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_4129258
_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
'C34 H46 Mo N2 P2, 2(C F3 O3 S), 0.33(C2 H3 N)'
_chemical_formula_sum            'C36.67 H46 F6 Mo N2.33 O6 P2 S2'
_chemical_formula_weight         951.42
_space_group_crystal_system      trigonal
_space_group_IT_number           161
_space_group_name_Hall           'R 3 -2"c'
_space_group_name_H-M_alt        'R 3 c :H'
_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                 90
_cell_angle_gamma                120
_cell_formula_units_Z            18
_cell_length_a                   32.0444(10)
_cell_length_b                   32.0444(10)
_cell_length_c                   21.1665(9)
_cell_measurement_reflns_used    9356
_cell_measurement_temperature    100
_cell_measurement_theta_max      38.62
_cell_measurement_theta_min      2.20
_cell_volume                     18822.8(12)
_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 1.000
_diffrn_measured_fraction_theta_max 0.988
_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  0.0406
_diffrn_reflns_av_unetI/netI     0.0295
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.988
_diffrn_reflns_limit_h_max       60
_diffrn_reflns_limit_h_min       -61
_diffrn_reflns_limit_k_max       49
_diffrn_reflns_limit_k_min       -61
_diffrn_reflns_limit_l_max       40
_diffrn_reflns_limit_l_min       -39
_diffrn_reflns_number            328984
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.977
_diffrn_reflns_theta_full        25.000
_diffrn_reflns_theta_max         43.500
_diffrn_reflns_theta_min         2.059
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.563
_exptl_absorpt_correction_T_max  0.7486
_exptl_absorpt_correction_T_min  0.6909
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2014/2 (Bruker,2014) was used for absorption correction.
wR2(int) was 0.0534 before and 0.0513 after correction.
The Ratio of minimum to maximum transmission is 0.9229.
The \l/2 correction factor is 0.00150.
;
_exptl_crystal_colour            green
_exptl_crystal_colour_primary    green
_exptl_crystal_density_diffrn    1.511
_exptl_crystal_description       odd
_exptl_crystal_F_000             8790
_exptl_crystal_size_max          0.372
_exptl_crystal_size_mid          0.305
_exptl_crystal_size_min          0.301
_refine_diff_density_max         1.889
_refine_diff_density_min         -0.903
_refine_diff_density_rms         0.104
_refine_ls_abs_structure_details
;
 Flack x determined using 12369 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   -0.015(3)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.056
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     516
_refine_ls_number_reflns         31107
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.056
_refine_ls_R_factor_all          0.0487
_refine_ls_R_factor_gt           0.0371
_refine_ls_shift/su_max          0.006
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0468P)^2^+18.4494P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0855
_refine_ls_wR_factor_ref         0.0909
_reflns_Friedel_coverage         0.976
_reflns_Friedel_fraction_full    1.000
_reflns_Friedel_fraction_max     0.965
_reflns_number_gt                27294
_reflns_number_total             31107
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ja5059923_si_002.cif
_cod_data_source_block           gae10
_cod_original_cell_volume        18822.7(14)
_cod_original_sg_symbol_H-M      'R 3 c'
_cod_database_code               4129258
_shelxl_version_number           2014-2
_shelx_estimated_absorpt_t_max   0.849
_shelx_estimated_absorpt_t_min   0.818
_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
 Fixed Sof: H1CC(0.33333) H1CA(0.33333) H1CB(0.33333)
3.a Ternary CH refined with riding coordinates:
 C6(H6), C3(H3), C5(H5), C2(H2), C22(H22), C28(H28), C19(H19), C25(H25)
3.b Aromatic/amide H refined with riding coordinates:
 C11(H11), C10(H10), C9(H9), C18(H18), C15(H15), C16(H16), C1A(H1A), C1B(H1B)
3.c Idealised Me refined as rotating group:
 C17(H17A,H17B,H17C), C29(H29A,H29B,H29C), C30(H30A,H30B,H30C), C26(H26A,H26B,
 H26C), C20(H20A,H20B,H20C), C23(H23A,H23B,H23C), C27(H27A,H27B,H27C), C24(H24A,
 H24B,H24C), C37(H37A,H37B,H37C), C38(H38A,H38B,H38C), C1C(H1CC,H1CA,H1CB)
;
_olex2_submission_special_instructions 'No special instructions were received'