Ligand properties of 1H-diphosphirenes and diphosphirenylium salts towards iron carbonyl fragments
Bourissou, Didier; Canac, Yves; Gornitzka, Heinz; Baceiredo, Antoine; Bertrand, Guy; Chemical Communications  (1999) 1535–; doi:10.1039/a904747f

data_7110620
_publ_section_title
;
 Ligand properties of 1H-diphosphirenes and diphosphirenylium salts
 towards iron carbonyl fragments
;
_journal_issue                   16
_journal_name_full               'Chemical Communications'
_journal_page_first              1535
_journal_paper_doi               10.1039/a904747f
_journal_year                    1999
_chemical_formula_sum            'C19 H28 Fe2 N2 O6 P2'
_chemical_formula_weight         554.07
_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
_cell_angle_alpha                90.00
_cell_angle_beta                 99.85(2)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   9.885(2)
_cell_length_b                   18.173(3)
_cell_length_c                   14.729(3)
_cell_measurement_reflns_used    5000
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      24.0
_cell_measurement_theta_min      1.8
_cell_volume                     2606.9(9)
_computing_cell_refinement       STOE-IPDS
_computing_data_collection       STOE-IPDS
_computing_data_reduction        STOE-IPDS
_computing_publication_material  'SHELXL-96 (Sheldrick, 1996)'
_computing_structure_refinement  'SHELXL-96 (Sheldrick, 1996)'
_computing_structure_solution    'SHELXS-96 (Sheldrick, 1990)'
_diffrn_ambient_temperature      293(2)
_diffrn_measurement_device       STOE-IPDS
_diffrn_measurement_method       Phi-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  0.1451
_diffrn_reflns_av_sigmaI/netI    0.0901
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_number            17710
_diffrn_reflns_theta_max         22.72
_diffrn_reflns_theta_min         2.24
_exptl_absorpt_coefficient_mu    1.269
_exptl_absorpt_correction_T_max  0.8889
_exptl_absorpt_correction_T_min  0.7035
_exptl_absorpt_correction_type   numerical
_exptl_crystal_colour            rouge
_exptl_crystal_density_diffrn    1.412
_exptl_crystal_description       block
_exptl_crystal_F_000             1144
_exptl_crystal_size_max          0.3
_exptl_crystal_size_mid          0.3
_exptl_crystal_size_min          0.2
_refine_diff_density_max         0.729
_refine_diff_density_min         -0.636
_refine_diff_density_rms         0.099
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_all   1.007
_refine_ls_goodness_of_fit_obs   1.078
_refine_ls_matrix_type           full
_refine_ls_number_parameters     287
_refine_ls_number_reflns         3493
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.007
_refine_ls_restrained_S_obs      1.078
_refine_ls_R_factor_all          0.1134
_refine_ls_R_factor_obs          0.0693
_refine_ls_shift/esd_max         0.000
_refine_ls_shift/esd_mean        0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.1154P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.1942
_refine_ls_wR_factor_obs         0.1628
_reflns_number_observed          2227
_reflns_number_total             3493
_reflns_observed_criterion       >2sigma(I)
_cod_data_source_file            904747fsup1.cif
_cod_data_source_block           3
_cod_depositor_comments
;
The following automatic conversions were performed:

'_refine_ls_weighting_scheme' value 'calc
w=1/[\s^2^(Fo^2^)+(0.1154P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' was
changed to 'calc'. New tag '_refine_ls_weighting_details' was
created. The value of the new tag was set to
'w=1/[\s^2^(Fo^2^)+(0.1154P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'.

Automatic conversion script
Id: cif_fix_values 3143 2015-03-26 13:38:13Z robertas 
;
_cod_original_sg_symbol_H-M      P2(1)/n
_cod_database_code               7110620