Synthesis, reactivity and structural characterisation of bicyclic tetraphosphapentazanes
Thirupathi, Natesan; Krishnamurthy, Setharampattu S.; Nethaji, Munirathinam; Journal of the Chemical Society, Dalton Transactions  (1998) 1469–; doi:10.1039/a801443d

data_7702308
_publ_section_title
;
 Synthesis, reactivity and structural characterisation of bicyclic
 tetraphosphapentazanes
;
_journal_issue                   9
_journal_name_full
'Journal of the Chemical Society, Dalton Transactions'
_journal_page_first              1469
_journal_paper_doi               10.1039/a801443d
_journal_year                    1998
_chemical_compound_source        synthesis
_chemical_formula_moiety         '[Mo(CO)4{(EtN)5P4(OPh)2}]'
_chemical_formula_sum            'C26 H35 Mo N5 O6 P4'
_chemical_formula_weight         733.41
_chemical_melting_point          416.15
_space_group_IT_number           13
_space_group_name_Hall           '-P 2yc'
_space_group_name_H-M_alt        'P 1 2/c 1'
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_H-M   'P 1 2/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL
_cell_angle_alpha                90.00
_cell_angle_beta                 111.57(2)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   17.299(5)
_cell_length_b                   12.324(5)
_cell_length_c                   17.412(6)
_cell_measurement_reflns_used    25
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      12
_cell_measurement_theta_min      8
_cell_volume                     3452(2)
_computing_cell_refinement       'least-square refinement'
_computing_data_collection       'Enraf-Nonius CAD-4 program'
_computing_data_reduction        local
_computing_molecular_graphics    'ORTEP II'
_computing_publication_material  CIF
_computing_structure_refinement  'SHELXL-93 (Sheldrick, 1993)'
_computing_structure_solution    'SHELXS-86 (Sheldrick, 1990)'
_diffrn_ambient_temperature      293(2)
_diffrn_measurement_device       'Enraf-Nonius CAD-4 diffractometer'
_diffrn_measurement_method       'w-2theta scan'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoKa
_diffrn_radiation_wavelength     0.71070
_diffrn_reflns_av_R_equivalents  0.0943
_diffrn_reflns_av_sigmaI/netI    0.0398
_diffrn_reflns_limit_h_max       20
_diffrn_reflns_limit_h_min       0
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            6345
_diffrn_reflns_theta_max         24.97
_diffrn_reflns_theta_min         1.27
_diffrn_standards_interval_count 100
_diffrn_standards_interval_time  3600
_diffrn_standards_number         3
_exptl_absorpt_coefficient_mu    0.609
_exptl_absorpt_correction_type   'not applied'
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.411
_exptl_crystal_density_meas      ?
_exptl_crystal_description       rectangular
_exptl_crystal_F_000             1504
_exptl_crystal_size_max          0.19
_exptl_crystal_size_mid          0.12
_exptl_crystal_size_min          0.10
_refine_diff_density_max         .802
_refine_diff_density_min         -1.699
_refine_diff_density_rms         .108
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_all   1.049
_refine_ls_goodness_of_fit_obs   1.035
_refine_ls_hydrogen_treatment    constraint
_refine_ls_matrix_type           full
_refine_ls_number_parameters     403
_refine_ls_number_reflns         6074
_refine_ls_number_restraints     12
_refine_ls_restrained_S_all      1.051
_refine_ls_restrained_S_obs      1.035
_refine_ls_R_factor_all          0.1001
_refine_ls_R_factor_obs          0.0644
_refine_ls_shift/esd_max         -0.939
_refine_ls_shift/esd_mean        0.022
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[s^2^(Fo^2^)+( 0.1110P)^2^+4.8012P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.1963
_refine_ls_wR_factor_obs         0.1588
_reflns_number_observed          4188
_reflns_number_total             6076
_reflns_observed_criterion       >2sigma(I)
_cod_data_source_file            d801443.txt
_cod_data_source_block           purbic
_cod_depositor_comments
;
The following automatic conversions were performed:

data item '_chemical_melting_point' value '143 degree' was changed to
'416.15' -- it was converted from degrees Celsius(C) to Kelvins(K).

data item '_exptl_crystal_density_meas' value 'not measured' was
changed to '?' -- the value is perceived as not measured.

data item '_refine_ls_weighting_scheme' value 'calc
w=1/[s^2^(Fo^2^)+( 0.1110P)^2^+4.8012P] where P=(Fo^2^+2Fc^2^)/3' was
changed to 'calc'. A new data item '_refine_ls_weighting_details' was
created with the value set to 'w=1/[s^2^(Fo^2^)+(
0.1110P)^2^+4.8012P] where P=(Fo^2^+2Fc^2^)/3'.

Automatic conversion script
Id: cif_fix_values 6909 2019-04-08 15:41:33Z antanas 
;
_cod_original_cell_volume        3452.1(21)
_cod_original_sg_symbol_H-M      P2/c
_cod_database_code               7702308