Molybdenum Hydride and Dihydride Complexes Bearing Diphosphine Ligands with a Pendant Amine: Formation of Complexes with Bound Amines.
Zhang, Shaoguang; Bullock, R. Morris; Inorganic chemistry 54 (2015) 6397–6409; doi:10.1021/acs.inorgchem.5b00728

data_4343269
_publ_section_title
;
 Molybdenum Hydride and Dihydride Complexes Bearing Diphosphine Ligands
 with a Pendant Amine: Formation of Complexes with Bound Amines.
;
_journal_issue                   13
_journal_name_full               'Inorganic chemistry'
_journal_page_first              6397
_journal_page_last               6409
_journal_paper_doi               10.1021/acs.inorgchem.5b00728
_journal_volume                  54
_journal_year                    2015
_chemical_formula_moiety         'C33 H33 Mo N O P2'
_chemical_formula_sum            'C33 H33 Mo N O P2'
_chemical_formula_weight         617.48
_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   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_date             2015-02-24
_audit_creation_method
;
Olex2 1.2
(compiled 2014.07.22 svn.r2960 for OlexSys, GUI svn.r4862)
;
_cell_angle_alpha                67.165(6)
_cell_angle_beta                 80.541(6)
_cell_angle_gamma                70.222(6)
_cell_formula_units_Z            2
_cell_length_a                   9.5859(13)
_cell_length_b                   12.2921(18)
_cell_length_c                   13.7379(19)
_cell_measurement_reflns_used    9926
_cell_measurement_temperature    100
_cell_volume                     1402.9(3)
_computing_cell_refinement       'SAINT v7.68A (Bruker, 2009)'
_computing_data_collection       'APEX II, Bruker'
_computing_data_reduction        'SAINT v7.68A (Bruker, 2009)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      100.15
_diffrn_measured_fraction_theta_full 0.994
_diffrn_measured_fraction_theta_max 0.994
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_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  0.0453
_diffrn_reflns_av_unetI/netI     0.0391
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            23190
_diffrn_reflns_theta_full        27.53
_diffrn_reflns_theta_max         27.53
_diffrn_reflns_theta_min         1.61
_diffrn_source                   'fine-focus sealed tube'
_exptl_absorpt_coefficient_mu    0.609
_exptl_absorpt_correction_T_max  0.7456
_exptl_absorpt_correction_T_min  0.6892
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
'SADABS-2008/1 (Bruker,2008) was used for absorption correction. wR2(int) was 0.0621 before and 0.0582 after correction. The Ratio of minimum to maximum transmission is 0.9244. The \l/2 correction factor is 0.0015.'
_exptl_crystal_colour            'light yellow'
_exptl_crystal_density_diffrn    1.462
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             636
_exptl_crystal_size_max          0.2
_exptl_crystal_size_mid          0.2
_exptl_crystal_size_min          0.1
_refine_diff_density_max         0.446
_refine_diff_density_min         -0.341
_refine_diff_density_rms         0.068
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.980
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     348
_refine_ls_number_reflns         6416
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.980
_refine_ls_R_factor_all          0.0278
_refine_ls_R_factor_gt           0.0251
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0224P)^2^+1.1228P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0630
_refine_ls_wR_factor_ref         0.0647
_reflns_number_gt                5936
_reflns_number_total             6416
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic5b00728_si_002.cif
_cod_data_source_block           miller021_0m
_cod_depositor_comments
'Adding full bibliography for 4343268--4343274.cif.'
_cod_database_code               4343269
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2.a Secondary CH2 refined with riding coordinates:
 C7(H2A,H2B), C9(H3A,H3B)
2.b Aromatic/amide H refined with riding coordinates:
 C2(H10), C3(H11), C4(H12), C5(H13), C6(H14), C11(H20), C12(H21), C13(H22),
 C14(H23), C15(H24), C17(H19), C18(H18), C19(H17), C20(H16), C21(H15), C23(H5),
 C24(H6), C25(H7), C26(H8), C27(H9), C28(H25), C29(H26), C30(H27), C31(H28),
 C32(H29)
2.c Idealised Me refined as rotating group:
 C8(H4A,H4B,H4C)
;
_olex2_submission_special_instructions 'No special instructions were received'