn_reflns_limit_h_max       21
_diffrn_reflns_limit_h_min       -21
_diffrn_reflns_limit_k_max       24
_diffrn_reflns_limit_k_min       -24
_diffrn_reflns_limit_l_max       25
_diffrn_reflns_limit_l_min       -24
_diffrn_reflns_number            68275
_diffrn_reflns_theta_full        29.13
_diffrn_reflns_theta_max         29.13
_diffrn_reflns_theta_min         2.05
_exptl_absorpt_coefficient_mu    0.570
_exptl_absorpt_correction_T_max  0.9144
_exptl_absorpt_correction_T_min  0.8754
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   '(SADABS; Bruker, 1999)'
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.195
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             1984
_exptl_crystal_size_max          0.24
_exptl_crystal_size_mid          0.20
_exptl_crystal_size_min          0.16
_refine_diff_density_max         0.367
_refine_diff_density_min         -0.291
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.042
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     226
_refine_ls_number_reflns         6973
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.042
_refine_ls_R_factor_all          0.0364
_refine_ls_R_factor_gt           0.0248
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w = 1/[\s^2^(Fo^2^)+(0.0241P)^2^+2.7021P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0568
_refine_ls_wR_factor_ref         0.0629
_reflns_number_gt                5714
_reflns_number_total             6973
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            hg2378.cif
_cod_data_source_block           I
_cod_database_code               2217784
_cod_database_fobs_code          2217784