Quadruply Bonded Dimetal Units Supported by 2,4,6-Triisopropylbenzoates MM(TiPB)4 (MM = Mo2, MoW, and W2): Preparation and Photophysical Properties
Brian G. Alberding; Malcolm H. Chisholm; Yi-Hsuan Chou; Judith C. Gallucci; Yagnaseni Ghosh; Terry L. Gustafson; Nathan J. Patmore; Carly R. Reed; Claudia Turro; Inorganic Chemistry 48 (2009) 4394–4399; doi:10.1021/ic900092c

data_4302127
_publ_section_title
;
Quadruply Bonded Dimetal Units Supported by 2,4,6-Triisopropylbenzoates
MM(TiPB)4 (MM = Mo2, MoW, and W2): Preparation and Photophysical Properties
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              4394
_journal_page_last               4399
_journal_paper_doi               10.1021/ic900092c
_journal_volume                  48
_journal_year                    2009
_chemical_compound_source        'synthesis as described'
_chemical_formula_moiety         'C64 H92 O8 W2, 2(C4 H8 O)'
_chemical_formula_sum            'C72 H108 O10 W2'
_chemical_formula_weight         1501.28
_chemical_name_common            'Chisholm 1695'
_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             2009-01-07T17:24:05-00:00
_audit_creation_method           'WinGX routine CIF_UPDATE'
_cell_angle_alpha                67.441(1)
_cell_angle_beta                 70.731(1)
_cell_angle_gamma                88.835(1)
_cell_formula_units_Z            1
_cell_length_a                   11.8352(1)
_cell_length_b                   12.2014(1)
_cell_length_c                   14.1662(1)
_cell_measurement_reflns_used    8090
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      27.485
_cell_measurement_theta_min      2.037
_cell_measurement_wavelength     0.71073
_cell_volume                     1770.03(3)
_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, 1997)'
_computing_structure_solution    'SHELXS-96 (Sheldrick, 1986)'
_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      -0.566925E-1
_diffrn_orient_matrix_UB_12      -0.325587E-1
_diffrn_orient_matrix_UB_13      -0.245591E-1
_diffrn_orient_matrix_UB_21      -0.96703E-2
_diffrn_orient_matrix_UB_22      -0.798794E-1
_diffrn_orient_matrix_UB_23      0.607796E-1
_diffrn_orient_matrix_UB_31      -0.694618E-1
_diffrn_orient_matrix_UB_32      0.235427E-1
_diffrn_orient_matrix_UB_33      0.48537E-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  0.044
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            52154
_diffrn_reflns_theta_full        27.51
_diffrn_reflns_theta_max         27.51
_diffrn_reflns_theta_min         2.42
_diffrn_source                   'Enraf Nonius FR590'
_exptl_absorpt_coefficient_mu    3.301
_exptl_absorpt_correction_T_max  0.468
_exptl_absorpt_correction_T_min  0.385
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'HKL Scalepack (Otwinowski & Minor, 1997)'
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    1.408
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       'almost cube shaped chunk'
_exptl_crystal_F_000             768
_exptl_crystal_size_max          0.23
_exptl_crystal_size_mid          0.23
_exptl_crystal_size_min          0.23
_refine_diff_density_max         1.09
_refine_diff_density_min         -0.828
_refine_diff_density_rms         0.093
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     389
_refine_ls_number_reflns         8121
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1
_refine_ls_R_factor_all          0.0401
_refine_ls_R_factor_gt           0.027
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0336P)^2^+0.3076P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.059
_refine_ls_wR_factor_ref         0.0628
_reflns_number_gt                6819
_reflns_number_total             8121
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic900092c_si_001.cif
_cod_data_source_block           Chisholm1695
_cod_original_cell_volume        1770.03(2)
_cod_database_code               4302127