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_4343270
_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         'C17 H32 Mo N O P2, C32 H12 B F24'
_chemical_formula_sum            'C49 H44 B F24 Mo N O P2'
_chemical_formula_weight         1287.54
_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
_audit_creation_date             2015-03-17
_audit_creation_method
;
Olex2 1.2
(compiled 2014.07.22 svn.r2960 for OlexSys, GUI svn.r4862)
;
_cell_angle_alpha                66.032(4)
_cell_angle_beta                 70.298(4)
_cell_angle_gamma                86.114(4)
_cell_formula_units_Z            2
_cell_length_a                   12.6750(11)
_cell_length_b                   14.7018(13)
_cell_length_c                   16.5713(14)
_cell_measurement_reflns_used    9918
_cell_measurement_temperature    100
_cell_volume                     2647.9(4)
_computing_cell_refinement       'SAINT v8.34A (Bruker, 2013)'
_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  'ShelXL (Sheldrick, 2008)'
_diffrn_ambient_temperature      100
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.996
_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  0.0308
_diffrn_reflns_av_unetI/netI     0.0327
_diffrn_reflns_laue_measured_fraction_full 1.000
_diffrn_reflns_laue_measured_fraction_max 0.996
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_h_min       -18
_diffrn_reflns_limit_k_max       21
_diffrn_reflns_limit_k_min       -21
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_limit_l_min       -24
_diffrn_reflns_number            67656
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.996
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         32.080
_diffrn_reflns_theta_min         1.521
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.431
_exptl_absorpt_correction_T_max  0.7463
_exptl_absorpt_correction_T_min  0.6682
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2012/1 (Bruker,2012) was used for absorption correction.
wR2(int) was 0.0559 before and 0.0478 after correction.
The Ratio of minimum to maximum transmission is 0.8954.
The \l/2 correction factor is 0.0015.
;
_exptl_crystal_colour            'clear light orange'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   light
_exptl_crystal_colour_primary    orange
_exptl_crystal_density_diffrn    1.615
_exptl_crystal_description       block
_exptl_crystal_F_000             1292
_exptl_crystal_size_max          0.522
_exptl_crystal_size_mid          0.228
_exptl_crystal_size_min          0.211
_refine_diff_density_max         1.319
_refine_diff_density_min         -1.182
_refine_diff_density_rms         0.079
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.064
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     817
_refine_ls_number_reflns         18424
_refine_ls_number_restraints     130
_refine_ls_restrained_S_all      1.131
_refine_ls_R_factor_all          0.0454
_refine_ls_R_factor_gt           0.0384
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0446P)^2^+1.8509P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0956
_refine_ls_wR_factor_ref         0.0993
_reflns_Friedel_coverage         0.000
_reflns_number_gt                16009
_reflns_number_total             18424
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ic5b00728_si_002.cif
_cod_data_source_block           zhang005a
_cod_depositor_comments
'Adding full bibliography for 4343268--4343274.cif.'
_cod_database_code               4343270
_shelxl_version_number           2013-4
_shelx_estimated_absorpt_t_max   0.915
_shelx_estimated_absorpt_t_min   0.806
_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. Restrained distances
 F11-C44 \\sim F11A-C44 \\sim F10-C44 \\sim F10A-C44 \\sim F12-C44 \\sim
F12A-C44
 with sigma of 0.002
 C49-C27 \\sim C49A-C27
 with sigma of 0.02
3. Uiso/Uaniso restraints and constraints
Uanis(F16A) \\sim Ueq: with sigma of 0.1 and sigma for terminal atoms of 0.2
Uanis(C49) = Uanis(C49A)
Uanis(F16) = Uanis(F16A)
4. Rigid body (RIGU) restrains
 C47, F5A, F4A, F6A
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 C47, F5, F4, F6
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 C44, F10, F12, F11
 with sigma for 1-2 distances of 0.002 and sigma for 1-3 distances of 0.002
 C44, F10A, F12A, F11A
 with sigma for 1-2 distances of 0.002 and sigma for 1-3 distances of 0.002
 C41, F16, F18, F17
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 C41, F16A, F18A, F17A
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
5. Others
 Sof(F11A)=Sof(F10A)=Sof(F12A)=1-FVAR(1)
 Sof(F12)=Sof(F10)=Sof(F11)=FVAR(1)
 Sof(F17A)=Sof(F16A)=Sof(F18A)=1-FVAR(2)
 Sof(F18)=Sof(F16)=Sof(F17)=FVAR(2)
 Sof(F6A)=Sof(F4A)=Sof(F5A)=1-FVAR(3)
 Sof(F5)=Sof(F4)=Sof(F6)=FVAR(3)
 Sof(F22A)=Sof(F23A)=Sof(C49)=1-FVAR(4)
 Sof(F23)=Sof(F22)=Sof(C49A)=FVAR(4)
6.a Secondary CH2 refined with riding coordinates:
 C8(H44A,H44B), C2(H46A,H46B), C3(H49A,H49B), C4(H50A,H50B), C6(H52A,H52B),
 C10(H54A,H54B)
6.b Aromatic/amide H refined with riding coordinates:
 C36(H4), C28(H7), C40(H10), C38(H13), C22(H18), C20(H21), C18(H23), C30(H27),
 C32(H29), C34(H31), C24(H34), C26(H37), C14(H38), C15(H39), C16(H40), C12(H41),
  C13(H42)
6.c Idealised Me refined as rotating group:
 C9(H45A,H45B,H45C), C1(H48A,H48B,H48C), C5(H51A,H51B,H51C), C7(H53A,H53B,
 H53C), C11(H55A,H55B,H55C)
;
_shelx_res_checksum              60759
_shelx_hkl_checksum              30661
_olex2_submission_special_instructions 'No special instructions were received'