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_4068471
_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            'C21 H51 N4 P Si3 Zr'
_chemical_formula_weight         566.12
_chemical_name_systematic
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 ?

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_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                   16.8829(9)
_cell_length_b                   17.5894(10)
_cell_length_c                   20.3466(11)
_cell_measurement_reflns_used    9900
_cell_measurement_temperature    125(2)
_cell_measurement_theta_max      29.99
_cell_measurement_theta_min      2.32
_cell_volume                     6042.1(6)
_computing_cell_refinement       'Bruker SMART'
_computing_data_collection       'Bruker SMART'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      125(2)
_diffrn_measured_fraction_theta_full 0.967
_diffrn_measured_fraction_theta_max 0.967
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       'phi and omega 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  0.0610
_diffrn_reflns_av_sigmaI/netI    0.0368
_diffrn_reflns_limit_h_max       23
_diffrn_reflns_limit_h_min       -23
_diffrn_reflns_limit_k_max       24
_diffrn_reflns_limit_k_min       -24
_diffrn_reflns_limit_l_max       28
_diffrn_reflns_limit_l_min       -28
_diffrn_reflns_number            81714
_diffrn_reflns_theta_full        30.46
_diffrn_reflns_theta_max         30.46
_diffrn_reflns_theta_min         1.95
_exptl_absorpt_coefficient_mu    0.551
_exptl_absorpt_correction_T_max  0.9730
_exptl_absorpt_correction_T_min  0.8837
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_process_details   sadabs
_exptl_crystal_colour            Yellow
_exptl_crystal_density_diffrn    1.245
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       Block
_exptl_crystal_F_000             2416
_exptl_crystal_size_max          0.23
_exptl_crystal_size_mid          0.13
_exptl_crystal_size_min          0.05
_refine_diff_density_max         0.436
_refine_diff_density_min         -0.378
_refine_diff_density_rms         0.069
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.007
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     348
_refine_ls_number_reflns         8889
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.007
_refine_ls_R_factor_all          0.0603
_refine_ls_R_factor_gt           0.0320
_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^)+(0.0293P)^2^+3.0235P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0649
_refine_ls_wR_factor_ref         0.0746
_reflns_number_gt                6404
_reflns_number_total             8889
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            om8008684_si_002.cif
_cod_data_source_block           (N3N)ZrPHCy
_cod_depositor_comments
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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 
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_cod_original_sg_symbol_H-M      Pbca
_cod_database_code               4068471