Trianionic Pincer Complexes of Niobium and Tantalum as Precatalysts for ROMP of Norbornene
VenkatRamani, Sudarsan; Roland, Christopher D.; Zhang, James G.; Ghiviriga, Ion; Abboud, Khalil A.; Veige, Adam S.; Organometallics 35 (2016) 2675–; doi:10.1021/acs.organomet.6b00421

data_4088772
_publ_section_title
;
 Trianionic Pincer Complexes of Niobium and Tantalum as Precatalysts for
 ROMP of Norbornene
;
_journal_issue                   16
_journal_name_full               Organometallics
_journal_page_first              2675
_journal_paper_doi               10.1021/acs.organomet.6b00421
_journal_volume                  35
_journal_year                    2016
_chemical_formula_sum            'C40 H38 F12 N Nb O2'
_chemical_formula_weight         885.62
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2ybc'
_space_group_name_H-M_alt        'P 1 21/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-2014/6
_audit_update_record
;
2015-11-11 # Formatted by publCIF

;
_cell_angle_alpha                90
_cell_angle_beta                 108.6413(10)
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   21.8594(9)
_cell_length_b                   19.7815(9)
_cell_length_c                   18.6796(8)
_cell_measurement_reflns_used    8453
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      28.0
_cell_measurement_theta_min      2.0
_cell_volume                     7653.5(6)
_computing_cell_refinement       'Bruker APEX2 (Bruker, 2014)'
_computing_data_collection       'Bruker APEX2 (Bruker, 2014)'
_computing_data_reduction        'Bruker SHELXTL (Bruker 2000)'
_computing_molecular_graphics    'XP in SHELXTL-plus, Bruker 2014'
_computing_publication_material  'SHELXL2014/6, Sheldrick, G. M. 2014'
_computing_structure_refinement  'SHELXL2014/6, Sheldrick G. M. 2014'
_computing_structure_solution    'SHELXL2014/6, Sheldrick G. M. 2014'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 1.000
_diffrn_measurement_device_type  'Bruker APEX-II DUO'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0678
_diffrn_reflns_av_unetI/netI     0.0590
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 1.000
_diffrn_reflns_limit_h_max       28
_diffrn_reflns_limit_h_min       -27
_diffrn_reflns_limit_k_max       25
_diffrn_reflns_limit_k_min       -25
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -24
_diffrn_reflns_number            125631
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 1.000
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.498
_diffrn_reflns_theta_min         1.423
_diffrn_source                   'fine-focus sealed tube'
_exptl_absorpt_coefficient_mu    0.409
_exptl_absorpt_correction_T_max  0.9667
_exptl_absorpt_correction_T_min  0.9150
_exptl_absorpt_correction_type   analytical
_exptl_absorpt_process_details
'based on measured indexed crystal faces, Bruker SHELXTL2014 (Sheldrick, 2014)'
_exptl_crystal_colour            orange
_exptl_crystal_density_diffrn    1.537
_exptl_crystal_description       plate
_exptl_crystal_F_000             3600
_exptl_crystal_size_max          0.325
_exptl_crystal_size_mid          0.224
_exptl_crystal_size_min          0.124
_refine_diff_density_max         0.759
_refine_diff_density_min         -0.564
_refine_diff_density_rms         0.073
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.947
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1021
_refine_ls_number_reflns         17576
_refine_ls_number_restraints     996
_refine_ls_restrained_S_all      0.925
_refine_ls_R_factor_all          0.0588
_refine_ls_R_factor_gt           0.0348
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0327P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0703
_refine_ls_wR_factor_ref         0.0777
_reflns_Friedel_coverage         0.000
_reflns_number_gt                12671
_reflns_number_total             17576
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            om6b00421_si_001.cif
_cod_data_source_block           sud14
_cod_original_sg_symbol_H-M      'P 21/c'
_cod_database_code               4088772
_shelx_estimated_absorpt_t_min   0.878
_shelx_estimated_absorpt_t_max   0.951
_shelxl_version_number           2014/6
_shelx_res_checksum              88909
_shelx_hkl_checksum              93692