MM quadruple bonds supported by cyanoacrylate ligands. Extending photon harvesting into the near infrared and studies of the MLCT states
Brown-Xu, Samantha E.; Chisholm, Malcolm H.; Durr, Christopher B.; Lewis, Sharlene A.; Naseri, Vesal; Spilker, Thomas F.; Chemical Science 4 (2013) 2105–; doi:10.1039/c3sc50322d

data_1514709
_publ_section_title
;
 MM quadruple bonds supported by cyanoacrylate ligands. Extending photon
 harvesting into the near infrared and studies of the MLCT states
;
_journal_issue                   5
_journal_name_full               'Chemical Science'
_journal_page_first              2105
_journal_paper_doi               10.1039/c3sc50322d
_journal_volume                  4
_journal_year                    2013
_chemical_compound_source        'synthesis as described'
_chemical_formula_moiety         'C84 H80 Mo2 N4 O8 S2, 2(C4 H8 O)'
_chemical_formula_sum            'C92 H96 Mo2 N4 O10 S2'
_chemical_formula_weight         1673.73
_chemical_name_common            'Chisholm 1904'
_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             2012-07-05T18:16:19-00:00
_audit_creation_method           'WinGX routine CIF_UPDATE'
_cell_angle_alpha                81.3950(10)
_cell_angle_beta                 89.3820(10)
_cell_angle_gamma                84.0390(10)
_cell_formula_units_Z            1
_cell_length_a                   12.6203(2)
_cell_length_b                   13.1151(2)
_cell_length_c                   13.4075(2)
_cell_measurement_reflns_used    7670
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      25.028
_cell_measurement_theta_min      1.018
_cell_measurement_wavelength     0.71073
_cell_volume                     2182.29(6)
_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 rotation images, thick slices'
_diffrn_orient_matrix_type       'by Bruker AXS Collect from scalepack cell'
_diffrn_orient_matrix_UB_11      0.767793E-1
_diffrn_orient_matrix_UB_12      -0.76053E-2
_diffrn_orient_matrix_UB_13      -0.195719E-1
_diffrn_orient_matrix_UB_21      -0.58992E-2
_diffrn_orient_matrix_UB_22      0.748025E-1
_diffrn_orient_matrix_UB_23      -0.30408E-1
_diffrn_orient_matrix_UB_31      0.20428E-1
_diffrn_orient_matrix_UB_32      0.189184E-1
_diffrn_orient_matrix_UB_33      0.662024E-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  0.042
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_number            14970
_diffrn_reflns_theta_full        25.02
_diffrn_reflns_theta_max         25.02
_diffrn_reflns_theta_min         1.54
_diffrn_source                   'Enraf Nonius FR590'
_exptl_absorpt_coefficient_mu    0.393
_exptl_absorpt_correction_T_max  0.9433
_exptl_absorpt_correction_T_min  0.524
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'HKL Scalepack (Otwinowski & Minor, 1997)'
_exptl_crystal_colour            brown
_exptl_crystal_density_diffrn    1.274
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             872
_exptl_crystal_size_max          0.23
_exptl_crystal_size_mid          0.19
_exptl_crystal_size_min          0.15
_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 33 electrons from the solvent accessible void which correlates to
one disordered THF molecule.
;
_platon_squeeze_void_average_x   0.500
_platon_squeeze_void_average_y   1.000
_platon_squeeze_void_average_z   0.500
_platon_squeeze_void_content     THF
_platon_squeeze_void_count_electrons 33
_platon_squeeze_void_volume      162
_refine_diff_density_max         0.568
_refine_diff_density_min         -0.412
_refine_diff_density_rms         0.065
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.079
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     515
_refine_ls_number_reflns         7685
_refine_ls_number_restraints     3
_refine_ls_restrained_S_all      1.08
_refine_ls_R_factor_all          0.0467
_refine_ls_R_factor_gt           0.0347
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0530P)^2^+0.3378P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.085
_refine_ls_wR_factor_ref         0.0924
_reflns_number_gt                6377
_reflns_number_total             7685
_reflns_threshold_expression     >2\s(I)
_cod_data_source_file            c3sc50322d.txt
_cod_data_source_block           importp
_cod_original_sg_symbol_H-M      P-1
_cod_database_code               1514709