Synthesis and reactivity of molybdenum and tungsten bis(dinitrogen) complexes supported by diphosphine chelates containing pendant amines.
Weiss, Charles J.; Groves, Amy N.; Mock, Michael T.; Dougherty, William G.; Kassel, W. Scott; Helm, Monte L.; Dubois, Daniel L.; Bullock, R. Morris; Dalton transactions (Cambridge, England : 2003) 41 (2012) 4517–4529; doi:10.1039/c2dt12224c

data_7018632
_publ_section_title
;
 Synthesis and reactivity of molybdenum and tungsten bis(dinitrogen)
 complexes supported by diphosphine chelates containing pendant amines.
;
_journal_issue                   15
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              4517
_journal_page_last               4529
_journal_paper_doi               10.1039/c2dt12224c
_journal_volume                  41
_journal_year                    2012
_chemical_formula_sum            'C33 H31 Mo0.5 N3 P2'
_chemical_formula_weight         579.52
_space_group_IT_number           15
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-C 2yc'
_symmetry_space_group_name_H-M   'C 1 2/c 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                 102.277(8)
_cell_angle_gamma                90.00
_cell_formula_units_Z            8
_cell_length_a                   23.123(4)
_cell_length_b                   16.082(3)
_cell_length_c                   15.539(3)
_cell_measurement_reflns_used    6161
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      28.09
_cell_measurement_theta_min      2.87
_cell_volume                     5646.2(18)
_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 0.992
_diffrn_measured_fraction_theta_max 0.992
_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  0.0832
_diffrn_reflns_av_sigmaI/netI    0.0852
_diffrn_reflns_limit_h_max       35
_diffrn_reflns_limit_h_min       -35
_diffrn_reflns_limit_k_max       24
_diffrn_reflns_limit_k_min       -24
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_number            51596
_diffrn_reflns_theta_full        33.26
_diffrn_reflns_theta_max         33.26
_diffrn_reflns_theta_min         1.80
_exptl_absorpt_coefficient_mu    0.394
_exptl_absorpt_correction_T_max  0.9844
_exptl_absorpt_correction_T_min  0.9254
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   SADABS
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.363
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       rod
_exptl_crystal_F_000             2408
_exptl_crystal_size_max          0.20
_exptl_crystal_size_mid          0.05
_exptl_crystal_size_min          0.04
_refine_diff_density_max         0.535
_refine_diff_density_min         -0.579
_refine_diff_density_rms         0.105
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.004
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     349
_refine_ls_number_reflns         10782
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.004
_refine_ls_R_factor_all          0.0885
_refine_ls_R_factor_gt           0.0448
_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^)+(0.0388P)^2^+1.5250P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0850
_refine_ls_wR_factor_ref         0.0992
_reflns_number_gt                7228
_reflns_number_total             10782
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c2dt12224c.txt
_cod_data_source_block           trans-Mo(N2)2(PPhNBnPPh)2_(8)
_cod_depositor_comments
;
The following automatic conversions were performed:

'_symmetry_cell_setting' value 'Monoclinic' changed to 'monoclinic'
according to /home/saulius/struct/CIF-dictionaries/cif_core.dic
dictionary named 'cif_core.dic' version 2.4.1 from 2010-06-29.

Automatic conversion script
Id: cif_fix_values 1715 2011-07-08 13:25:40Z adriana 
;
_cod_original_cell_volume        5646.4(17)
_cod_original_sg_symbol_H-M      C2/c
_cod_original_formula_sum        'C33 H31 Mo0.50 N3 P2'
_cod_database_code               7018632