General Preparation of (N3N)ZrX (N3N = N(CH2CH2NSiMe3)33−) Complexes from a Hydride Surrogate
Roering, Andrew J.; Maddox, Annalese F.; Elrod, L. Taylor; Chan, Stephanie M.; Ghebreab, Michael B.; Donovan, Kyle L.; Davidson, Jillian J.; Hughes, Russell P.; Shalumova, Tamila; MacMillan, Samantha N.; Tanski, Joseph M.; Waterman, Rory; Organometallics 28 (2009) 573–; doi:10.1021/om8008684

data_4068470
_publ_section_title
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 General Preparation of (N3N)ZrX (N3N = N(CH2CH2NSiMe3)33&#x2212;)
 Complexes from a Hydride Surrogate
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_journal_issue                   2
_journal_name_full               Organometallics
_journal_page_first              573
_journal_paper_doi               10.1021/om8008684
_journal_volume                  28
_journal_year                    2009
_chemical_formula_sum            'C19 H48 N4 S Si3 Zr'
_chemical_formula_weight         540.16
_chemical_name_systematic
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 ?

;
_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                 95.3890(10)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   11.8438(5)
_cell_length_b                   20.1540(8)
_cell_length_c                   12.0195(5)
_cell_measurement_reflns_used    9923
_cell_measurement_temperature    125(2)
_cell_measurement_theta_max      30.40
_cell_measurement_theta_min      2.52
_cell_volume                     2856.4(2)
_computing_cell_refinement       'Bruker SAINT'
_computing_data_collection       'Bruker APEX2'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS-97 (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 APEX-II CCD'
_diffrn_measurement_method       '\f and \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  0.0248
_diffrn_reflns_av_sigmaI/netI    0.0176
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       27
_diffrn_reflns_limit_k_min       -27
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_number            38319
_diffrn_reflns_theta_full        28.70
_diffrn_reflns_theta_max         28.70
_diffrn_reflns_theta_min         1.98
_exptl_absorpt_coefficient_mu    0.596
_exptl_absorpt_correction_T_max  0.9212
_exptl_absorpt_correction_T_min  0.8461
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_process_details   sadabs
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.256
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             1152
_exptl_crystal_size_max          0.29
_exptl_crystal_size_mid          0.28
_exptl_crystal_size_min          0.14
_refine_diff_density_max         0.371
_refine_diff_density_min         -0.282
_refine_diff_density_rms         0.051
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.045
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     265
_refine_ls_number_reflns         7374
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.045
_refine_ls_R_factor_all          0.0250
_refine_ls_R_factor_gt           0.0212
_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^)+(0.0281P)^2^+0.9986P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0548
_refine_ls_wR_factor_ref         0.0571
_reflns_number_gt                6668
_reflns_number_total             7374
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            om8008684_si_002.cif
_cod_data_source_block           (N3N)ZrStBu
_cod_depositor_comments
;
The following automatic conversions were performed:

'_symmetry_cell_setting' value 'Monoclinic' changed to 'monoclinic'
according to /home/saulius/struct/CIF-dictionaries/cif_core.dic
dictionary named 'cif_core.dic' version 2.4.2 from 2011-04-26.

Automatic conversion script
Id: cif_fix_values 1715 2011-07-08 13:25:40Z adriana 
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_cod_original_sg_symbol_H-M      P2(1)/n
_cod_database_code               4068470