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_4126047
_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 H38 Mo N2 O P2'
_chemical_formula_sum            'C36 H38 Mo N2 O P2'
_chemical_formula_weight         672.56
_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
_atom_sites_solution_primary     iterative
_audit_creation_date             2014-04-22
_audit_creation_method
;
Olex2 1.2
(compiled 2014.03.20 svn.r2914 for OlexSys, GUI svn.r4816)
;
_cell_angle_alpha                92.4907(18)
_cell_angle_beta                 90.7171(16)
_cell_angle_gamma                114.4376(14)
_cell_formula_units_Z            2
_cell_length_a                   9.1514(3)
_cell_length_b                   10.2736(3)
_cell_length_c                   18.5352(6)
_cell_measurement_reflns_used    9896
_cell_measurement_temperature    100
_cell_volume                     1584.13(9)
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2008)'
_computing_structure_solution    'olex2.solve (Bourhis et al., 2013)'
_diffrn_ambient_temperature      100
_diffrn_measured_fraction_theta_full 0.983
_diffrn_measured_fraction_theta_max 0.963
_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  0.0621
_diffrn_reflns_av_unetI/netI     0.0730
_diffrn_reflns_Laue_measured_fraction_full 0.983
_diffrn_reflns_Laue_measured_fraction_max 0.963
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       26
_diffrn_reflns_limit_l_min       -25
_diffrn_reflns_number            33477
_diffrn_reflns_point_group_measured_fraction_full 0.983
_diffrn_reflns_point_group_measured_fraction_max 0.963
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         30.643
_diffrn_reflns_theta_min         1.100
_exptl_absorpt_coefficient_mu    0.547
_exptl_absorpt_correction_T_max  0.8212
_exptl_absorpt_correction_T_min  0.0015
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2012/1 (Bruker,2012) was used for absorption correction.
wR2(int) was 0.0463 before and 0.0292 after correction.
The Ratio of minimum to maximum transmission is 0.8212.
The \l/2 correction factor is 0.0015.
;
_exptl_crystal_colour            'clear light yellow'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   light
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    1.410
_exptl_crystal_description       plate
_exptl_crystal_F_000             696
_exptl_crystal_size_max          0.266
_exptl_crystal_size_mid          0.18
_exptl_crystal_size_min          0.064
_refine_diff_density_max         0.766
_refine_diff_density_min         -1.076
_refine_diff_density_rms         0.094
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.966
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     383
_refine_ls_number_reflns         9423
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.966
_refine_ls_R_factor_all          0.0515
_refine_ls_R_factor_gt           0.0353
_refine_ls_shift/su_max          0.003
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
;
 w=1/[\s^2^(Fo^2^)+(0.0284P)^2^]
 where P=(Fo^2^+2Fc^2^)/3
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0666
_refine_ls_wR_factor_ref         0.0699
_reflns_Friedel_coverage         0.000
_reflns_number_gt                7376
_reflns_number_total             9423
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ja7b03053_si_002.cif
_cod_data_source_block           PhBnMoH
_cod_depositor_comments
'Adding full bibliography for 4126047--4126059.cif.'
_cod_database_code               4126047
_shelxl_version_number           2013-2
_shelx_estimated_absorpt_t_max   0.966
_shelx_estimated_absorpt_t_min   0.868
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
2.a Secondary CH2 refined with riding coordinates:
 C4(H3,H2), C2(H6,H7), C5(H5,H4), C18(H18,H17), C25(H10,H11), C3(H9,H8)
2.b Aromatic/amide H refined with riding coordinates:
 C30(H15), C27(H12), C17(H29), C32(H35), C16(H30), C31(H16), C10(H25),
 C34(H37), C33(H36), C8(H27), C35(H38), C13(H33), C22(H20), C14(H32), C23(H22),
 C19(H23), C7(H28), C21(H19), C11(H24), C29(H14), C9(H26), C15(H31), C24(H21),
 C28(H13), C36(H34)
;
_shelx_res_checksum              82800
_shelx_hkl_checksum              86522