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_4126058
_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         'C32 H47 Mo N2 O P2, C32 H12 B F24'
_chemical_formula_sum            'C64 H59 B F24 Mo N2 O P2'
_chemical_formula_weight         1496.82
_chemical_name_systematic
;
 ?
;
_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'
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 1'
_atom_sites_solution_hydrogens   mixed
_audit_creation_date             2015-10-01
_audit_creation_method
;
Olex2 1.2
(compiled 2015.01.26 svn.r3150 for OlexSys, GUI svn.r4998)
;
_cell_angle_alpha                90
_cell_angle_beta                 96.564(4)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   10.1440(7)
_cell_length_b                   23.5478(17)
_cell_length_c                   27.0590(19)
_cell_measurement_reflns_used    9817
_cell_measurement_temperature    100
_cell_measurement_theta_max      27.43
_cell_measurement_theta_min      2.20
_cell_volume                     6421.2(8)
_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      100
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.992
_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  0.0583
_diffrn_reflns_av_unetI/netI     0.0575
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.992
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       31
_diffrn_reflns_limit_k_min       -31
_diffrn_reflns_limit_l_max       36
_diffrn_reflns_limit_l_min       -36
_diffrn_reflns_number            111680
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.992
_diffrn_reflns_theta_full        26.000
_diffrn_reflns_theta_max         28.432
_diffrn_reflns_theta_min         1.730
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.368
_exptl_absorpt_correction_T_max  0.7457
_exptl_absorpt_correction_T_min  0.6649
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2012/1 (Bruker,2012) was used for absorption correction.
wR2(int) was 0.0639 before and 0.0528 after correction.
The Ratio of minimum to maximum transmission is 0.8916.
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    1.548
_exptl_crystal_description       plate
_exptl_crystal_F_000             3032
_exptl_crystal_size_max          0.231
_exptl_crystal_size_mid          0.178
_exptl_crystal_size_min          0.108
_refine_diff_density_max         1.809
_refine_diff_density_min         -1.181
_refine_diff_density_rms         0.102
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.022
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     864
_refine_ls_number_reflns         16055
_refine_ls_number_restraints     2
_refine_ls_restrained_S_all      1.023
_refine_ls_R_factor_all          0.0932
_refine_ls_R_factor_gt           0.0600
_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^)+(0.0675P)^2^+15.2820P]
 where P=(Fo^2^+2Fc^2^)/3
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1398
_refine_ls_wR_factor_ref         0.1555
_reflns_Friedel_coverage         0.000
_reflns_number_gt                11455
_reflns_number_total             16055
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ja7b03053_si_002.cif
_cod_data_source_block           tBuBnMoHNH+
_cod_depositor_comments
'Adding full bibliography for 4126047--4126059.cif.'
_cod_database_code               4126058
_shelxl_version_number           2013-2
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups, All N(H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Restrained distances
 Mo1-H1
 1.61 with sigma of 0.02
 C1-H1
 2.347 with sigma of 0.02
3. Uiso/Uaniso restraints and constraints
Uanis(F10) = Uanis(F10A)
Uanis(F11) = Uanis(F11A)
Uanis(F12) = Uanis(F12A)
Uanis(F10) = Uanis(F11A)
Uanis(F11) = Uanis(F12A)
Uanis(F12) = Uanis(F10A)
4. Others
 Sof(F10A)=Sof(F12A)=Sof(F11A)=1-FVAR(1)
 Sof(F11)=Sof(F10)=Sof(F12)=FVAR(1)
5.a Ternary CH refined with riding coordinates:
 N1(H2)
5.b Secondary CH2 refined with riding coordinates:
 C2(H2A,H2B), C3(H3A,H3B), C4(H4A,H4B), C19(H19A,H19B), C6(H6A,H6B), C5(H5A,H5B)
5.c Aromatic/amide H refined with riding coordinates:
 C62(H62), C42(H42), C37(H37), C17(H17), C46(H46), C56(H56), C50(H50),
 C39(H39), C12(H12), C59(H59), C18(H18), C34(H34), C44(H44), C16(H16), C64(H64),
  C8(H8), C14(H14), C53(H53), C32(H32), C15(H15), C30(H30), C9(H9), C11(H11),
 C31(H31), C28(H28), C29(H29), C10(H10)
5.d Idealised Me refined as rotating group:
 C25(H25A,H25B,H25C), C27(H27A,H27B,H27C), C26(H26A,H26B,H26C), C21(H21A,H21B,
 H21C), C23(H23A,H23B,H23C), C22(H22A,H22B,H22C)
;
_shelx_res_checksum              5682
_shelx_hkl_checksum              90113
_olex2_submission_special_instructions 'No special instructions were received'