One-step synthesis of Mo(0) and W(0) bis(dinitrogen) complexes with the linear tetraphosphine ligand prP4: stereoselective formation of cis-[M(N2)2(rac-prP4)] and trans-[M(N2)2(meso-prP4)]; M = Mo, W.
Römer, René; Gradert, Christian; Bannwarth, Alexander; Peters, Gerhard; Näther, Christian; Tuczek, Felix; Dalton transactions (Cambridge, England : 2003) 40 (2011) 3229–3236; doi:10.1039/c0dt01646b

data_7015475
_publ_section_title
;
 One-step synthesis of Mo(0) and W(0) bis(dinitrogen) complexes with
 the linear tetraphosphine ligand prP4: stereoselective formation of
 cis-[M(N2)2(rac-prP4)] and trans-[M(N2)2(meso-prP4)]; M = Mo, W.
;
_journal_issue                   13
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              3229
_journal_page_last               3236
_journal_paper_doi               10.1039/c0dt01646b
_journal_volume                  40
_journal_year                    2011
_chemical_formula_sum            'C43 H44 Mo N4 P4'
_chemical_formula_weight         836.64
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                92.688(11)
_cell_angle_beta                 90.529(10)
_cell_angle_gamma                112.629(10)
_cell_formula_units_Z            2
_cell_length_a                   9.4885(8)
_cell_length_b                   11.4201(11)
_cell_length_c                   19.3015(17)
_cell_measurement_reflns_used    8000
_cell_measurement_temperature    170(2)
_cell_measurement_theta_max      22
_cell_measurement_theta_min      14
_cell_volume                     1927.5(3)
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      170(2)
_diffrn_measured_fraction_theta_full 0.958
_diffrn_measured_fraction_theta_max 0.958
_diffrn_measurement_device_type  'STOE IPDS-1'
_diffrn_measurement_method       'Omega scan'
_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  0.0449
_diffrn_reflns_av_sigmaI/netI    0.0565
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_number            14373
_diffrn_reflns_theta_full        26.02
_diffrn_reflns_theta_max         26.02
_diffrn_reflns_theta_min         2.15
_diffrn_standards_decay_%        none
_diffrn_standards_interval_time  0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.544
_exptl_absorpt_correction_type   none
_exptl_crystal_density_diffrn    1.442
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             864
_exptl_crystal_size_max          0.3
_exptl_crystal_size_mid          0.1
_exptl_crystal_size_min          0.1
_refine_diff_density_max         2.497
_refine_diff_density_min         -1.133
_refine_diff_density_rms         0.150
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.141
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     474
_refine_ls_number_reflns         7286
_refine_ls_number_restraints     2
_refine_ls_restrained_S_all      1.142
_refine_ls_R_factor_all          0.0952
_refine_ls_R_factor_gt           0.0725
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0462P)^2^+26.8250P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1884
_refine_ls_wR_factor_ref         0.2007
_reflns_number_gt                5725
_reflns_number_total             7286
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c0dt01646b.txt
_cod_data_source_block           felix65
_cod_original_sg_symbol_H-M      P-1
_cod_database_code               7015475