Fully Localized Mixed-Valence Oxidation Products of Molecules Containing Two Linked Dimolybdenum Units: An Effective Structural Criterion
F. Albert Cotton; Naresh S. Dalal; Chun Y. Liu; Carlos A. Murillo; J. Micah North; Xiaoping Wang; Journal of the American Chemical Society 125 (2003) 12945–12952; doi:10.1021/ja036920+

data_4114284
_publ_section_title
;
 Fully Localized Mixed-Valence Oxidation Products of Molecules Containing
 Two Linked Dimolybdenum Units: An Effective Structural Criterion
;
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              12945
_journal_page_last               12952
_journal_paper_doi               10.1021/ja036920+
_journal_volume                  125
_journal_year                    2003
_chemical_formula_moiety         '[Mo2(C15H15N2O2)3]2Zn(OCH3)4(PF6),4(CH2Cl2)'
_chemical_formula_sum            'C98 H110 Cl8 F6 Mo4 N12 O16 P Zn'
_chemical_formula_weight         2589.68
_chemical_name_common            '[Mo2(DAniF)3]2Zn(OCH3)4(PF6),4(CH2Cl2)'
_space_group_IT_number           76
_symmetry_cell_setting           tetragonal
_symmetry_space_group_name_Hall  'P 4w'
_symmetry_space_group_name_H-M   'P 41'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   13.8487(3)
_cell_length_b                   13.8487(3)
_cell_length_c                   57.189(2)
_cell_measurement_reflns_used    28858
_cell_measurement_temperature    213(2)
_cell_measurement_theta_max      26.3525
_cell_measurement_theta_min      2.1190
_cell_volume                     10968.1(5)
_computing_cell_refinement       SMART
_computing_data_collection       SMART
_computing_data_reduction        SAINT
_computing_molecular_graphics    XP
_computing_publication_material  CIFTAB
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      213(2)
_diffrn_measured_fraction_theta_full 0.903
_diffrn_measured_fraction_theta_max 0.903
_diffrn_measurement_device_type  'BRUKER SMART 1000'
_diffrn_measurement_method       \w-scans
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'normal-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0464
_diffrn_reflns_av_sigmaI/netI    0.0662
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -3
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       72
_diffrn_reflns_limit_l_min       -28
_diffrn_reflns_number            35152
_diffrn_reflns_theta_full        26.74
_diffrn_reflns_theta_max         26.74
_diffrn_reflns_theta_min         1.51
_diffrn_standards_number         'none (area detector data)'
_exptl_absorpt_coefficient_mu    0.947
_exptl_absorpt_correction_T_max  0.8446
_exptl_absorpt_correction_T_min  0.6881
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   SADABS
_exptl_crystal_colour            'dark brown'
_exptl_crystal_density_diffrn    1.568
_exptl_crystal_description       block
_exptl_crystal_F_000             5252
_exptl_crystal_size_max          0.400
_exptl_crystal_size_mid          0.270
_exptl_crystal_size_min          0.178
_refine_diff_density_max         0.907
_refine_diff_density_min         -1.640
_refine_diff_density_rms         0.124
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   0.34(4)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.092
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1309
_refine_ls_number_reflns         14684
_refine_ls_number_restraints     31
_refine_ls_restrained_S_all      1.094
_refine_ls_R_factor_all          0.0785
_refine_ls_R_factor_gt           0.0696
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0466P)^2^+72.0594P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1619
_refine_ls_wR_factor_ref         0.1673
_reflns_number_gt                12924
_reflns_number_total             14684
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja0369202Bsi20030626_032614_1.cif
_cod_data_source_block           cmpd3
_cod_original_cell_volume        10968.1(6)
_cod_database_code               4114284