Niobium‒η-cyclopentadienyl compounds with imido and amido ligands derived from 2,6-dimethylaniline
Humphries, Martin J.; Green, Malcolm L. H.; Douthwaite, Richard E.; Rees, Leigh H.; Journal of the Chemical Society, Dalton Transactions  (2000) 4555–; doi:10.1039/b007178l

data_7010227
_publ_section_title
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 Niobium--\h-cyclopentadienyl compounds with imido and amido ligands
 derived from 2,6-dimethylaniline
;
_journal_issue                   24
_journal_name_full
'Journal of the Chemical Society, Dalton Transactions'
_journal_page_first              4555
_journal_paper_doi               10.1039/b007178l
_journal_year                    2000
_chemical_compound_source        'synthesis as described'
_chemical_formula_moiety         'C58 H68 N6 Nb2'
_chemical_formula_structural     'C58 H68 N6 NB2'
_chemical_formula_sum            'C58 H68 N6 Nb2'
_chemical_formula_weight         1035.00
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_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
_cell_angle_alpha                76.26(6)
_cell_angle_beta                 89.60(3)
_cell_angle_gamma                89.97(5)
_cell_formula_units_Z            2
_cell_length_a                   7.969(10)
_cell_length_b                   17.246(20)
_cell_length_c                   18.845(10)
_cell_measurement_reflns_used    166
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      0
_cell_measurement_theta_min      0
_cell_volume                     2516(5)
_computing_cell_refinement       DENZO
_computing_data_collection       'DIP2000 Software XPRESS (Mac Science)'
_computing_data_reduction        'DENZO & SCALEPACK'
_computing_molecular_graphics    'CAMERON (Watkin & Pearce, 1997)'
_computing_publication_material  'WinGX publication routines (Farrugia, 1998)'
_computing_structure_refinement  'SHELXL-93 (Sheldrick, 1993)'
_computing_structure_solution    SIR-92
_diffrn_ambient_temperature      293(2)
_diffrn_measurement_device       'Enraf-Nonius DIP2000'
_diffrn_measurement_method       \w
_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  0.024
_diffrn_reflns_av_sigmaI/netI    0.0405
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_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_number            7909
_diffrn_reflns_theta_max         25.00
_diffrn_reflns_theta_min         1.44
_diffrn_standards_decay_%        0
_diffrn_standards_interval_count 0
_diffrn_standards_interval_time  0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.500
_exptl_absorpt_correction_T_max  0.9142
_exptl_absorpt_correction_T_min  0.7773
_exptl_absorpt_correction_type   refdelf
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.366
_exptl_crystal_density_method    none
_exptl_crystal_description       prism
_exptl_crystal_F_000             1080
_exptl_crystal_size_max          0.5
_exptl_crystal_size_mid          0.4
_exptl_crystal_size_min          0.4
_refine_diff_density_max         0.392
_refine_diff_density_min         -0.744
_refine_diff_density_rms         0.073
_refine_ls_extinction_method     none
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_refine_ls_goodness_of_fit_obs   1.430
_refine_ls_matrix_type           full
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_refine_ls_number_reflns         7901
_refine_ls_number_restraints     24
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_refine_ls_restrained_S_obs      1.428
_refine_ls_R_factor_all          0.0689
_refine_ls_R_factor_obs          0.0667
_refine_ls_shift/esd_max         0.005
_refine_ls_shift/esd_mean        0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0000P)^2^+7.9882P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.1551
_refine_ls_wR_factor_obs         0.1319
_reflns_number_observed          7866
_reflns_number_total             7909
_reflns_observed_criterion       2sigma(I)
_cod_data_source_file            b007178l.txt
_cod_data_source_block           structure4
_cod_depositor_comments
;
The following automatic conversions were performed:

'_refine_ls_weighting_scheme' value 'calc
w=1/[\s^2^(Fo^2^)+(0.0000P)^2^+7.9882P] where P=(Fo^2^+2Fc^2^)/3' was
changed to 'calc'. New tag '_refine_ls_weighting_details' was
created. The value of the new tag was set to
'w=1/[\s^2^(Fo^2^)+(0.0000P)^2^+7.9882P] where P=(Fo^2^+2Fc^2^)/3'.

Automatic conversion script
Id: cif_fix_values 3143 2015-03-26 13:38:13Z robertas 
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_cod_original_cell_volume        2515.7(45)
_cod_database_code               7010227