Extent of M2δ to Ligand π-Conjugation in Neutral and Mixed Valence States of Bis(4-isonicotinate)-bis(2,4,6-triisopropylbenzoate) Dimetal Complexes (MM), Where M = Mo or W, and Their Adducts with Tris(pentafluorophenyl)boron
Philip Bunting; Malcolm H. Chisholm; Judith C. Gallucci; Benjamin J. Lear; Journal of the American Chemical Society 133 (2011) 5873–5881; doi:10.1021/ja109522b

data_4105940
_publ_section_title
;
 Extent of M2\d to Ligand \p-Conjugation in Neutral and Mixed Valence
 States of Bis(4-isonicotinate)-bis(2,4,6-triisopropylbenzoate) Dimetal
 Complexes (MM), Where M = Mo or W, and Their Adducts with
 Tris(pentafluorophenyl)boron
;
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              5873
_journal_page_last               5881
_journal_paper_doi               10.1021/ja109522b
_journal_volume                  133
_journal_year                    2011
_chemical_compound_source        'synthesis as described'
_chemical_formula_moiety         'C80 H54 B2 F30 Mo2 N2 O8, C6 H14,  2(C4 H8 O)'
_chemical_formula_sum            'C94 H84 B2 F30 Mo2 N2 O10'
_chemical_formula_weight         2185.13
_chemical_name_common            'Chisholm 1774'
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_symmetry_Int_Tables_number      2
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     heavy
_atom_sites_solution_secondary   difmap
_audit_conform_dict_location     ftp://ftp.iucr.org/pub/cif_core.dic
_audit_conform_dict_name         cif_core.dic
_audit_conform_dict_version      2.4
_audit_creation_date             2010-07-07T11:33:46-00:00
_audit_creation_method           'WinGX routine CIF_UPDATE'
_cell_angle_alpha                115.641(1)
_cell_angle_beta                 94.922(1)
_cell_angle_gamma                96.875(1)
_cell_formula_units_Z            1
_cell_length_a                   10.4023(1)
_cell_length_b                   15.7963(1)
_cell_length_c                   16.9541(1)
_cell_measurement_reflns_used    8677
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      25.028
_cell_measurement_theta_min      2.037
_cell_measurement_wavelength     0.71073
_cell_volume                     2463.82(4)
_computing_cell_refinement       'HKL Scalepack (Otwinowski & Minor 1997)'
_computing_data_collection       'Collect (Nonius BV, 1997-2000)'
_computing_data_reduction
'HKL Denzo and Scalepack (Otwinowski & Minor 1997)'
_computing_molecular_graphics    'Ortep-3 for Windows (Farrugia, 1997)'
_computing_publication_material  'WinGX publication routines (Farrugia, 1999)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      150(2)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 9
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device       '95mm CCD camera on \k-goniostat'
_diffrn_measurement_device_type  'Nonius KappaCCD'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_orient_matrix_type       'by Nonius Collect from scalepack cell'
_diffrn_orient_matrix_UB_11      -0.890169E-1
_diffrn_orient_matrix_UB_12      0.153914E-1
_diffrn_orient_matrix_UB_13      -0.87335E-2
_diffrn_orient_matrix_UB_21      0.48237E-2
_diffrn_orient_matrix_UB_22      -0.215482E-1
_diffrn_orient_matrix_UB_23      -0.643268E-1
_diffrn_orient_matrix_UB_31      -0.406874E-1
_diffrn_orient_matrix_UB_32      -0.662178E-1
_diffrn_orient_matrix_UB_33      -0.130337E-1
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.032
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            69441
_diffrn_reflns_theta_full        25.02
_diffrn_reflns_theta_max         25.02
_diffrn_reflns_theta_min         2.23
_diffrn_source                   'Enraf Nonius FR590'
_exptl_absorpt_coefficient_mu    0.368
_exptl_absorpt_correction_T_max  0.946
_exptl_absorpt_correction_T_min  0.883
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'HKL Scalepack (Otwinowski & Minor, 1997)'
_exptl_crystal_colour            'dark brown'
_exptl_crystal_density_diffrn    1.473
_exptl_crystal_description       'rectangular block'
_exptl_crystal_F_000             1106
_exptl_crystal_size_max          0.31
_exptl_crystal_size_mid          0.23
_exptl_crystal_size_min          0.15
_platon_squeeze_details
;
;
_refine_diff_density_max         0.469
_refine_diff_density_min         -0.339
_refine_diff_density_rms         0.057
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.048
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     659
_refine_ls_number_reflns         8688
_refine_ls_number_restraints     54
_refine_ls_restrained_S_all      1.049
_refine_ls_R_factor_all          0.0381
_refine_ls_R_factor_gt           0.0316
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0488P)^2^+1.2054P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0835
_refine_ls_wR_factor_ref         0.0865
_reflns_number_gt                7589
_reflns_number_total             8688
_reflns_threshold_expression     >2\s(I)
_cod_data_source_file            ja109522b_si_003.cif
_cod_data_source_block           shelxl
_cod_original_cell_volume        2463.82(3)
_cod_database_code               4105940