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_4347549
_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         'C35 H44 Mo N2 O3 P2, 2(C F3 O3 S)'
_chemical_formula_sum            'C37 H44 F6 Mo N2 O9 P2 S2'
_chemical_formula_weight         996.74
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2yn'
_space_group_name_H-M_alt        'P 1 21/n 1'
_atom_sites_solution_hydrogens   geom
_audit_creation_date             2016-01-04
_audit_creation_method
;
Olex2 1.2
(compiled 2015.09.30 svn.r3233 for OlexSys, GUI svn.r5103)
;
_cell_angle_alpha                90
_cell_angle_beta                 94.1710(10)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   11.3464(4)
_cell_length_b                   21.2519(8)
_cell_length_c                   17.4117(7)
_cell_measurement_reflns_used    9894
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      39.31
_cell_measurement_theta_min      2.25
_cell_volume                     4187.4(3)
_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  'ShelXL (Sheldrick, 2015)'
_diffrn_ambient_temperature      99.97
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.993
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0431
_diffrn_reflns_av_unetI/netI     0.0318
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.993
_diffrn_reflns_limit_h_max       22
_diffrn_reflns_limit_h_min       -21
_diffrn_reflns_limit_k_max       41
_diffrn_reflns_limit_k_min       -41
_diffrn_reflns_limit_l_max       33
_diffrn_reflns_limit_l_min       -33
_diffrn_reflns_number            213710
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.993
_diffrn_reflns_theta_full        26.000
_diffrn_reflns_theta_max         43.711
_diffrn_reflns_theta_min         2.629
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.571
_exptl_absorpt_correction_T_max  0.7486
_exptl_absorpt_correction_T_min  0.6809
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
'SADABS-2014/5 (Bruker,2014/5) was used for absorption correction. wR2(int) was 0.0665 before and 0.0493 after correction. The Ratio of minimum to maximum transmission is 0.9096. The \l/2 correction factor is 0.00150.'
_exptl_crystal_colour            orange
_exptl_crystal_colour_primary    orange
_exptl_crystal_density_diffrn    1.581
_exptl_crystal_description       plate
_exptl_crystal_F_000             2040
_exptl_crystal_size_max          0.21
_exptl_crystal_size_mid          0.21
_exptl_crystal_size_min          0.08
_refine_diff_density_max         1.218
_refine_diff_density_min         -1.091
_refine_diff_density_rms         0.099
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.592
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     542
_refine_ls_number_reflns         32006
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.592
_refine_ls_R_factor_all          0.0495
_refine_ls_R_factor_gt           0.0317
_refine_ls_shift/su_max          0.005
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.1213P)^2^+9.9161P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0958
_refine_ls_wR_factor_ref         0.1212
_reflns_Friedel_coverage         0.000
_reflns_number_gt                25553
_reflns_number_total             32006
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ic6b00331_si_001.cif
_cod_data_source_block           5b
_cod_database_code               4347549
_shelx_estimated_absorpt_t_max   0.956
_shelx_estimated_absorpt_t_min   0.889
_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:
 C00N(H00N), C00W(H00W), C012(H012), C019(H019), C01B(H01H), C01F(H01P)
2.b Aromatic/amide H refined with riding coordinates:
 C00V(H00V), C00X(H00X), C016(H016), C018(H018), C01A(H01G), C01D(H01L),
 C01G(H01Q), C01H(H01R)
2.c Idealised Me refined as rotating group:
 C00S(H00A,H00B,H00C), C00Z(H00D,H00E,H00F), C014(H01A,H01B,H01C), C015(H01D,
 H01E,H01F), C01C(H01I,H01J,H01K), C01E(H01M,H01N,H01O), C01K(H01S,H01T,H01U),
 C01L(H01V,H01W,H01X), C01M(H01Y,H,HA), C01N(H01Z,HB,HC)
;
_shelx_res_checksum              71491
_shelx_hkl_checksum              98192
_shelx_shelxl_version_number     2014/7
_olex2_submission_special_instructions 'No special instructions were received'