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_4123386
_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(C33 H40 Mo O5 P2), 4.5(C6 H6)'
_chemical_formula_sum            'C93 H107 Mo2 O10 P4'
_chemical_formula_weight         1700.55
_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                106.621(3)
_cell_angle_beta                 91.522(3)
_cell_angle_gamma                109.707(3)
_cell_formula_units_Z            2
_cell_length_a                   11.9691(7)
_cell_length_b                   16.9351(10)
_cell_length_c                   22.8410(13)
_cell_measurement_reflns_used    9679
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      38.02
_cell_measurement_theta_min      2.43
_cell_volume                     4137.5(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    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_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  0.0558
_diffrn_reflns_av_unetI/netI     0.0243
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       23
_diffrn_reflns_limit_k_min       -23
_diffrn_reflns_limit_l_max       32
_diffrn_reflns_limit_l_min       -32
_diffrn_reflns_number            295474
_diffrn_reflns_theta_full        30.00
_diffrn_reflns_theta_max         30.00
_diffrn_reflns_theta_min         1.84
_diffrn_source                   'fine-focus sealed tube'
_exptl_absorpt_coefficient_mu    0.440
_exptl_absorpt_correction_T_max  0.7478
_exptl_absorpt_correction_T_min  0.6687
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
'SADABS-2014/2 (Bruker,2014) was used for absorption correction. wR2(int) was 0.0722 before and 0.0634 after correction. The Ratio of minimum to maximum transmission is 0.8942. The \l/2 correction factor is 0.00150.'
_exptl_crystal_colour            orange
_exptl_crystal_colour_primary    orange
_exptl_crystal_density_diffrn    1.365
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       blade
_exptl_crystal_F_000             1778
_exptl_crystal_size_max          0.436
_exptl_crystal_size_mid          0.404
_exptl_crystal_size_min          0.155
_refine_diff_density_max         1.977
_refine_diff_density_min         -1.765
_refine_diff_density_rms         0.114
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.633
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1002
_refine_ls_number_reflns         24087
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.633
_refine_ls_R_factor_all          0.0613
_refine_ls_R_factor_gt           0.0506
_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^)+(0.1000P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1879
_refine_ls_wR_factor_ref         0.2015
_reflns_number_gt                20634
_reflns_number_total             24087
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja5100405_si_001.cif
_cod_data_source_block           2a
_cod_depositor_comments
'Adding full bibliography for 4123386--4123389.cif.'
_cod_database_code               4123386
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
 At 1.5 times of:
  All C(H,H,H) groups, All O(H) groups
2.a Ternary CH refined with riding coordinates:
 C19(H19), C22(H22), C25(H25), C28(H28), C58(H58), C61(H61), C64(H64), C67(H67)
2.b Aromatic/amide H refined with riding coordinates:
 C2(H2A), C3(H3), C4(H4), C5(H5), C8(H8), C9(H9), C14(H14), C15(H15), C16(H16),
  C17(H17), C41(H41), C42(H42), C43(H43), C44(H44), C47(H47), C48(H48),
 C54(H54), C55(H55), C56(H56), C57(H57), C34(H34), C35(H35), C36(H36), C37(H37),
  C38(H38), C39(H39), C106(H106), C107(H107), C108(H108), C109(H109),
 C110(H110), C111(H111), C145(H145), C146(H146), C147(H147), C151(H151),
 C152(H152), C153(H153), C154(H154), C155(H155), C156(H156), C175(H175),
 C176(H176), C177(H177), C178(H178), C179(H179), C180(H180)
2.c Idealised Me refined as rotating group:
 C20(H20A,H20B,H20C), C21(H21A,H21B,H21C), C23(H23A,H23B,H23C), C24(H24A,H24B,
 H24C), C26(H26A,H26B,H26C), C27(H27A,H27B,H27C), C29(H29A,H29B,H29C), C30(H30A,
 H30B,H30C), C59(H59A,H59B,H59C), C60(H60A,H60B,H60C), C62(H62A,H62B,H62C),
 C63(H63A,H63B,H63C), C65(H65A,H65B,H65C), C66(H66A,H66B,H66C), C68(H68A,H68B,
 H68C), C69(H69A,H69B,H69C)
2.d Idealised tetrahedral OH refined as rotating group:
 O1(H1), O2(H2), O6(H6), O7(H7)
;
_olex2_submission_special_instructions 'No special instructions were received'