Early Transition Metal Complexes Containing 1,2,4-Triazolato and Tetrazolato Ligands: Synthesis, Structure, and Molecular Orbital Studies
Carlos Yélamos; Karl R. Gust; Anwar G. Baboul; Mary Jane Heeg; H. Bernhard Schlegel; Charles H. Winter; Inorganic Chemistry 40 (2001) 6451–6462; doi:10.1021/ic0109389

data_4320682
_publ_section_title
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 Early Transition Metal Complexes Containing 1,2,4-Triazolato and
 Tetrazolato Ligands: Synthesis, Structure, and Molecular Orbital Studies
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              6451
_journal_page_last               6462
_journal_paper_doi               10.1021/ic0109389
_journal_volume                  40
_journal_year                    2001
_chemical_formula_sum            'C47 H67 N14 Nb'
_chemical_formula_weight         921.06
_chemical_name_systematic
;
  ?
;
_space_group_IT_number           4
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  'P 2yb'
_symmetry_space_group_name_H-M   'P 1 21 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                 112.8500(10)
_cell_angle_gamma                90.00
_cell_formula_units_Z            2
_cell_length_a                   12.6843(2)
_cell_length_b                   18.3911(3)
_cell_length_c                   13.1692(3)
_cell_measurement_reflns_used    8192
_cell_measurement_temperature    295(2)
_cell_volume                     2831.00(9)
_computing_cell_refinement       'Bruker SAINT'
_computing_data_collection       'Bruker SMART'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    SHELXTL-Plus
_computing_publication_material  SHELXL-93
_computing_structure_refinement  'SHELXL-93 (Sheldrick, 1993)'
_computing_structure_solution    'SHELXS-86 (Sheldrick, 1990)'
_diffrn_ambient_temperature      295(2)
_diffrn_measurement_device       'Bruker P4/CCD'
_diffrn_measurement_method       'SMART CCD'
_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  0.030
_diffrn_reflns_av_sigmaI/netI    0.0665
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       23
_diffrn_reflns_limit_k_min       -24
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_number            16587
_diffrn_reflns_theta_max         28.35
_diffrn_reflns_theta_min         2.01
_exptl_absorpt_coefficient_mu    0.253
_exptl_absorpt_correction_type   multi-scan
_exptl_crystal_colour            orange
_exptl_crystal_density_diffrn    1.081
_exptl_crystal_description       rhomboids
_exptl_crystal_F_000             976
_exptl_crystal_size_max          0.40
_exptl_crystal_size_mid          0.32
_exptl_crystal_size_min          0.24
_refine_diff_density_max         0.998
_refine_diff_density_min         -0.353
_refine_diff_density_rms         0.092
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   -0.01(4)
_refine_ls_extinction_coef       0.0029(7)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     SHELXL
_refine_ls_goodness_of_fit_all   1.041
_refine_ls_goodness_of_fit_obs   1.107
_refine_ls_matrix_type           full
_refine_ls_number_parameters     572
_refine_ls_number_reflns         10128
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.041
_refine_ls_restrained_S_obs      1.107
_refine_ls_R_factor_all          0.0682
_refine_ls_R_factor_obs          0.0523
_refine_ls_shift/esd_max         -0.419
_refine_ls_shift/esd_mean        0.014
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0902P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.1459
_refine_ls_wR_factor_obs         0.1388
_reflns_number_observed          8182
_reflns_number_total             10128
_reflns_observed_criterion       >2sigma(I)
_cod_data_source_file            ic0109389_6.cif
_cod_data_source_block           oran(11)
_cod_depositor_comments
;
The following automatic conversions were performed:

'_exptl_absorpt_correction_type' value 'Multi-scan' changed to
'multi-scan' 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:

'_refine_ls_weighting_scheme' value 'calc
w=1/[\s^2^(Fo^2^)+(0.0902P)^2^+0.0000P] 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^)+(0.0902P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'.

Automatic conversion script
Id: cif_fix_values 3143 2015-03-26 13:38:13Z robertas 
;
_cod_database_code               4320682