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_4343271
_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
'C32.62 H31.21 Mo N O P2, C32 H12 B F24.1, C6 H5 F, C5.25 H4.62 F0.87'
_chemical_formula_sum            'C75.91 H52.82 B F25.98 Mo N O P2'
_chemical_formula_weight         1657.33
_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                64.602(4)
_cell_angle_beta                 87.969(4)
_cell_angle_gamma                83.355(3)
_cell_formula_units_Z            2
_cell_length_a                   12.8744(9)
_cell_length_b                   17.2752(13)
_cell_length_c                   18.0432(14)
_cell_measurement_reflns_used    9875
_cell_measurement_temperature    100
_cell_volume                     3600.3(5)
_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 0.999
_diffrn_measured_fraction_theta_max 0.975
_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  0.0422
_diffrn_reflns_av_unetI/netI     0.0683
_diffrn_reflns_laue_measured_fraction_full 0.999
_diffrn_reflns_laue_measured_fraction_max 0.975
_diffrn_reflns_limit_h_max       19
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       26
_diffrn_reflns_limit_k_min       -25
_diffrn_reflns_limit_l_max       27
_diffrn_reflns_limit_l_min       -27
_diffrn_reflns_number            90960
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.975
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         32.457
_diffrn_reflns_theta_min         1.249
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.340
_exptl_absorpt_correction_T_max  0.7464
_exptl_absorpt_correction_T_min  0.6491
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2012/1 (Bruker,2012) was used for absorption correction.
wR2(int) was 0.0568 before and 0.0484 after correction.
The Ratio of minimum to maximum transmission is 0.8696.
The \l/2 correction factor is 0.0015.
;
_exptl_crystal_colour            'clear light red'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   light
_exptl_crystal_colour_primary    red
_exptl_crystal_density_diffrn    1.529
_exptl_crystal_description       block
_exptl_crystal_F_000             1668
_exptl_crystal_size_max          0.204
_exptl_crystal_size_mid          0.136
_exptl_crystal_size_min          0.125
_refine_diff_density_max         1.822
_refine_diff_density_min         -0.868
_refine_diff_density_rms         0.110
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.059
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1151
_refine_ls_number_reflns         25350
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.059
_refine_ls_R_factor_all          0.0941
_refine_ls_R_factor_gt           0.0596
_refine_ls_shift/su_max          0.003
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0866P)^2^+2.2601P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1530
_refine_ls_wR_factor_ref         0.1728
_reflns_Friedel_coverage         0.000
_reflns_number_gt                17725
_reflns_number_total             25350
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ic5b00728_si_002.cif
_cod_data_source_block           zhang021a
_cod_depositor_comments
'Adding full bibliography for 4343268--4343274.cif.'
_cod_database_code               4343271
_shelxl_version_number           2013-4
_shelx_estimated_absorpt_t_max   0.959
_shelx_estimated_absorpt_t_min   0.934
_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. Uiso/Uaniso restraints and constraints
Uanis(F1) = Uanis(F9)
Uanis(C37) = Uanis(C38)
Uanis(C34) = Uanis(C39)
3. Others
 Sof(C34)=Sof(C39)=Sof(H39)=Sof(C38)=Sof(H38)=Sof(C37)=Sof(C36)=Sof(C35)=
 Sof(H35)=Sof(F25)=FVAR(1)
 Sof(C28)=Sof(C33)=Sof(C32)=Sof(H32)=Sof(C31)=Sof(H31)=Sof(C30)=Sof(H30)=
 Sof(C29)=Sof(H29)=FVAR(2)
 Fixed Sof: F21(0.5) F19(0.5) F20(0.5) C60(0.5) C44(0.5) H44(0.5) C43A(0.5)
 H43A(0.5) C44A(0.5) H44A(0.5) C45A(0.5) H45A(0.5) C43(0.5) H43(0.5) C42A(0.5)
 H42A(0.5) C41A(0.5) H41A(0.5) C42(0.5) H42(0.5) C40A(0.5) F26(0.5) F80(0.5)
 C76A(0.5) C40(0.5) C45(0.5) H45(0.5) C41(0.5) H41(0.5) F7(0.5) F4(0.5)
 F1C(0.5) F1D(0.5) F1E(0.5) F1F(0.5) F23(0.5) F1(0.5) F2(0.5) F24(0.5) F1I(0.5)
 F1J(0.5) C60A(0.5) F9(0.5) C76(0.5) F22(0.5) F8(0.5)
4.a Secondary CH2 refined with riding coordinates:
 C2(H2A,H2B), C3(H3A,H3B)
4.b Aromatic/amide H refined with riding coordinates:
 C61(H61), C17(H17), C16(H16), C47(H47), C70(H70), C63(H63), C65(H65),
 C49(H49), C51(H51), C59(H59), C57(H57), C55(H55), C74(H74), C72(H72), C10(H10),
  C11(H11), C12(H12), C13(H13), C14(H14), C6(H6), C7(H7), C8(H8), C9(H9),
 C4(H4), C18(H18), C20(H20), C19(H19), C22(H22), C27(H27), C26(H26), C25(H25),
 C24(H24), C33(H33), C32(H32), C31(H31), C30(H30), C29(H29), C44(H44),
 C43A(H43A), C44A(H44A), C45A(H45A), C43(H43), C42A(H42A), C41A(H41A), C42(H42),
  C39(H39), C38(H38), C37(H37), C36(H36), C35(H35), C45(H45), C41(H41)
4.c Fitted hexagon refined as free rotating group:
 C34(C39,C38,C37,C36,C35)
4.d Idealised Me refined as rotating group:
 C21(H21A,H21B,H21C)
;
_shelx_res_checksum              53003
_shelx_hkl_checksum              94872
_olex2_computing_structure_refinement_long 'ShelXL (Sheldrick, 2008)'
_olex2_submission_special_instructions 'No special instructions were received'