Molybdenum catalyzed ammonia borane dehydrogenation: oxidation state specific mechanisms.
Buss, Joshua A.; Edouard, Guy A.; Cheng, Christine; Shi, Jade; Agapie, Theodor; Journal of the American Chemical Society 136 (2014) 11272–11275; doi:10.1021/ja5059923

data_4129257
_publ_section_title
;
 Molybdenum catalyzed ammonia borane dehydrogenation: oxidation state
 specific mechanisms.
;
_journal_issue                   32
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              11272
_journal_page_last               11275
_journal_paper_doi               10.1021/ja5059923
_journal_volume                  136
_journal_year                    2014
_chemical_formula_moiety         'C32 H40 Mo O2 P2, 2(C F3 O3 S)'
_chemical_formula_sum            'C34 H40 F6 Mo O8 P2 S2'
_chemical_formula_weight         912.66
_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             2014-06-07
_audit_creation_method
;
Olex2 1.2
(compiled 2014.05.21 svn.r2940 for OlexSys, GUI svn.r4846),
 SHELXL-2014,
 and manual edit
;
_cell_angle_alpha                90
_cell_angle_beta                 91.785(2)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   12.7866(6)
_cell_length_b                   16.4447(7)
_cell_length_c                   17.5292(7)
_cell_measurement_reflns_used    9500
_cell_measurement_temperature    100
_cell_measurement_theta_max      42.91
_cell_measurement_theta_min      2.30
_cell_volume                     3684.1(3)
_computing_cell_refinement       'SAINT v8.34A (Bruker, 2013)'
_computing_data_collection       'APEX2_2011.2-3 (Bruker-AXS, 2007)'
_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    'XT-2014/1 (Sheldrick, 2012)'
_diffrn_ambient_temperature      100
_diffrn_detector_area_resol_mean 8.33
_diffrn_measured_fraction_theta_full 0.996
_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_unetI/netI     0.0368
_diffrn_reflns_Laue_measured_fraction_full 0.996
_diffrn_reflns_Laue_measured_fraction_max 0.992
_diffrn_reflns_limit_h_max       25
_diffrn_reflns_limit_h_min       -25
_diffrn_reflns_limit_k_max       32
_diffrn_reflns_limit_k_min       -32
_diffrn_reflns_limit_l_max       35
_diffrn_reflns_limit_l_min       -24
_diffrn_reflns_number            30803
_diffrn_reflns_point_group_measured_fraction_full 0.996
_diffrn_reflns_point_group_measured_fraction_max 0.992
_diffrn_reflns_theta_full        25.000
_diffrn_reflns_theta_max         45.424
_diffrn_reflns_theta_min         1.698
_diffrn_source_current           30.0
_diffrn_source_power             1.5
_diffrn_source_voltage           50.0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.637
_exptl_absorpt_correction_T_max  0.7489
_exptl_absorpt_correction_T_min  0.6643
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
'SADABS-2014/2 (Bruker,2014) was used for absorption correction. wR2(int) was 0.0577 before and 0.0530 after correction. The Ratio of minimum to maximum transmission is 0.8870. The \l/2 correction factor is 0.00150.'
_exptl_crystal_colour            yellow
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    1.645
_exptl_crystal_description       rhomboidal
_exptl_crystal_F_000             1864
_exptl_crystal_size_max          0.41
_exptl_crystal_size_mid          0.17
_exptl_crystal_size_min          0.13
_refine_diff_density_max         4.057
_refine_diff_density_min         -2.495
_refine_diff_density_rms         0.161
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.130
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     487
_refine_ls_number_reflns         30803
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.130
_refine_ls_R_factor_all          0.0619
_refine_ls_R_factor_gt           0.0464
_refine_ls_shift/su_max          0.004
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0442P)^2^+5.9227P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1251
_refine_ls_wR_factor_ref         0.1329
_reflns_Friedel_coverage         0.000
_reflns_number_gt                25176
_reflns_number_total             30803
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ja5059923_si_002.cif
_cod_data_source_block           gae07
_cod_database_code               4129257
_shelxl_version_number           2014-2
_shelx_estimated_absorpt_t_max   0.922
_shelx_estimated_absorpt_t_min   0.780
_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:
 C25(H25), C28(H28), C19(H19), C22(H22)
2.b Aromatic/amide H refined with riding coordinates:
 C18(H18), C17(H17), C16(H16), C15(H15), C5(H5), C6(H6), C12(H12), C11(H11),
 C10(H10), C9(H9), C2(H2), C3(H3)
2.c Idealised Me refined as rotating group:
 C26(H26A,H26B,H26C), C27(H27A,H27B,H27C), C29(H29A,H29B,H29C), C30(H30A,H30B,
 H30C), C21(H21A,H21B,H21C), C20(H20A,H20B,H20C), C24(H24A,H24B,H24C), C23(H23A,
 H23B,H23C)
;
_olex2_submission_original_sample_id gae07
_olex2_submission_special_instructions 'No special instructions were received'