One-Pot Synthesis of Mo0 Dinitrogen Complexes Possessing Monodentate and Multidentate Phosphine Ligands
Yalan Ning; Amy A. Sarjeant; Charlotte L. Stern; Thomas H. Peterson; SonBinh T. Nguyen; Inorganic Chemistry 51 (2012) 3051–3058; doi:10.1021/ic202430m

data_4328526
_publ_section_title
;
 One-Pot Synthesis of Mo0 Dinitrogen Complexes Possessing Monodentate and
 Multidentate Phosphine Ligands
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              3051
_journal_page_last               3058
_journal_paper_doi               10.1021/ic202430m
_journal_volume                  51
_journal_year                    2012
_chemical_formula_moiety         'C54 H52 Mo P4, 2(C H3 O)'
_chemical_formula_sum            'C56 H58 Mo O2 P4'
_chemical_formula_weight         982.84
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 92.6510(10)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   9.70500(10)
_cell_length_b                   23.4962(3)
_cell_length_c                   20.9927(2)
_cell_measurement_reflns_used    9977
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      27.93
_cell_measurement_theta_min      2.43
_cell_volume                     4781.86(9)
_computing_cell_refinement       'Bruker SAINT'
_computing_data_collection       'Bruker APEX2'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 0.978
_diffrn_measured_fraction_theta_max 0.978
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0712
_diffrn_reflns_av_sigmaI/netI    0.1236
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       34
_diffrn_reflns_limit_k_min       -34
_diffrn_reflns_limit_l_max       30
_diffrn_reflns_limit_l_min       -26
_diffrn_reflns_number            71094
_diffrn_reflns_theta_full        31.16
_diffrn_reflns_theta_max         31.16
_diffrn_reflns_theta_min         1.30
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.450
_exptl_absorpt_correction_T_max  0.9923
_exptl_absorpt_correction_T_min  0.8992
_exptl_absorpt_correction_type   numerical
_exptl_absorpt_process_details   face-indexed
_exptl_crystal_colour            orange
_exptl_crystal_density_diffrn    1.365
_exptl_crystal_description       plate
_exptl_crystal_F_000             2048
_exptl_crystal_size_max          0.37
_exptl_crystal_size_mid          0.32
_exptl_crystal_size_min          0.02
_refine_diff_density_max         1.064
_refine_diff_density_min         -0.893
_refine_diff_density_rms         0.142
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.925
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     614
_refine_ls_number_reflns         15115
_refine_ls_number_restraints     43
_refine_ls_restrained_S_all      0.928
_refine_ls_R_factor_all          0.1002
_refine_ls_R_factor_gt           0.0460
_refine_ls_shift/su_max          0.006
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0489P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0962
_refine_ls_wR_factor_ref         0.1187
_reflns_number_gt                8521
_reflns_number_total             15115
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic202430m_si_003.cif
_cod_data_source_block           n0660
_cod_original_cell_volume        4781.85(9)
_cod_database_code               4328526