Derivatization of Niobium Complexes Bearing Imido and Acetophenone Imine Ligands
Neshat, Abdollah; Schmidt, Joseph A. R.; Organometallics 29 (2010) 6219–; doi:10.1021/om100657r

data_4066816
_publ_section_title
;
 Derivatization of Niobium Complexes Bearing Imido and Acetophenone Imine
 Ligands
;
_journal_issue                   23
_journal_name_full               Organometallics
_journal_page_first              6219
_journal_paper_doi               10.1021/om100657r
_journal_volume                  29
_journal_year                    2010
_chemical_formula_moiety         '3(C55 H68 N3 Nb O5), 2(C5 H12)'
_chemical_formula_sum            'C175 H228 N9 Nb3 O15'
_chemical_formula_weight         2976.39
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_symmetry_Int_Tables_number      2
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                105.298(3)
_cell_angle_beta                 91.241(3)
_cell_angle_gamma                100.978(3)
_cell_formula_units_Z            2
_cell_length_a                   12.8639(18)
_cell_length_b                   23.269(3)
_cell_length_c                   27.346(4)
_cell_measurement_reflns_used    875
_cell_measurement_temperature    140(2)
_cell_measurement_theta_max      19.87
_cell_measurement_theta_min      2.63
_cell_volume                     7728.6(19)
_computing_cell_refinement       'Bruker SAINT v6.22'
_computing_data_collection       'Bruker SMART v5.625'
_computing_data_reduction        'Bruker SAINT v6.22'
_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      140(2)
_diffrn_measured_fraction_theta_full 0.995
_diffrn_measured_fraction_theta_max 0.995
_diffrn_measurement_device_type  'SMART CCD'
_diffrn_measurement_method       \w-scan
_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  0.1090
_diffrn_reflns_av_sigmaI/netI    0.1898
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       26
_diffrn_reflns_limit_k_min       -27
_diffrn_reflns_limit_l_max       31
_diffrn_reflns_limit_l_min       -31
_diffrn_reflns_number            55717
_diffrn_reflns_theta_full        24.45
_diffrn_reflns_theta_max         24.45
_diffrn_reflns_theta_min         1.55
_exptl_absorpt_coefficient_mu    0.285
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.831
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_process_details   SADABS
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.279
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             3168
_exptl_crystal_size_max          0.10
_exptl_crystal_size_mid          0.06
_exptl_crystal_size_min          0.04
_refine_diff_density_max         0.779
_refine_diff_density_min         -1.571
_refine_diff_density_rms         0.216
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.987
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1819
_refine_ls_number_reflns         25439
_refine_ls_number_restraints     14
_refine_ls_restrained_S_all      0.987
_refine_ls_R_factor_all          0.1641
_refine_ls_R_factor_gt           0.0646
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0994P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1483
_refine_ls_wR_factor_ref         0.2121
_reflns_number_gt                12831
_reflns_number_total             25439
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            om100657r_si_002.cif
_cod_data_source_block           15f
_cod_depositor_comments
;
The following automatic conversions were performed:

'_symmetry_cell_setting' value 'Triclinic' changed to 'triclinic'
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_cell_volume        7728.5(19)
_cod_original_sg_symbol_H-M      P-1
_cod_database_code               4066816