Reversible Heterolytic Cleavage of the H-H Bond by Molybdenum Complexes: Controlling the Dynamics of Exchange Between Proton and Hydride.
Zhang, Shaoguang; Appel, Aaron M.; Bullock, R. Morris; Journal of the American Chemical Society 139 (2017) 7376–7387; doi:10.1021/jacs.7b03053

data_4126056
_publ_section_title
;
 Reversible Heterolytic Cleavage of the H-H Bond by Molybdenum Complexes:
 Controlling the Dynamics of Exchange Between Proton and Hydride.
;
_journal_issue                   21
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              7376
_journal_page_last               7387
_journal_paper_doi               10.1021/jacs.7b03053
_journal_volume                  139
_journal_year                    2017
_chemical_formula_moiety         'C36 H39 Mo N2 O P2, C32 H12 B F24'
_chemical_formula_sum            'C68 H51 B F24 Mo N2 O P2'
_chemical_formula_weight         1536.79
_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   mixed
_audit_creation_date             2014-11-18
_audit_creation_method
;
Olex2 1.2
(compiled 2014.07.22 svn.r2960 for OlexSys, GUI svn.r4862)
;
_cell_angle_alpha                89.961(4)
_cell_angle_beta                 72.330(3)
_cell_angle_gamma                74.987(4)
_cell_formula_units_Z            2
_cell_length_a                   11.3495(8)
_cell_length_b                   16.8735(13)
_cell_length_c                   18.6417(14)
_cell_measurement_reflns_used    9990
_cell_measurement_temperature    150
_cell_volume                     3273.7(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  'ShelXL (Sheldrick, 2008)'
_diffrn_ambient_temperature      150
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.994
_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  0.0471
_diffrn_reflns_av_unetI/netI     0.0645
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.994
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       22
_diffrn_reflns_limit_k_min       -22
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_limit_l_min       -24
_diffrn_reflns_number            57392
_diffrn_reflns_point_group_measured_fraction_full 0.997
_diffrn_reflns_point_group_measured_fraction_max 0.994
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.964
_diffrn_reflns_theta_min         1.151
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.363
_exptl_absorpt_correction_T_max  0.7456
_exptl_absorpt_correction_T_min  0.6655
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2012/1 (Bruker,2012) was used for absorption correction.
wR2(int) was 0.0535 before and 0.0465 after correction.
The Ratio of minimum to maximum transmission is 0.8926.
The \l/2 correction factor is 0.0015.
;
_exptl_crystal_colour            'clear light orange'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   light
_exptl_crystal_colour_primary    orange
_exptl_crystal_density_diffrn    1.559
_exptl_crystal_description       needle
_exptl_crystal_F_000             1548
_exptl_crystal_size_max          0.284
_exptl_crystal_size_mid          0.073
_exptl_crystal_size_min          0.064
_refine_diff_density_max         1.618
_refine_diff_density_min         -0.908
_refine_diff_density_rms         0.100
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.034
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     938
_refine_ls_number_reflns         15663
_refine_ls_number_restraints     2
_refine_ls_restrained_S_all      1.035
_refine_ls_R_factor_all          0.0978
_refine_ls_R_factor_gt           0.0629
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0825P)^2^+5.1778P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1536
_refine_ls_wR_factor_ref         0.1709
_reflns_Friedel_coverage         0.000
_reflns_number_gt                11074
_reflns_number_total             15663
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ja7b03053_si_002.cif
_cod_data_source_block           PhBnMoHNH+
_cod_depositor_comments
'Adding full bibliography for 4126047--4126059.cif.'
_cod_database_code               4126056
_shelxl_version_number           2013-4
_shelx_estimated_absorpt_t_max   0.977
_shelx_estimated_absorpt_t_min   0.904
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
2. Restrained distances
 Mo1-H1
 1.474 with sigma of 0.02
 C1-H1
 2.022 with sigma of 0.04
3. Uiso/Uaniso restraints and constraints
Uanis(F4) = Uanis(F4A)
Uanis(F5) = Uanis(F5A)
Uanis(F6) = Uanis(F6A)
4. Others
 Sof(F4A)=Sof(F5A)=Sof(F6A)=1-FVAR(1)
 Sof(F4)=Sof(F5)=Sof(F6)=FVAR(1)
 Sof(F1)=Sof(F3)=Sof(F2)=1-FVAR(2)
 Sof(F1A)=Sof(F3A)=Sof(F2A)=FVAR(2)
5.a Secondary CH2 refined with riding coordinates:
 C6(H6A,H6B), C3(H3A,H3B), C19(H19A,H19B), C2(H2A,H2B), C5(H5A,H5B), C4(H4A,H4B)
5.b Aromatic/amide H refined with riding coordinates:
 C21(H21), C22(H22), C23(H23), C24(H24), C25(H25), C12(H12), C11(H11),
 C10(H10), C9(H9), C8(H8), C27(H27), C28(H28), C29(H29), C30(H30), C31(H31),
 C18(H18), C17(H17), C16(H16), C15(H15), C14(H14), C32(H32), C36(H36), C35(H35),
  C34(H34), C33(H33), C48(H48), C50(H50), C42(H42), C38(H38), C40(H40),
 C54(H54), C56(H56), C58(H58), C62(H62), C64(H64), C66(H66), C46(H46)
;
_shelx_res_checksum              76402
_shelx_hkl_checksum              31789
_olex2_submission_special_instructions 'No special instructions were received'