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_4129260
_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 H44 Mo N P2, C24 H20 B'
_chemical_formula_sum            'C56 H64 B Mo N P2'
_chemical_formula_weight         919.77
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2ybc'
_space_group_name_H-M_alt        'P 1 21/c 1'
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     direct
_audit_creation_date             2014-06-07
_audit_creation_method
;
Olex2 1.2
(compiled 2014.05.21 svn.r2940 for OlexSys, GUI svn.r4846)
;
_cell_angle_alpha                90
_cell_angle_beta                 101.250(2)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   12.7883(6)
_cell_length_b                   16.1757(7)
_cell_length_c                   23.2443(10)
_cell_measurement_reflns_used    9039
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      38.86
_cell_measurement_theta_min      2.36
_cell_volume                     4715.9(4)
_computing_cell_refinement       'SAINT v8.34A (Bruker, 2013)'
_computing_data_collection       'APEX2 2013.2-0 (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 (Sheldrick, 2008)'
_diffrn_ambient_temperature      99.99
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.931
_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  0.0456
_diffrn_reflns_av_unetI/netI     0.0319
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.931
_diffrn_reflns_limit_h_max       21
_diffrn_reflns_limit_h_min       -21
_diffrn_reflns_limit_k_max       27
_diffrn_reflns_limit_k_min       -27
_diffrn_reflns_limit_l_max       39
_diffrn_reflns_limit_l_min       -41
_diffrn_reflns_number            296142
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.931
_diffrn_reflns_theta_full        25.000
_diffrn_reflns_theta_max         39.298
_diffrn_reflns_theta_min         1.544
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.384
_exptl_absorpt_correction_T_max  1.0000
_exptl_absorpt_correction_T_min  0.8658
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2012/1 (Bruker,2012) was used for absorption correction.
wR2(int) was 0.0677 before and 0.0536 after correction.
The Ratio of minimum to maximum transmission is 0.8658.
The \l/2 correction factor is 0.0015.
;
_exptl_crystal_colour            red
_exptl_crystal_colour_primary    red
_exptl_crystal_density_diffrn    1.295
_exptl_crystal_description       blockish
_exptl_crystal_F_000             1936
_exptl_crystal_size_max          0.95
_exptl_crystal_size_mid          0.72
_exptl_crystal_size_min          0.7
_refine_diff_density_max         2.897
_refine_diff_density_min         -2.086
_refine_diff_density_rms         0.122
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.120
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     622
_refine_ls_number_reflns         26004
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.120
_refine_ls_R_factor_all          0.1259
_refine_ls_R_factor_gt           0.0731
_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^)+(0.0296P)^2^+13.6982P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1418
_refine_ls_wR_factor_ref         0.1777
_reflns_Friedel_coverage         0.000
_reflns_number_gt                17430
_reflns_number_total             26004
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ja5059923_si_002.cif
_cod_data_source_block           a14006
_cod_database_code               4129260
_shelxl_version_number           2013-3
_shelx_estimated_absorpt_t_max   0.775
_shelx_estimated_absorpt_t_min   0.712
_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. Others
 Sof(C28B)=Sof(H28B)=Sof(C30B)=Sof(H30D)=Sof(H30E)=Sof(H30F)=Sof(C29B)=
 Sof(H29D)=Sof(H29E)=Sof(H29F)=Sof(C22B)=Sof(H22B)=Sof(C23B)=Sof(H23D)=
 Sof(H23E)=Sof(H23F)=Sof(C24B)=Sof(H24D)=Sof(H24E)=Sof(H24F)=1-FVAR(1)
 Sof(C28A)=Sof(H28A)=Sof(C30A)=Sof(H30A)=Sof(H30B)=Sof(H30C)=Sof(C29A)=
 Sof(H29A)=Sof(H29B)=Sof(H29C)=Sof(C22A)=Sof(H22A)=Sof(C23A)=Sof(H23A)=
 Sof(H23B)=Sof(H23C)=Sof(C24A)=Sof(H24A)=Sof(H24B)=Sof(H24C)=FVAR(1)
3.a Ternary CH refined with riding coordinates:
 C25(H25), C19(H19), C28A(H28A), C22A(H22A), C28B(H28B), C22B(H22B)
3.b Aromatic/amide H refined with riding coordinates:
 C5(H5), C6(H6), C2(H2), C3(H3), C15(H15), C16(H16), C17(H17), C18(H18),
 C9(H9), C10(H10), C11(H11), C12(H12), C34(H34), C35(H35), C36(H36), C37(H37),
 C38(H38), C40(H40), C41(H41), C42(H42), C43(H43), C44(H44), C46(H46), C47(H47),
  C48(H48), C49(H49), C50(H50), C52(H52), C53(H53), C54(H54), C55(H55), C56(H56)
3.c Idealised Me refined as rotating group:
 C26(H26A,H26B,H26C), C27(H27A,H27B,H27C), C21(H21A,H21B,H21C), C20(H20A,H20B,
 H20C), C32(H32A,H32B,H32C), C30A(H30A,H30B,H30C), C29A(H29A,H29B,H29C),
 C23A(H23A,H23B,H23C), C24A(H24A,H24B,H24C), C30B(H30D,H30E,H30F), C29B(H29D,
 H29E,H29F), C23B(H23D,H23E,H23F), C24B(H24D,H24E,H24F)
;
_shelx_res_checksum              18600
_shelx_hkl_checksum              51793
_olex2_submission_special_instructions 'No special instructions were received'