MM Quadruply Bonded Complexes Supported by Vinylbenzoate Ligands: Synthesis, Characterization, Photophysical Properties and Application as Synthons.
Brown-Xu, Samantha E; Chisholm, Malcolm H.; Durr, Christopher B.; Spilker, Thomas F.; Young, Philip J.; Chemical science (Royal Society of Chemistry : 2010) 6 (2015) 1780–1791; doi:10.1039/C4SC02542C

data_1518544
_publ_section_title
;
 MM Quadruply Bonded Complexes Supported by Vinylbenzoate Ligands:
 Synthesis, Characterization, Photophysical Properties and Application as
 Synthons.
;
_journal_issue                   3
_journal_name_full
'Chemical science (Royal Society of Chemistry : 2010)'
_journal_page_first              1780
_journal_page_last               1791
_journal_paper_doi               10.1039/C4SC02542C
_journal_volume                  6
_journal_year                    2015
_chemical_formula_sum            'C58 H76 Mo2 O10'
_chemical_formula_weight         1125.06
_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
_audit_conform_dict_location     ftp://ftp.iucr.org/pub/cif_core.dic
_audit_conform_dict_name         cif_core.dic
_audit_conform_dict_version      2.4.3
_audit_creation_date             2014-07-22T13:15:58-00:00
_audit_creation_method           'WinGX routine CIF_UPDATE'
_audit_update_record
;
2014-07-23 deposited with the CCDC.
2014-12-09 downloaded from the CCDC.
;
_cell_angle_alpha                107.0000(10)
_cell_angle_beta                 105.1650(10)
_cell_angle_gamma                90.1140(10)
_cell_formula_units_Z            1
_cell_length_a                   9.8343(2)
_cell_length_b                   11.2520(2)
_cell_length_c                   15.7140(3)
_cell_measurement_reflns_used    7302
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      27.48
_cell_measurement_theta_min      1.02
_cell_measurement_wavelength     0.71073
_cell_volume                     1599.14(5)
_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 for Windows (Farrugia, 2012)'
_computing_publication_material  'WinGX publication routines (Farrugia, 2012)'
_computing_structure_refinement  'SHELXL-2014 (Sheldrick, 2014)'
_diffrn_ambient_temperature      150(2)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 9
_diffrn_measured_fraction_theta_full 1
_diffrn_measured_fraction_theta_max 0.998
_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_UB_11      -0.099414
_diffrn_orient_matrix_UB_12      0.020285
_diffrn_orient_matrix_UB_13      -0.00159
_diffrn_orient_matrix_UB_21      0.029537
_diffrn_orient_matrix_UB_22      0.039413
_diffrn_orient_matrix_UB_23      0.068629
_diffrn_orient_matrix_UB_31      0.020605
_diffrn_orient_matrix_UB_32      0.082065
_diffrn_orient_matrix_UB_33      -0.008701
_diffrn_radiation_monochromator  'horizonally mounted graphite crystal'
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.038
_diffrn_reflns_Laue_measured_fraction_full 1
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            14219
_diffrn_reflns_point_group_measured_fraction_full 1
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.467
_diffrn_reflns_theta_min         1.899
_diffrn_source                   'Enraf Nonius FR590'
_exptl_absorpt_coefficient_mu    0.44
_exptl_absorpt_correction_T_max  0.936
_exptl_absorpt_correction_T_min  0.774
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'HKL Scalepack (Otwinowski & Minor, 1997)'
_exptl_crystal_colour            orange
_exptl_crystal_density_diffrn    1.168
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             588
_exptl_crystal_size_max          0.23
_exptl_crystal_size_mid          0.23
_exptl_crystal_size_min          0.15
_platon_squeeze_details
;                         
  A net of residual "Q" peaks remained in the difference map after the
 final refinement that could not be adequately modeled as solvent. The PLATON 
 squeeze program was utilized to remove the residual electron density. The program
 removed 45 electrons from the solvent accessible void which correlates 
 to highly disordered hexanes which was used in crystalization.
  
;
_refine_diff_density_max         0.559
_refine_diff_density_min         -0.477
_refine_diff_density_rms         0.084
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.06
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_constraints    0
_refine_ls_number_parameters     326
_refine_ls_number_reflns         7310
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.064
_refine_ls_R_factor_all          0.0496
_refine_ls_R_factor_gt           0.0378
_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^)+(0.0572P)^2^+0.4904P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0978
_refine_ls_wR_factor_ref         0.1038
_reflns_number_gt                6114
_reflns_number_total             7310
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c4sc02542c2.cif
_cod_data_source_block           CBD018
_cod_depositor_comments
;Adding full bibliography for 1518543--1518544.cif.

 Adding full bibliography for 1518543--1518544.cif.
;
_cod_database_code               1518544