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_4129259
_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         'C30 H40 Mo N2 P2'
_chemical_formula_sum            'C30 H40 Mo N2 P2'
_chemical_formula_weight         586.52
_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
;
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_cell_angle_gamma                90
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_cell_length_b                   23.8655(7)
_cell_length_c                   12.7797(4)
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_cell_measurement_theta_min      2.34
_cell_volume                     2732.38(15)
_computing_cell_refinement       'SAINT v6.45A (Bruker, 2003)'
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_computing_data_reduction        'SAINT v6.45A (Bruker, 2003)'
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_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'XL (Sheldrick, 2008)'
_diffrn_ambient_temperature      100
_diffrn_detector_area_resol_mean 8.16
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.984
_diffrn_measurement_device_type  'Bruker SMART v5.054 (Bruker-AXS, 2007)'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0619
_diffrn_reflns_av_unetI/netI     0.0615
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.984
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       47
_diffrn_reflns_limit_k_min       -47
_diffrn_reflns_limit_l_max       25
_diffrn_reflns_limit_l_min       -25
_diffrn_reflns_number            105013
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.984
_diffrn_reflns_theta_full        25.000
_diffrn_reflns_theta_max         45.535
_diffrn_reflns_theta_min         1.707
_diffrn_source_current           30.0
_diffrn_source_power             1.5
_diffrn_source_voltage           50.0
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_exptl_absorpt_correction_T_max  0.7490
_exptl_absorpt_correction_T_min  0.6757
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_exptl_absorpt_process_details
'SADABS-2014/2 (Bruker,2014) was used for absorption correction. wR2(int) was 0.0692 before and 0.0564 after correction. The Ratio of minimum to maximum transmission is 0.9021. The \l/2 correction factor is 0.00150.'
_exptl_crystal_colour            Red
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_exptl_crystal_F_000             1224
_refine_diff_density_max         2.749
_refine_diff_density_min         -0.886
_refine_diff_density_rms         0.174
_refine_ls_extinction_method     none
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_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     324
_refine_ls_number_reflns         22772
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.101
_refine_ls_R_factor_all          0.0899
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_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0292P)^2^+3.3369P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0978
_refine_ls_wR_factor_ref         0.1151
_reflns_Friedel_coverage         0.000
_reflns_number_gt                15022
_reflns_number_total             22772
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ja5059923_si_002.cif
_cod_data_source_block           ctc02
_cod_original_cell_volume        2732.37(15)
_cod_database_code               4129259
_shelxl_version_number           2014-2
_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:
 C3(H3), C2(H2), C6(H6), C5(H5), C25(H25), C19(H19), C28(H28), C22(H22)
2.b Aromatic/amide H refined with riding coordinates:
 C18(H18), C9(H9), C15(H15), C12(H12), C16(H16), C17(H17), C10(H10), C11(H11)
2.c Idealised Me refined as rotating group:
 C21(H21A,H21B,H21C), C23(H23A,H23B,H23C), C20(H20A,H20B,H20C), C29(H29A,H29B,
 H29C), C24(H24A,H24B,H24C), C26(H26A,H26B,H26C), C27(H27A,H27B,H27C), C30(H30A,
 H30B,H30C)
;
_shelx_res_checksum              1569
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_olex2_submission_special_instructions 'No special instructions were received'