(dme)MCl3(NNPh2) (dme = dimethoxyethane; M = Nb, Ta): A Versatile Synthon for [Ta=NNPh2] Hydrazido(2-) Complexes
Ian A. Tonks; John E. Bercaw; Inorganic Chemistry 49 (2010) 4648–4656; doi:10.1021/ic1004193

data_4315536
_publ_section_title
;
 (dme)MCl3(NNPh2) (dme = dimethoxyethane; M = Nb, Ta): A Versatile Synthon
 for [Ta=NNPh2] Hydrazido(2-) Complexes
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              4648
_journal_page_last               4656
_journal_paper_doi               10.1021/ic1004193
_journal_volume                  49
_journal_year                    2010
_chemical_formula_moiety         'C23 H39 Cl N5 Si2 Ta'
_chemical_formula_sum            'C23 H39 Cl N5 Si2 Ta'
_chemical_formula_weight         658.17
_chemical_name_systematic
;
 ?
;
_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   difmap
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 90.622(3)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   13.1052(6)
_cell_length_b                   12.9574(6)
_cell_length_c                   16.9529(8)
_cell_measurement_reflns_used    9392
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      40.07
_cell_measurement_theta_min      2.51
_cell_volume                     2878.6(2)
_computing_cell_refinement       'Bruker SAINT-Plus v7.66A'
_computing_data_collection       'Bruker APEX2 v2009.7-0'
_computing_data_reduction        'Bruker SAINT-Plus v7.66A'
_computing_molecular_graphics    'Bruker XP v5.1'
_computing_publication_material  'Bruker XCIF 2008'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 0.986
_diffrn_measured_fraction_theta_max 0.986
_diffrn_measurement_device_type  'Bruker KAPPA APEX II'
_diffrn_measurement_method       '\w scans; 21 settings'
_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  0.0416
_diffrn_reflns_av_sigmaI/netI    0.0249
_diffrn_reflns_limit_h_max       25
_diffrn_reflns_limit_h_min       -25
_diffrn_reflns_limit_k_max       25
_diffrn_reflns_limit_k_min       -24
_diffrn_reflns_limit_l_max       32
_diffrn_reflns_limit_l_min       -32
_diffrn_reflns_number            201289
_diffrn_reflns_theta_full        43.76
_diffrn_reflns_theta_max         43.76
_diffrn_reflns_theta_min         1.95
_exptl_absorpt_coefficient_mu    4.014
_exptl_absorpt_correction_T_max  0.7486
_exptl_absorpt_correction_T_min  0.5883
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS v2008/v, Bruker-AXS, Madison, WI'
_exptl_crystal_colour            Yellow
_exptl_crystal_density_diffrn    1.519
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       Column
_exptl_crystal_F_000             1320
_exptl_crystal_size_max          0.23
_exptl_crystal_size_mid          0.14
_exptl_crystal_size_min          0.08
_refine_diff_density_max         4.170
_refine_diff_density_min         -2.602
_refine_diff_density_rms         0.152
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   2.205
_refine_ls_hydrogen_treatment    refall
_refine_ls_matrix_type           'Full matrix'
_refine_ls_number_parameters     445
_refine_ls_number_reflns         21919
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      2.205
_refine_ls_R_factor_all          0.0444
_refine_ls_R_factor_gt           0.0285
_refine_ls_shift/su_max          0.011
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details     w=1/s^2^(Fo^2^)
_refine_ls_weighting_scheme      sigma
_refine_ls_wR_factor_gt          0.0506
_refine_ls_wR_factor_ref         0.0517
_reflns_number_gt                17487
_reflns_number_total             21919
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic1004193_si_002_6.cif
_cod_data_source_block           complex10
_cod_depositor_comments
;
The following automatic conversions were performed:

'_symmetry_cell_setting' value 'Monoclinic' changed to 'monoclinic'
according to the built-in table from CIF Core dictionary named
'cif_core.dic' version 2.4.1 from
2010-06-29.

'_refine_ls_weighting_scheme' value 'Sigma' changed to
'sigma' according to the built-in table from CIF Core dictionary
named 'cif_core.dic' version 2.4.1 from 2010-06-29.

Automatic conversion script
Id: cif_fix_values 1646 2011-03-28 12:23:43Z adriana 

The following automatic conversions were performed:

'_atom_sites_solution_primary' value 'Direct methods' was changed to
'direct'.

'_atom_sites_solution_secondary' value 'Difference Fourier map' was
changed to 'difmap'.

'_atom_sites_solution_hydrogens' value 'Difference Fourier map' was
changed to 'difmap'.

Automatic conversion script
Id: cif_fix_values 6452 2018-10-05 10:23:21Z andrius 
;
_cod_database_code               4315536