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_4343274
_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 O P2, 2(C H2 Cl2), B C24 F20'
_chemical_formula_sum            'C59 H37 B Cl4 F20 Mo O P2'
_chemical_formula_weight         1452.37
_chemical_name_systematic
;
 ?
;
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2ybc'
_space_group_name_H-M_alt        'P 1 21/c 1'
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/c 1'
_atom_sites_solution_hydrogens   mixed
_audit_creation_date             2014-12-02
_audit_creation_method
;
Olex2 1.2
(compiled 2014.07.22 svn.r2960 for OlexSys, GUI svn.r4862)
;
_cell_angle_alpha                90
_cell_angle_beta                 93.598(2)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   11.7870(6)
_cell_length_b                   17.0199(8)
_cell_length_c                   28.9129(13)
_cell_measurement_reflns_used    9962
_cell_measurement_temperature    100
_cell_volume                     5788.9(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 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  0.0735
_diffrn_reflns_av_unetI/netI     0.0644
_diffrn_reflns_laue_measured_fraction_full 1.000
_diffrn_reflns_laue_measured_fraction_max 0.996
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       22
_diffrn_reflns_limit_k_min       -22
_diffrn_reflns_limit_l_max       38
_diffrn_reflns_limit_l_min       -38
_diffrn_reflns_number            101941
_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         28.417
_diffrn_reflns_theta_min         1.389
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.574
_exptl_absorpt_correction_T_max  0.7457
_exptl_absorpt_correction_T_min  0.6362
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2012/1 (Bruker,2012) was used for absorption correction.
wR2(int) was 0.1072 before and 0.0510 after correction.
The Ratio of minimum to maximum transmission is 0.8532.
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    1.666
_exptl_crystal_description       plate
_exptl_crystal_F_000             2896
_exptl_crystal_size_max          0.29
_exptl_crystal_size_mid          0.263
_exptl_crystal_size_min          0.095
_refine_diff_density_max         1.106
_refine_diff_density_min         -1.669
_refine_diff_density_rms         0.120
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.038
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     801
_refine_ls_number_reflns         14504
_refine_ls_number_restraints     2
_refine_ls_restrained_S_all      1.038
_refine_ls_R_factor_all          0.0988
_refine_ls_R_factor_gt           0.0591
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0760P)^2^+14.2886P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1461
_refine_ls_wR_factor_ref         0.1649
_reflns_Friedel_coverage         0.000
_reflns_number_gt                10028
_reflns_number_total             14504
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ic5b00728_si_002.cif
_cod_data_source_block           zhang019b
_cod_depositor_comments
'Adding full bibliography for 4343268--4343274.cif.'
_cod_database_code               4343274
_shelxl_version_number           2013-4
_shelx_estimated_absorpt_t_max   0.948
_shelx_estimated_absorpt_t_min   0.851
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
2. Restrained distances
 Mo1-H2
 1.67 with sigma of 0.02
 C33-H2
 2.122 with sigma of 0.04
3.a Secondary CH2 refined with riding coordinates:
 C7(H7A,H7B), C8(H8A,H8B), C9(H9A,H9B), C58(H58A,H58B), C59(H59A,H59B)
3.b Aromatic/amide H refined with riding coordinates:
 C2(H7), C3(H3), C4(H4), C5(H5), C6(H6), C11(H11), C12(H12), C13(H13),
 C14(H14), C15(H15), C17(H17), C18(H18), C19(H19), C20(H20), C21(H21), C23(H23),
  C24(H24), C25(H25), C26(H26), C27(H27), C28(H28), C29(H29), C30(H30),
 C31(H31), C32(H32)
;
_shelx_res_checksum              70502
_shelx_hkl_checksum              53329
_olex2_submission_special_instructions 'No special instructions were received'