Niobium Bis-alkylidene Complexes Prepared by a Multi-Electron Redox Process
Kilgore, Uriah J.; Tomaszewski, John; Fan, Hongjun; Huffman, John C.; Mindiola, Daniel J.; Organometallics 26 (2007) 6132–; doi:10.1021/om7008233

data_4074017
_publ_section_title
;
 Niobium Bis-alkylidene Complexes Prepared by a Multi-Electron Redox
 Process
;
_journal_issue                   25
_journal_name_full               Organometallics
_journal_page_first              6132
_journal_paper_doi               10.1021/om7008233
_journal_volume                  26
_journal_year                    2007
_chemical_formula_sum            'C35 H62.5 N Nb O0.25 P2 Si2'
_chemical_formula_weight         712.39
_chemical_name_systematic
; 
 ? 
;
_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-97
_cell_angle_alpha                82.957(3)
_cell_angle_beta                 81.382(3)
_cell_angle_gamma                77.863(3)
_cell_formula_units_Z            4
_cell_length_a                   11.3020(13)
_cell_length_b                   11.7003(13)
_cell_length_c                   31.275(4)
_cell_measurement_reflns_used    1955
_cell_measurement_temperature    133(2)
_cell_measurement_theta_max      27.40
_cell_measurement_theta_min      2.79
_cell_volume                     3979.8(8)
_computing_cell_refinement       'SAINT (Bruker, 1999)'
_computing_data_collection       'SMART (Bruker, 1999)'
_computing_data_reduction        'SAINT (Bruker, 1999), XTEL (local package)'
_computing_molecular_graphics    'Reciprocal Net (http://recipnet.org)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      133(2)
_diffrn_detector                 'CCD area detector'
_diffrn_detector_area_resol_mean 44.52
_diffrn_detector_type            'Bruker SMART 6000'
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measurement_details
'   0.30 degree frames measured for 5.16 seconds each'
_diffrn_measurement_device       'three-circle goniometer with fixed chi'
_diffrn_measurement_device_type  'Bruker Platform goniometer'
_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  0.0704
_diffrn_reflns_av_sigmaI/netI    0.0478
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       40
_diffrn_reflns_limit_l_min       -40
_diffrn_reflns_number            120379
_diffrn_reflns_theta_full        27.55
_diffrn_reflns_theta_max         27.55
_diffrn_reflns_theta_min         1.85
_diffrn_standards_decay_%        0.0
_exptl_absorpt_coefficient_mu    0.466
_exptl_absorpt_correction_T_max  1.00
_exptl_absorpt_correction_T_min  0.92
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'Bruker-AXS SADABS'
_exptl_crystal_colour            black
_exptl_crystal_density_diffrn    1.189
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       'gooey mess!'
_exptl_crystal_F_000             1522
_exptl_crystal_size_max          0.35
_exptl_crystal_size_mid          0.35
_exptl_crystal_size_min          0.18
_refine_diff_density_max         0.686
_refine_diff_density_min         -0.698
_refine_diff_density_rms         0.071
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.983
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     959
_refine_ls_number_reflns         18322
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.983
_refine_ls_R_factor_all          0.0582
_refine_ls_R_factor_gt           0.0365
_refine_ls_shift/su_max          0.028
_refine_ls_shift/su_mean         0.001
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0559P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0921
_refine_ls_wR_factor_ref         0.1008
_reflns_number_gt                13219
_reflns_number_total             18322
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            om70082332.cif
_cod_data_source_block           06179
_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_sg_symbol_H-M      'P-1   '
_cod_original_formula_sum        'C35 H62.50 N Nb O0.25 P2 Si2'
_cod_database_code               4074017