New Alkylimido Niobium Complexes Supported by Guanidinate Ligands: Synthesis, Characterization, and Migratory Insertion Reactions
Elorriaga, David; Carrillo-Hermosilla, Fernando; Antiñolo, Antonio; López-Solera, Isabel; Menot, Bérengère; Fernández-Galán, Rafael; Villaseñor, Elena; Otero, Antonio; Organometallics 31 (2012) 1840–; doi:10.1021/om201192w

data_4076419
_publ_section_title
;
 New Alkylimido Niobium Complexes Supported by Guanidinate Ligands:
 Synthesis, Characterization, and Migratory Insertion Reactions
;
_journal_issue                   5
_journal_name_full               Organometallics
_journal_page_first              1840
_journal_paper_doi               10.1021/om201192w
_journal_volume                  31
_journal_year                    2012
_chemical_formula_moiety         'C56 H80 N8 Nb2, 2(C4 H8 O)'
_chemical_formula_sum            'C64 H96 N8 Nb2 O2'
_chemical_formula_weight         1195.31
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           15
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-C 2yc'
_symmetry_space_group_name_H-M   'C 1 2/c 1'
_atom_sites_solution_hydrogens   const
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 121.992(2)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   29.609(3)
_cell_length_b                   15.5693(14)
_cell_length_c                   16.6469(15)
_cell_measurement_reflns_used    662
_cell_measurement_temperature    230(2)
_cell_measurement_theta_max      17.071
_cell_measurement_theta_min      2.866
_cell_volume                     6508.6(11)
_computing_cell_refinement       'Bruker SAINT'
_computing_data_collection       'Bruker APEX'
_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      230(2)
_diffrn_measured_fraction_theta_full 0.995
_diffrn_measured_fraction_theta_max 0.995
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       'omega 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  0.1250
_diffrn_reflns_av_sigmaI/netI    0.1932
_diffrn_reflns_limit_h_max       41
_diffrn_reflns_limit_h_min       -42
_diffrn_reflns_limit_k_max       22
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            22551
_diffrn_reflns_theta_full        30.45
_diffrn_reflns_theta_max         30.45
_diffrn_reflns_theta_min         2.39
_exptl_absorpt_coefficient_mu    0.398
_exptl_absorpt_correction_T_max  0.7461
_exptl_absorpt_correction_T_min  0.6149
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   SADABS
_exptl_crystal_colour            Yellow
_exptl_crystal_density_diffrn    1.220
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       Prismatic
_exptl_crystal_F_000             2536
_exptl_crystal_size_max          0.530
_exptl_crystal_size_mid          0.473
_exptl_crystal_size_min          0.452
_refine_diff_density_max         0.445
_refine_diff_density_min         -0.734
_refine_diff_density_rms         0.087
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.922
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     374
_refine_ls_number_reflns         9858
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.922
_refine_ls_R_factor_all          0.2040
_refine_ls_R_factor_gt           0.0787
_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^)+(0.0608P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1447
_refine_ls_wR_factor_ref         0.1936
_reflns_number_gt                3899
_reflns_number_total             9858
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            om201192w_si_001.cif
_cod_data_source_block           9
_cod_depositor_comments
;
The following automatic conversions were performed:

'_symmetry_cell_setting' value 'Monoclinic' changed to 'monoclinic'
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_cell_volume        6508.5(10)
_cod_original_sg_symbol_H-M      C2/c
_cod_database_code               4076419