Synthesis and Properties of Cyclopentadienylniobium(III) Complexes. A Magneto−Structural Correlation for 16-Electron Four-Legged Piano Stool Complexes†
Fettinger, J. C.; Keogh, D. Webster; Kraatz, Heinz-Bernhard; Poli, Rinaldo; Organometallics 15 (1996) 5489–; doi:10.1021/om960384v

data_4078364
_publ_section_title
;
 Synthesis and Properties of Cyclopentadienylniobium(III) Complexes. A
 Magneto&#x2212;Structural Correlation for 16-Electron Four-Legged Piano
 Stool Complexes&#x2020;
;
_journal_issue                   26
_journal_name_full               Organometallics
_journal_page_first              5489
_journal_paper_doi               10.1021/om960384v
_journal_volume                  15
_journal_year                    1996
_chemical_formula_sum            'C18 H37 Cl2 Nb P2'
_chemical_formula_weight         479.23
_chemical_name_systematic
;
 ?
;
_space_group_IT_number           14
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL
_cell_angle_alpha                90.00
_cell_angle_beta                 90.3421(7)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   8.0735(5)
_cell_length_b                   13.9677(9)
_cell_length_c                   20.458(2)
_cell_measurement_reflns_used    25
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      18.1
_cell_measurement_theta_min      9.2
_cell_volume                     2307.0(3)
_computing_cell_refinement       'Enraf-Nonius EXPRESS'
_computing_data_collection       'Enraf-Nonius EXPRESS'
_computing_data_reduction        'XCAD4, (Harms,1993)'
_computing_molecular_graphics    'ORTEP (NRCVAX)'
_computing_publication_material  'XCIF, SHELXL-93 (Sheldrick, 1993)'
_computing_structure_refinement  'SHELXL-93 (Sheldrick, 1993)'
_computing_structure_solution    'SHELXS-86 (Sheldrick, 1990)'
_diffrn_ambient_temperature      293(2)
_diffrn_measurement_device       'Enraf-Nonius CAD4'
_diffrn_measurement_method       '\w scans'
_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  0.0378
_diffrn_reflns_av_sigmaI/netI    0.0397
_diffrn_reflns_limit_h_max       8
_diffrn_reflns_limit_h_min       -8
_diffrn_reflns_limit_k_max       0
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       0
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_diffrn_reflns_theta_max         22.47
_diffrn_reflns_theta_min         2.47
_diffrn_standards_decay_%        0
_diffrn_standards_interval_time  120
_diffrn_standards_number         3
_exptl_absorpt_coefficient_mu    0.420
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    1.380
_exptl_crystal_F_000             1000
_exptl_crystal_size_max          0.20
_exptl_crystal_size_mid          0.20
_exptl_crystal_size_min          0.20
_refine_diff_density_max         0.638
_refine_diff_density_min         -0.451
_refine_diff_density_rms         0.078
_refine_ls_extinction_method     none
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_refine_ls_goodness_of_fit_obs   1.068
_refine_ls_matrix_type           full
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_refine_ls_number_reflns         2995
_refine_ls_number_restraints     0
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_refine_ls_restrained_S_obs      1.068
_refine_ls_R_factor_all          0.0808
_refine_ls_R_factor_obs          0.0498
_refine_ls_shift/esd_max         -0.002
_refine_ls_shift/esd_mean        0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0717P)^2^+3.3474P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.1382
_refine_ls_wR_factor_obs         0.1193
_reflns_number_observed          2162
_reflns_number_total             2995
_reflns_observed_criterion       >2sigma(I)
_cod_data_source_file            om960384v.cif
_cod_data_source_block           Cp'NbCl2(PEt3)2
_cod_depositor_comments
;
The following automatic conversions were performed:

'_refine_ls_weighting_scheme' value 'calc
w=1/[\s^2^(Fo^2^)+(0.0717P)^2^+3.3474P] 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^)+(0.0717P)^2^+3.3474P] where P=(Fo^2^+2Fc^2^)/3'.

Automatic conversion script
Id: cif_fix_values 3143 2015-03-26 13:38:13Z robertas 
;
_cod_original_cell_volume        2306.9(3)
_cod_database_code               4078364