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_1514710
_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         'C76 H76 Mo2 N4 O8, 3(4 H8 O)'
_chemical_formula_sum            'C88 H100 Mo2 N4 O11'
_chemical_formula_weight         1581.6
_chemical_name_common            'Chisholm 1892'
_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             2013-01-04T12:38:10-00:00
_audit_creation_method           'WinGX routine CIF_UPDATE'
_cell_angle_alpha                74.31(3)
_cell_angle_beta                 76.48(3)
_cell_angle_gamma                72.72(3)
_cell_formula_units_Z            2
_cell_length_a                   12.843(3)
_cell_length_b                   16.816(3)
_cell_length_c                   21.696(4)
_cell_measurement_reflns_used    14939
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      25.028
_cell_measurement_theta_min      1.018
_cell_measurement_wavelength     0.71073
_cell_volume                     4247.0(17)
_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      0.581724E-1
_diffrn_orient_matrix_UB_12      -0.397376E-1
_diffrn_orient_matrix_UB_13      -0.246276E-1
_diffrn_orient_matrix_UB_21      0.474633E-1
_diffrn_orient_matrix_UB_22      0.413492E-1
_diffrn_orient_matrix_UB_23      -0.130064E-1
_diffrn_orient_matrix_UB_31      0.346885E-1
_diffrn_orient_matrix_UB_32      -0.279388E-1
_diffrn_orient_matrix_UB_33      0.397742E-1
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_unetI/netI     0.0644
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       25
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_number            14467
_diffrn_reflns_theta_full        24.71
_diffrn_reflns_theta_max         24.71
_diffrn_reflns_theta_min         2.57
_diffrn_source                   'Enraf Nonius FR590'
_exptl_absorpt_coefficient_mu    0.354
_exptl_absorpt_correction_T_max  0.958
_exptl_absorpt_correction_T_min  0.796
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'HKL Scalepack (Otwinowski & Minor, 1997)'
_exptl_crystal_colour            brown
_exptl_crystal_density_diffrn    1.237
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             1656
_exptl_crystal_size_max          0.27
_exptl_crystal_size_mid          0.23
_exptl_crystal_size_min          0.12
_platon_squeeze_void_average_x   0.500
_platon_squeeze_void_average_y   0.500
_platon_squeeze_void_average_z   0.000
_platon_squeeze_void_count_electrons 43
_platon_squeeze_void_nr          1
_platon_squeeze_void_volume      290
_refine_diff_density_max         0.929
_refine_diff_density_min         -0.508
_refine_diff_density_rms         0.085
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.08
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     946
_refine_ls_number_reflns         14467
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.08
_refine_ls_R_factor_all          0.0998
_refine_ls_R_factor_gt           0.059
_refine_ls_shift/su_max          0.035
_refine_ls_shift/su_mean         0.004
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0947P)^2^+1.0219P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1544
_refine_ls_wR_factor_ref         0.1682
_reflns_number_gt                9794
_reflns_number_total             14467
_reflns_threshold_expression     >2\s(I)
_cod_data_source_file            c3sc50322d.txt
_cod_data_source_block           sharlene2
_cod_depositor_comments
;

2019-04-22
Z value and formula fixed to values more according to usual
chemical conventions.                 miguel
;
_cod_original_cell_volume        4247.0(15)
_cod_original_formula_moiety
'C84 H92 Mo2 N4 O10, C76 H76 Mo2 N4 O8, 4(C4 H8 O)'
_cod_original_formula_sum        'C176 H200 Mo4 N8 O22'
_cod_original_formula_units_Z    1
_cod_original_formula_weight     3163.2
_cod_database_code               1514710