Quadruply Bonded Dimolybdenum Atoms Surrounded by Dendrons: Preparation, Characterization, and Electrochemistry
Teerayuth Liwporncharoenvong; Rudy L. Luck; Journal of the American Chemical Society 123 (2001) 3615–3616; doi:10.1021/ja0155130

data_4115475
_publ_contact_author             'Luck, Rudy L.'
_publ_contact_author_email       rluck@mtu.edu
_publ_section_title
;
 Quadruply Bonded Dimolybdenum Atoms Surrounded by Dendrons: Preparation,
 Characterization, and Electrochemistry
;
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              3615
_journal_page_last               3616
_journal_paper_doi               10.1021/ja0155130
_journal_volume                  123
_journal_year                    2001
_chemical_compound_source        'synthesis as described'
_chemical_formula_moiety         'C14 H10 Cl0.5 K0.50 Mo O8'
_chemical_formula_structural     'C28 H20 Cl1 K1 Mo2 O16'
_chemical_formula_sum            'C14 H10 Cl0.5 K0.5 Mo O8'
_chemical_formula_weight         439.44
_chemical_name_systematic
;
  ?
;
_space_group_IT_number           22
_symmetry_cell_setting           orthorhombic
_symmetry_Int_Tables_number      22
_symmetry_space_group_name_Hall  'F 2 2'
_symmetry_space_group_name_H-M   'F 2 2 2'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_date             2001-03-20T21:58:18-00:00
_audit_creation_method           'WinGX routine CIF_UPDATE'
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   13.060(3)
_cell_length_b                   19.961(6)
_cell_length_c                   19.985(6)
_cell_measurement_reflns_used    22
_cell_measurement_temperature    291(2)
_cell_measurement_theta_max      16
_cell_measurement_theta_min      8
_cell_measurement_wavelength     0.71073
_cell_volume                     5210(3)
_computing_cell_refinement       'CAD4 Express (Enraf Nonius, 1994)'
_computing_data_collection       'CAD4 Express (Enraf Nonius, 1994)'
_computing_data_reduction        'XCAD4 (Harms & Wocadlo, 1995)'
_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    'SIR97 (Altomare et al., 1999)'
_diffrn_ambient_temperature      291(2)
_diffrn_detector                 'scintillation LiI'
_diffrn_detector_dtime           1.195
_diffrn_measured_fraction_theta_full 1
_diffrn_measured_fraction_theta_max 1
_diffrn_measurement_device       '\k-geometry diffractometer'
_diffrn_measurement_device_type  'Enraf Nonius TurboCAD4'
_diffrn_measurement_method       'non-profiled omega/2theta scans'
_diffrn_orient_matrix_type
;
   x-axis points to radiation source
   the matrix is specified in reciprocal space
;
_diffrn_orient_matrix_UB_11      0.64056E-1
_diffrn_orient_matrix_UB_12      0.21022E-1
_diffrn_orient_matrix_UB_13      -0.17568E-1
_diffrn_orient_matrix_UB_21      -0.04036
_diffrn_orient_matrix_UB_22      0.22194E-1
_diffrn_orient_matrix_UB_23      -0.36273E-1
_diffrn_orient_matrix_UB_31      -0.11442E-1
_diffrn_orient_matrix_UB_32      0.03969
_diffrn_orient_matrix_UB_33      0.29655E-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  0.0191
_diffrn_reflns_av_unetI/netI     0.057
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       0
_diffrn_reflns_limit_k_max       21
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -1
_diffrn_reflns_number            1014
_diffrn_reflns_theta_full        22.42
_diffrn_reflns_theta_max         22.42
_diffrn_reflns_theta_min         2.03
_diffrn_source                   'Enraf Nonius FR590'
_diffrn_standards_decay_%        1
_diffrn_standards_interval_time  166
_diffrn_standards_number         3
_exptl_absorpt_coefficient_mu    0.659
_exptl_absorpt_correction_T_max  0.8991
_exptl_absorpt_correction_T_min  0.7707
_exptl_absorpt_correction_type   psi-scan
_exptl_absorpt_process_details   '(North, Phillips & Mathews, 1968)'
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.12
_exptl_crystal_description       prism
_exptl_crystal_F_000             1744
_exptl_crystal_size_max          0.2
_exptl_crystal_size_mid          0.2
_exptl_crystal_size_min          0.1
_refine_diff_density_max         1.633
_refine_diff_density_min         -0.769
_refine_diff_density_rms         0.27
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   -0.5(6)
_refine_ls_extinction_coef       0.0009(2)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     SHELXL
_refine_ls_goodness_of_fit_ref   1.212
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     93
_refine_ls_number_reflns         1012
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.212
_refine_ls_R_factor_all          0.1034
_refine_ls_R_factor_gt           0.079
_refine_ls_shift/su_max          0
_refine_ls_shift/su_mean         0
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.1484P)^2^+126.7681P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2367
_refine_ls_wR_factor_ref         0.2517
_reflns_number_gt                819
_reflns_number_total             1012
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja0155130.cif
_cod_data_source_block           yuthmo2
_cod_original_cell_volume        5210(2)
_cod_original_formula_sum        'C14 H10 Cl0.5 K0.50 Mo O8'
_cod_database_code               4115475
_exptl_absorpt_factor_mur        0.105
_exptl_absorpt_correction_t_ave  0.8375
_diffrn_standards_decay_corr_max 1.026
_diffrn_standards_decay_corr_min 0.992