Synthesis and coordination chemistry of neutral phospha(iii)guanidines. Formation of 1-aza-3-phospha-4-metallacyclobut-1-ene rings at group 6 metalsElectronic supplementary information (ESI) available: an ORTEP representation and bond lengths and angles for 3a; crystal structure and refinement data, bond lengths and angles and an ORTEP representation of the molecular structure of Mo(CO)4(pip)2. See http://www.rsc.org/suppdata/dt/b3/b302554c/
Grundy, Joanna; Coles, Martyn P.; Hitchcock, Peter B.; Dalton Transactions  (2003) 2573–; doi:10.1039/b302554c

data_7012920
_publ_section_title
;
 Synthesis and coordination chemistry of neutral
 phospha(iii)guanidines. Formation of
 1-aza-3-phospha-4-metallacyclobut-1-ene rings at group 6
 metalsElectronic supplementary information (ESI) available: an ORTEP
 representation and bond lengths and angles for 3a; crystal structure
 and refinement data, bond lengths and angles and an ORTEP
 representation of the molecular structure of Mo(CO)4(pip)2. See
 http://www.rsc.org/suppdata/dt/b3/b302554c/
;
_journal_issue                   12
_journal_name_full               'Dalton Transactions'
_journal_page_first              2573
_journal_paper_doi               10.1039/b302554c
_journal_year                    2003
_chemical_compound_source        'synthesis as described'
_chemical_formula_moiety         'C14 H20 Mo1 N2 O4'
_chemical_formula_sum            'C14 H20 Mo N2 O4'
_chemical_formula_weight         376.26
_chemical_name_common            '[Mo(CO)4(NC5H10)2]'
_space_group_IT_number           96
_symmetry_cell_setting           tetragonal
_symmetry_Int_Tables_number      96
_symmetry_space_group_name_Hall  'P 4nw 2abw'
_symmetry_space_group_name_H-M   'P 43 21 2'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_conform_dict_location     ftp://ftp.iucr.org/pub/cif_core.dic
_audit_conform_dict_name         cif_core.dic
_audit_conform_dict_version      2.2
_audit_creation_date             2002-10-03T16:43:47-00:00
_audit_creation_method           'WinGX routine CIF_UPDATE'
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   12.0134(3)
_cell_length_b                   12.0134(3)
_cell_length_c                   11.2821(3)
_cell_measurement_reflns_used    9124
_cell_measurement_temperature    223(2)
_cell_measurement_theta_max      28
_cell_measurement_theta_min      4
_cell_measurement_wavelength     0.71073
_cell_volume                     1628.25(7)
_computing_molecular_graphics    'Ortep-3 for Windows (Farrugia, 1997)'
_computing_publication_material  'WinGX publication routines (Farrugia, 1999)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1997)'
_diffrn_ambient_temperature      223(2)
_diffrn_measured_fraction_theta_full 0.956
_diffrn_measured_fraction_theta_max 0.956
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0386
_diffrn_reflns_av_unetI/netI     0.029
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       14
_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_number            9080
_diffrn_reflns_theta_full        28.68
_diffrn_reflns_theta_max         28.68
_diffrn_reflns_theta_min         3.79
_exptl_absorpt_coefficient_mu    0.821
_exptl_absorpt_correction_T_max  0.9502
_exptl_absorpt_correction_T_min  0.8966
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
[c.f. r.h. blessing, acta cryst. (1995), a51, 33-38]
;
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.535
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             768
_exptl_crystal_size_max          0.1
_exptl_crystal_size_mid          0.1
_exptl_crystal_size_min          0.1
_refine_diff_density_max         0.426
_refine_diff_density_min         -0.414
_refine_diff_density_rms         0.055
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   0.00(5)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.047
_refine_ls_hydrogen_treatment    riding
_refine_ls_matrix_type           full
_refine_ls_number_parameters     96
_refine_ls_number_reflns         2002
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.047
_refine_ls_R_factor_all          0.0285
_refine_ls_R_factor_gt           0.0251
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0276P)^2^+0.5934P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0567
_refine_ls_wR_factor_ref         0.058
_reflns_number_gt                1883
_reflns_number_total             2002
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            b302554c.txt
_cod_data_source_block           oct702
_cod_original_sg_symbol_H-M      P4(3)2(1)2
_cod_original_formula_sum        'C14 H20 Mo1 N2 O4'
_cod_database_code               7012920