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_4123387
_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         'C35 H44 Mo O5 P2 Si, C2 H3 N'
_chemical_formula_sum            'C37 H47 Mo N O5 P2 Si'
_chemical_formula_weight         771.73
_chemical_name_systematic
;
 ? 
;
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2ybc'
_space_group_name_H-M_alt        'P 1 21/c 1'
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     iterative
_atom_sites_solution_secondary   difmap
_audit_creation_date             2014-09-17
_audit_creation_method
;
Olex2 1.2
(compiled 2014.08.28 svn.r2986 for OlexSys, GUI svn.r4874)
;
_cell_angle_alpha                90.00
_cell_angle_beta                 102.3990(10)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   11.4020(4)
_cell_length_b                   17.1733(7)
_cell_length_c                   19.0484(7)
_cell_measurement_reflns_used    9854
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      31.689
_cell_measurement_theta_min      2.325
_cell_volume                     3642.9(2)
_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    'olex2.solve (Bourhis et al., 2013)'
_diffrn_ambient_temperature      100.0
_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  0.1725
_diffrn_reflns_av_unetI/netI     0.0772
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       25
_diffrn_reflns_limit_k_min       -26
_diffrn_reflns_limit_l_max       29
_diffrn_reflns_limit_l_min       -29
_diffrn_reflns_number            169433
_diffrn_reflns_theta_full        33.14
_diffrn_reflns_theta_max         33.14
_diffrn_reflns_theta_min         2.18
_diffrn_source                   'fine-focus sealed tube'
_exptl_absorpt_coefficient_mu    0.523
_exptl_absorpt_correction_T_max  0.7471
_exptl_absorpt_correction_T_min  0.6834
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2014/3 (Bruker,2014) was used for absorption correction.
wR2(int) was 0.0837 before and 0.0691 after correction.
The Ratio of minimum to maximum transmission is 0.9147.
The \l/2 correction factor is 0.00150.
;
_exptl_crystal_colour            orange
_exptl_crystal_colour_primary    orange
_exptl_crystal_density_diffrn    1.407
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             1608
_refine_diff_density_max         0.664
_refine_diff_density_min         -1.257
_refine_diff_density_rms         0.129
_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     435
_refine_ls_number_reflns         13897
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.990
_refine_ls_R_factor_all          0.0924
_refine_ls_R_factor_gt           0.0486
_refine_ls_shift/su_max          0.001
_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          0.1260
_refine_ls_wR_factor_ref         0.1523
_reflns_number_gt                9886
_reflns_number_total             13897
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja5100405_si_001.cif
_cod_data_source_block           2b
_cod_depositor_comments
'Adding full bibliography for 4123386--4123389.cif.'
_cod_database_code               4123387
_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
2.a Ternary CH refined with riding coordinates:
 C19(H19), C25(H25), C22(H22), C28(H28)
2.b Aromatic/amide H refined with riding coordinates:
 C2(H2), C9(H9), C3(H3), C5(H5), C17(H17), C16(H16), C8(H8), C14(H14), C4(H4),
 C15(H15)
2.c Idealised Me refined as rotating group:
 C23(H23A,H23B,H23C), C21(H21A,H21B,H21C), C24(H24A,H24B,H24C), C35(H35A,H35B,
 H35C), C29(H29A,H29B,H29C), C34(H34A,H34B,H34C), C27(H27A,H27B,H27C), C20(H20A,
 H20B,H20C), C26(H26A,H26B,H26C), C30(H30A,H30B,H30C), C37(H37A,H37B,H37C)
;
_olex2_submission_special_instructions 'No special instructions were received'