Modulation of Proton-Coupled Electron Transfer through Molybdenum-Quinonoid Interactions.
Henthorn, Justin T.; Agapie, Theodor; Inorganic chemistry 55 (2016) 5337–5342; doi:10.1021/acs.inorgchem.6b00331

data_4347550
_publ_section_title
;
 Modulation of Proton-Coupled Electron Transfer through
 Molybdenum-Quinonoid Interactions.
;
_journal_issue                   11
_journal_name_full               'Inorganic chemistry'
_journal_page_first              5337
_journal_page_last               5342
_journal_paper_doi               10.1021/acs.inorgchem.6b00331
_journal_volume                  55
_journal_year                    2016
_chemical_formula_moiety         'C31 H38 Cl2 Mo O3 P2'
_chemical_formula_sum            'C31 H38 Cl2 Mo O3 P2'
_chemical_formula_weight         687.39
_space_group_crystal_system      orthorhombic
_space_group_IT_number           61
_space_group_name_Hall           '-P 2ac 2ab'
_space_group_name_H-M_alt        'P b c a'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_date             2014-09-23
_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                 90.00
_cell_angle_gamma                90.00
_cell_formula_units_Z            8
_cell_length_a                   16.255
_cell_length_b                   16.2548(10)
_cell_length_c                   22.2047(15)
_cell_measurement_reflns_used    9676
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      43.224
_cell_measurement_theta_min      2.506
_cell_volume                     5867.0(5)
_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      100.02
_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  0.0838
_diffrn_reflns_av_unetI/netI     0.0606
_diffrn_reflns_limit_h_max       32
_diffrn_reflns_limit_h_min       -31
_diffrn_reflns_limit_k_max       32
_diffrn_reflns_limit_k_min       -28
_diffrn_reflns_limit_l_max       44
_diffrn_reflns_limit_l_min       -44
_diffrn_reflns_number            225462
_diffrn_reflns_theta_full        45.29
_diffrn_reflns_theta_max         45.29
_diffrn_reflns_theta_min         1.83
_diffrn_source                   'fine-focus sealed tube'
_exptl_absorpt_coefficient_mu    0.771
_exptl_absorpt_correction_T_max  0.7494
_exptl_absorpt_correction_T_min  0.6766
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2014/3 (Bruker,2014) was used for absorption correction.
wR2(int) was 0.1528 before and 0.0848 after correction.
The Ratio of minimum to maximum transmission is 0.9029.
The \l/2 correction factor is 0.00150.
;
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    1.556
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             2832
_refine_diff_density_max         1.703
_refine_diff_density_min         -1.067
_refine_diff_density_rms         0.118
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.954
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     360
_refine_ls_number_reflns         24530
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.954
_refine_ls_R_factor_all          0.0634
_refine_ls_R_factor_gt           0.0338
_refine_ls_shift/su_max          0.005
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0399P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0805
_refine_ls_wR_factor_ref         0.0868
_reflns_number_gt                16461
_reflns_number_total             24530
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic6b00331_si_001.cif
_cod_data_source_block           6
_cod_original_cell_volume        5866.9(5)
_cod_database_code               4347550
_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:
 C9(H9), C8(H8), C19(H19), C22(H22), C25(H25), C28(H28)
2.b Aromatic/amide H refined with riding coordinates:
 C5(H5), C4(H4), C14(H14), C3(H3), C16(H16), C17(H17), C15(H15), C2(H2)
2.c Idealised Me refined as rotating group:
 C24(H24A,H24B,H24C), C23(H23A,H23B,H23C), C30(H30A,H30B,H30C), C26(H26A,H26B,
 H26C), C27(H27A,H27B,H27C), C20(H20A,H20B,H20C), C21(H21A,H21B,H21C), C29(H29A,
 H29B,H29C)
;
_olex2_submission_special_instructions 'No special instructions were received'