Mononuclear Tantalum(IV, d1) Imido Complexes Supported by the Monocyclopentadienyl, Amidinate and Guanidinate Ligand Sets As Models to Explore Dinitrogen Fixation by “End-On-Bridged” Dinuclear {[Ta(IV, d1)]}2(μ-η1:η1-N2) Complexes
Yonke, Brendan L.; Keane, Andrew J.; Zavalij, Peter Y.; Sita, Lawrence R.; Organometallics 31 (2012) 345–; doi:10.1021/om200961r

data_4067950
_publ_section_title
;
 Mononuclear Tantalum(IV, d1) Imido Complexes Supported by the
 Monocyclopentadienyl, Amidinate and Guanidinate Ligand Sets As Models to
 Explore Dinitrogen Fixation by &#x201C;End-On-Bridged&#x201D; Dinuclear
 {[Ta(IV, d1)]}2(\m-\h1:\h1-N2) Complexes
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_journal_issue                   1
_journal_name_full               Organometallics
_journal_page_first              345
_journal_paper_doi               10.1021/om200961r
_journal_volume                  31
_journal_year                    2012
_chemical_formula_moiety         'C22 H41 N3 Ta'
_chemical_formula_sum            'C22 H41 N3 Ta'
_chemical_formula_weight         528.53
_chemical_name_systematic        Ta-complex
_space_group_IT_number           62
_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_Hall  '-P 2ac 2n'
_symmetry_space_group_name_H-M   'P n m a'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           'SHELXL-97 & ZCIF'
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   17.6074(7)
_cell_length_b                   15.0201(6)
_cell_length_c                   9.1566(4)
_cell_measurement_reflns_used    17972
_cell_measurement_temperature    200(2)
_cell_measurement_theta_max      32.0
_cell_measurement_theta_min      2.3
_cell_volume                     2421.60(17)
_computing_cell_refinement       Apex2
_computing_data_collection       'Apex2 (Bruker, 2005)'
_computing_data_reduction        Apex2
_computing_molecular_graphics    'XSHEL (Bruker, 2004)'
_computing_publication_material  SHELXL-97
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      200(2)
_diffrn_detector                 'CCD area detector'
_diffrn_detector_area_resol_mean 11.198
_diffrn_detector_type            'Bruker Smart Apex II'
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_details      366,366,366
_diffrn_measurement_device_type  'three-circle diffractometer'
_diffrn_measurement_method       '\w and \f scans'
_diffrn_measurement_specimen_support 'glass capillary'
_diffrn_orient_matrix_type       standard
_diffrn_orient_matrix_UB_11      -0.0737974
_diffrn_orient_matrix_UB_12      0.0059816
_diffrn_orient_matrix_UB_13      0.0415562
_diffrn_orient_matrix_UB_21      0.0394276
_diffrn_orient_matrix_UB_22      0.0603000
_diffrn_orient_matrix_UB_23      0.0126288
_diffrn_orient_matrix_UB_31      -0.0701887
_diffrn_orient_matrix_UB_32      0.0275799
_diffrn_orient_matrix_UB_33      -0.0365937
_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  0.0197
_diffrn_reflns_av_sigmaI/netI    0.0123
_diffrn_reflns_limit_h_max       24
_diffrn_reflns_limit_h_min       -24
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_k_min       -21
_diffrn_reflns_limit_l_max       12
_diffrn_reflns_limit_l_min       -12
_diffrn_reflns_number            24872
_diffrn_reflns_theta_full        30.00
_diffrn_reflns_theta_max         30.00
_diffrn_reflns_theta_min         2.31
_diffrn_source_current           30.00
_diffrn_source_voltage           50.00
_diffrn_standards_decay_%        0
_exptl_absorpt_coefficient_mu    4.549
_exptl_absorpt_correction_T_max  0.170
_exptl_absorpt_correction_T_min  0.123
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS (Sheldrick, 1996)'
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    1.450
_exptl_crystal_density_method    not-measured
_exptl_crystal_description       prism
_exptl_crystal_F_000             1068
_exptl_crystal_id                ' '
_exptl_crystal_size_max          0.495
_exptl_crystal_size_mid          0.49
_exptl_crystal_size_min          0.39
_refine_diff_density_max         2.838
_refine_diff_density_min         -1.953
_refine_diff_density_rms         0.088
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.000
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     138
_refine_ls_number_reflns         3653
_refine_ls_number_restraints     18
_refine_ls_restrained_S_all      1.020
_refine_ls_R_factor_all          0.0249
_refine_ls_R_factor_gt           0.0231
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.008P)^2^+7.18P], P=(max(Fo^2^,0)+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0486
_refine_ls_wR_factor_ref         0.0495
_reflns_number_gt                3449
_reflns_number_total             3653
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            om200961r_si_002.cif
_cod_data_source_block           cmpd1
_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 2.4.1 from 2010-06-29.

Automatic conversion script
Id: cif_fix_values 1715 2011-07-08 13:25:40Z adriana 
;
_cod_original_sg_symbol_H-M      Pnma
_cod_database_code               4067950