Mono-anionic acetophenone imine ligands: synthesis, ortho-lithiation and first examples of group (v) metal complexes
Neshat, Abdollah; Seambos, Cheryl L.; Beck, John F.; Schmidt, Joseph A. R.; Dalton Transactions  (2009) 4987–5000; doi:10.1039/b903836a

data_7001481
_publ_section_title
;
 Mono-anionic acetophenone imine ligands: synthesis, ortho-lithiation
 and first examples of group (v) metal complexes
;
_journal_issue                   25
_journal_name_full               'Dalton Transactions'
_journal_page_first              4987
_journal_page_last               5000
_journal_paper_doi               10.1039/b903836a
_journal_year                    2009
_chemical_formula_sum            'C52 H62 Cl N3 Nb O4.5'
_chemical_formula_weight         929.41
_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                106.767(3)
_cell_angle_beta                 91.047(3)
_cell_angle_gamma                101.570(3)
_cell_formula_units_Z            2
_cell_length_a                   9.557(1)
_cell_length_b                   12.424(2)
_cell_length_c                   21.471(3)
_cell_measurement_reflns_used    6448
_cell_measurement_temperature    175(2)
_cell_measurement_theta_max      28.15
_cell_measurement_theta_min      2.22
_cell_volume                     2383.5(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      175(2)
_diffrn_measured_fraction_theta_full 0.973
_diffrn_measured_fraction_theta_max 0.973
_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  0.0724
_diffrn_reflns_av_sigmaI/netI    0.1010
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       28
_diffrn_reflns_limit_l_min       -28
_diffrn_reflns_number            25946
_diffrn_reflns_theta_full        28.46
_diffrn_reflns_theta_max         28.46
_diffrn_reflns_theta_min         0.99
_exptl_absorpt_coefficient_mu    0.357
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.541
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_process_details   SADABS
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    1.295
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       tablet
_exptl_crystal_F_000             978
_exptl_crystal_size_max          0.60
_exptl_crystal_size_mid          0.16
_exptl_crystal_size_min          0.06
_refine_diff_density_max         1.599
_refine_diff_density_min         -2.484
_refine_diff_density_rms         0.131
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.002
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     558
_refine_ls_number_reflns         11698
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.002
_refine_ls_R_factor_all          0.1200
_refine_ls_R_factor_gt           0.0814
_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^)+(0.1396P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2050
_refine_ls_wR_factor_ref         0.2340
_reflns_number_gt                7098
_reflns_number_total             11698
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            b903836a.txt
_cod_data_source_block           (2)2Nb(N-2,6-iPr2C6H3)Cl_(16)
_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_enum 1527 2010-12-29 10:47:43Z saulius 
;
_cod_original_cell_volume        2383.4(5)
_cod_original_sg_symbol_H-M      P-1
_cod_original_formula_sum        'C52 H62 Cl N3 Nb O4.50'
_cod_database_code               7001481