Mixed Valency in Hydrogen Bonded 'Dimers of Dimers'
Luke A. Wilkinson; Laura McNeill; Anthony J. H. M. Meijer; Nathan J. Patmore; Journal of the American Chemical Society 135 (2013) 1723–1726; doi:10.1021/ja312176x

data_4119308
_publ_section_title
;
 Mixed Valency in Hydrogen Bonded 'Dimers of Dimers'
;
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              1723
_journal_page_last               1726
_journal_paper_doi               10.1021/ja312176x
_journal_volume                  135
_journal_year                    2013
_chemical_formula_moiety         'C84 H102 F6 Mo4 N4 O16, 2(C4 H8 O)'
_chemical_formula_sum            'C92 H118 F6 Mo4 N4 O18'
_chemical_formula_weight         2065.66
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_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_creation_method           SHELXL-97
_cell_angle_alpha                93.888(3)
_cell_angle_beta                 103.095(3)
_cell_angle_gamma                93.820(3)
_cell_formula_units_Z            1
_cell_length_a                   11.7619(11)
_cell_length_b                   14.1426(13)
_cell_length_c                   14.8459(13)
_cell_measurement_reflns_used    1815
_cell_measurement_temperature    120(2)
_cell_measurement_theta_max      20.984
_cell_measurement_theta_min      2.489
_cell_volume                     2391.2(4)
_computing_cell_refinement       'Bruker SMART'
_computing_data_collection       'Bruker SMART'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'Bruker SHELXTL'
_diffrn_ambient_temperature      120(2)
_diffrn_measured_fraction_theta_full 0.989
_diffrn_measured_fraction_theta_max 0.969
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0727
_diffrn_reflns_av_sigmaI/netI    0.1547
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            22287
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         27.53
_diffrn_reflns_theta_min         2.39
_exptl_absorpt_coefficient_mu    0.590
_exptl_absorpt_correction_T_max  0.9711
_exptl_absorpt_correction_T_min  0.9326
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   sadabs
_exptl_crystal_colour            orange
_exptl_crystal_density_diffrn    1.434
_exptl_crystal_description       block
_exptl_crystal_F_000             1064
_exptl_crystal_size_max          0.12
_exptl_crystal_size_mid          0.09
_exptl_crystal_size_min          0.05
_refine_diff_density_max         2.244
_refine_diff_density_min         -0.882
_refine_diff_density_rms         0.132
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.990
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     552
_refine_ls_number_reflns         10696
_refine_ls_number_restraints     43
_refine_ls_restrained_S_all      0.994
_refine_ls_R_factor_all          0.1597
_refine_ls_R_factor_gt           0.0734
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0945P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1707
_refine_ls_wR_factor_ref         0.2113
_reflns_number_gt                5341
_reflns_number_total             10696
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja312176x_si_002_2.cif
_cod_data_source_block           '[3]2.2THF'
_cod_database_code               4119308