Molybdenum–molybdenum quadruple bonds supported by 9,10-anthraquinone carboxylate ligands. Molecular, electronic, ground state and unusual photoexcited state properties
Brown-Xu, Samantha E.; Chisholm, Malcolm H.; Durr, Christopher B.; Lewis, Sharlene A.; Spilker, Thomas F.; Young, Philip J.; Chemical Science 5 (2014) 2657–; doi:10.1039/c4sc00341a

data_1515906
_publ_section_title
;
 Molybdenum--molybdenum quadruple bonds supported by 9,10-anthraquinone
 carboxylate ligands. Molecular, electronic, ground state and unusual
 photoexcited state properties
;
_journal_issue                   7
_journal_name_full               'Chemical Science'
_journal_page_first              2657
_journal_paper_doi               10.1039/c4sc00341a
_journal_volume                  5
_journal_year                    2014
_chemical_compound_source        'synthesis as described'
_chemical_formula_moiety         'C60 H52 Mo2 N6 O10'
_chemical_formula_sum            'C60 H52 Mo2 N6 O10'
_chemical_formula_weight         1208.96
_chemical_name_common            Chisholm1929
_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     direct
_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             2013-02-04
_audit_creation_method           'WinGX routine CIF_UPDATE'
_cell_angle_alpha                100.1970(10)
_cell_angle_beta                 100.3510(10)
_cell_angle_gamma                100.7980(10)
_cell_formula_units_Z            2
_cell_length_a                   9.8000(2)
_cell_length_b                   12.6442(2)
_cell_length_c                   23.2653(3)
_cell_measurement_reflns_used    12416
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      27.485
_cell_measurement_theta_min      1.018
_cell_measurement_wavelength     0.71073
_cell_volume                     2718.72(8)
_computing_cell_refinement       'HKL Scalepack (Otwinowski & Minor 1997)'
_computing_data_collection       'Collect (Bruker AXS BV, 1997-2004)'
_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)'
_diffrn_ambient_temperature      150(2)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 9
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device       '95mm CCD camera on \k-goniostat'
_diffrn_measurement_device_type  KappaCCD
_diffrn_measurement_method       CCD
_diffrn_orient_matrix_type       'by Bruker AXS Collect from scalepack cell'
_diffrn_orient_matrix_UB_11      0.0575213
_diffrn_orient_matrix_UB_12      0.0524242
_diffrn_orient_matrix_UB_13      0.0376043
_diffrn_orient_matrix_UB_21      0.0558873
_diffrn_orient_matrix_UB_22      0.0418399
_diffrn_orient_matrix_UB_23      -0.0240705
_diffrn_orient_matrix_UB_31      -0.0700618
_diffrn_orient_matrix_UB_32      0.0480319
_diffrn_orient_matrix_UB_33      -0.0033091
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.052
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       30
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_number            12452
_diffrn_reflns_theta_full        27.47
_diffrn_reflns_theta_max         27.47
_diffrn_reflns_theta_min         1.68
_diffrn_source                   'Enraf Nonius FR590'
_exptl_absorpt_coefficient_mu    0.527
_exptl_absorpt_correction_T_max  0.939
_exptl_absorpt_correction_T_min  0.837
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'HKL Scalepack (Otwinowski & Minor, 1997)'
_exptl_crystal_colour            'dark green'
_exptl_crystal_density_diffrn    1.477
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       rod
_exptl_crystal_F_000             1236
_exptl_crystal_size_max          0.38
_exptl_crystal_size_mid          0.15
_exptl_crystal_size_min          0.12
_platon_squeeze_details
;
 Several residual "Q" peaks remained in the difference map after final 
 refinement that could not be modeled as solvent. The PLATON squeeze 
 program was utilized to remove the residual electron density. The program
 removed 30 electrons from the solvent accessible void which likely correlates 
 to disordered Hexanes which was used in crystallization. 
;
_platon_squeeze_void_average_x   0.000
_platon_squeeze_void_average_y   0.500
_platon_squeeze_void_average_z   0.500
_platon_squeeze_void_content     Hexanes
_platon_squeeze_void_count_electrons 30
_platon_squeeze_void_volume      122
_refine_diff_density_max         1.253
_refine_diff_density_min         -0.402
_refine_diff_density_rms         0.082
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.022
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     703
_refine_ls_number_reflns         12452
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.022
_refine_ls_R_factor_all          0.0843
_refine_ls_R_factor_gt           0.0449
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0595P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1006
_refine_ls_wR_factor_ref         0.1108
_reflns_number_gt                8230
_reflns_number_total             12452
_reflns_threshold_expression     >2\s(I)
_cod_data_source_file            c4sc00341a2.cif
_cod_data_source_block           global
_cod_depositor_comments          'Adding full bibliography for 1515906.cif.'
_cod_original_sg_symbol_H-M      P-1
_cod_database_code               1515906