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_4068468
_publ_section_title
;
 General Preparation of (N3N)ZrX (N3N = N(CH2CH2NSiMe3)33&#x2212;)
 Complexes from a Hydride Surrogate
;
_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            'C17 H46 N4 P2 Si3 Zr'
_chemical_formula_weight         544.01
_chemical_name_systematic
;

 ?

;
_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
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                90.00
_cell_formula_units_Z            8
_cell_length_a                   17.0290(9)
_cell_length_b                   17.1007(9)
_cell_length_c                   20.1939(11)
_cell_measurement_reflns_used    9905
_cell_measurement_temperature    125(2)
_cell_measurement_theta_max      26.54
_cell_measurement_theta_min      2.35
_cell_volume                     5880.6(5)
_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 0.998
_diffrn_measured_fraction_theta_max 0.998
_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  0.0430
_diffrn_reflns_av_sigmaI/netI    0.0201
_diffrn_reflns_limit_h_max       21
_diffrn_reflns_limit_h_min       -21
_diffrn_reflns_limit_k_max       21
_diffrn_reflns_limit_k_min       -21
_diffrn_reflns_limit_l_max       25
_diffrn_reflns_limit_l_min       -25
_diffrn_reflns_number            64367
_diffrn_reflns_theta_full        26.62
_diffrn_reflns_theta_max         26.62
_diffrn_reflns_theta_min         1.97
_exptl_absorpt_coefficient_mu    0.615
_exptl_absorpt_correction_T_max  0.9080
_exptl_absorpt_correction_T_min  0.8614
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_process_details   sadabs
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.229
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             2304
_exptl_crystal_size_max          0.25
_exptl_crystal_size_mid          0.25
_exptl_crystal_size_min          0.16
_refine_diff_density_max         0.388
_refine_diff_density_min         -0.543
_refine_diff_density_rms         0.058
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.054
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     264
_refine_ls_number_reflns         6160
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.054
_refine_ls_R_factor_all          0.0407
_refine_ls_R_factor_gt           0.0283
_refine_ls_shift/su_max          0.019
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0257P)^2^+5.5512P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0640
_refine_ls_wR_factor_ref         0.0712
_reflns_number_gt                5008
_reflns_number_total             6160
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            om8008684_si_002.cif
_cod_data_source_block           (N3N)ZrPHCH2CH2PH2
_cod_depositor_comments
;
The following automatic conversions were performed:

'_symmetry_cell_setting' value 'Orthorhombic' changed to
'orthorhombic' 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 
;
_cod_original_sg_symbol_H-M      Pbca
_cod_database_code               4068468