Combination of Redox-Active Ligand and Lewis Acid for Dioxygen Reduction with π-Bound Molybdenum-Quinonoid Complexes.
Henthorn, Justin T.; Lin, Sibo; Agapie, Theodor; Journal of the American Chemical Society 137 (2015) 1458–1464; doi:10.1021/ja5100405

data_4123389
_publ_section_title
;
 Combination of Redox-Active Ligand and Lewis Acid for Dioxygen Reduction
 with \p-Bound Molybdenum-Quinonoid Complexes.
;
_journal_issue                   4
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              1458
_journal_page_last               1464
_journal_paper_doi               10.1021/ja5100405
_journal_volume                  137
_journal_year                    2015
_chemical_formula_moiety
'2(C35 H44 Mo O5 P2), B2 C36 F30 O2, 2(C H2 Cl2)'
_chemical_formula_sum            'C108 H92 B2 Cl4 F30 Mo2 O12 P4'
_chemical_formula_weight         2631.00
_chemical_name_systematic
;
 ? 
;
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_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_date             2014-09-18
_audit_creation_method
;
Olex2 1.2
(compiled 2014.08.28 svn.r2986 for OlexSys, GUI svn.r4874)
;
_cell_angle_alpha                64.704(3)
_cell_angle_beta                 81.599(3)
_cell_angle_gamma                85.342(3)
_cell_formula_units_Z            1
_cell_length_a                   12.5114(11)
_cell_length_b                   15.1452(14)
_cell_length_c                   15.6129(14)
_cell_measurement_reflns_used    6446
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      20.87
_cell_measurement_theta_min      2.33
_cell_volume                     2645.5(4)
_computing_cell_refinement       'SAINT v8.34A (Bruker, 2013)'
_computing_data_reduction        'SAINT v8.34A (Bruker, 2013)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'XL (Sheldrick, 2008)'
_computing_structure_solution    'XS (Sheldrick, 2008)'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 1.000
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.1382
_diffrn_reflns_av_unetI/netI     0.1706
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            75389
_diffrn_reflns_theta_full        27.48
_diffrn_reflns_theta_max         27.48
_diffrn_reflns_theta_min         1.45
_diffrn_source                   'fine-focus sealed tube'
_exptl_absorpt_coefficient_mu    0.514
_exptl_absorpt_correction_T_max  0.7460
_exptl_absorpt_correction_T_min  0.6860
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
'SADABS-2014/2 (Bruker,2014) was used for absorption correction. wR2(int) was 0.0695 before and 0.0621 after correction. The Ratio of minimum to maximum transmission is 0.9196. The \l/2 correction factor is 0.00150.'
_exptl_crystal_colour            violet
_exptl_crystal_colour_primary    violet
_exptl_crystal_density_diffrn    1.651
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       blade
_exptl_crystal_F_000             1328
_exptl_crystal_size_max          0.396
_exptl_crystal_size_mid          0.186
_exptl_crystal_size_min          0.11
_refine_diff_density_max         1.602
_refine_diff_density_min         -0.899
_refine_diff_density_rms         0.103
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.901
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     761
_refine_ls_number_reflns         12147
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.901
_refine_ls_R_factor_all          0.1379
_refine_ls_R_factor_gt           0.0576
_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^)+(0.0636P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1258
_refine_ls_wR_factor_ref         0.1453
_reflns_number_gt                5994
_reflns_number_total             12147
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja5100405_si_001.cif
_cod_data_source_block           4+
_cod_depositor_comments
'Adding full bibliography for 4123386--4123389.cif.'
_cod_database_code               4123389
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups, All C(H,H,H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Others
 Sof(H28A)=Sof(C30A)=Sof(H30A)=Sof(H30B)=Sof(H30C)=1-FVAR(1)
 Sof(H28)=Sof(C30B)=Sof(H30D)=Sof(H30E)=Sof(H30F)=FVAR(1)
 Sof(H54C)=Sof(H54D)=Sof(Cl2B)=1-FVAR(2)
 Sof(Cl2A)=Sof(H54A)=Sof(H54B)=FVAR(2)
3.a Ternary CH refined with riding coordinates:
 C19(H19), C22(H22), C28(H28A), C28(H28), C25(H25)
3.b Secondary CH2 refined with riding coordinates:
 C54(H54A,H54B), C54(H54C,H54D)
3.c Aromatic/amide H refined with riding coordinates:
 C2(H2), C3(H3), C4(H4), C5(H5), C8(H8), C9(H9), C14(H14), C15(H15), C16(H16),
 C17(H17)
3.d Idealised Me refined as rotating group:
 C20(H20A,H20B,H20C), C21(H21A,H21B,H21C), C24(H24A,H24B,H24C), C23(H23A,H23B,
 H23C), C29(H29A,H29B,H29C), C27(H27A,H27B,H27C), C26(H26A,H26B,H26C), C31(H31A,
 H31B,H31C), C32(H32A,H32B,H32C), C30A(H30A,H30B,H30C), C30B(H30D,H30E,H30F)
;
_olex2_submission_special_instructions 'No special instructions were received'