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_4076420
_publ_section_title
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 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         'C92 H116 N12 Nb2, 2(C5 H12)'
_chemical_formula_sum            'C102 H140 N12 Nb2'
_chemical_formula_weight         1720.08
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_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-97
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   13.083(7)
_cell_length_b                   22.920(12)
_cell_length_c                   33.053(17)
_cell_measurement_reflns_used    907
_cell_measurement_temperature    230(2)
_cell_measurement_theta_max      13.22
_cell_measurement_theta_min      2.36
_cell_volume                     9911(9)
_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 0.929
_diffrn_measured_fraction_theta_max 0.929
_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  0.2296
_diffrn_reflns_av_sigmaI/netI    0.3189
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -18
_diffrn_reflns_limit_k_max       31
_diffrn_reflns_limit_k_min       -31
_diffrn_reflns_limit_l_max       43
_diffrn_reflns_limit_l_min       -43
_diffrn_reflns_number            84423
_diffrn_reflns_theta_full        29.51
_diffrn_reflns_theta_max         29.51
_diffrn_reflns_theta_min         1.52
_exptl_absorpt_coefficient_mu    0.281
_exptl_absorpt_correction_T_max  0.7459
_exptl_absorpt_correction_T_min  0.6351
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   SADABS
_exptl_crystal_colour            Yellow
_exptl_crystal_density_diffrn    1.153
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       Prismatic
_exptl_crystal_F_000             3672
_exptl_crystal_size_max          0.237
_exptl_crystal_size_mid          0.077
_exptl_crystal_size_min          0.049
_refine_diff_density_max         0.398
_refine_diff_density_min         -0.520
_refine_diff_density_rms         0.079
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.921
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1079
_refine_ls_number_reflns         25676
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.921
_refine_ls_R_factor_all          0.2854
_refine_ls_R_factor_gt           0.0956
_refine_ls_shift/su_max          0.008
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0523P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1639
_refine_ls_wR_factor_ref         0.2287
_reflns_number_gt                8177
_reflns_number_total             25676
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            om201192w_si_001.cif
_cod_data_source_block           17
_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_sg_symbol_H-M      P2(1)/n
_cod_database_code               4076420