Selective formation of a unique diphosphonium-diphosphine from a tetraphosphine double protonation induced by zirconium salts
Jahel, Ali; Vologdin, Nikolay V.; Pirio, Nadine; Cattey, Hélène; Richard, Philippe; Meunier, Philippe; Hierso, Jean-Cyrille; Dalton Transactions  (2008) 4206–4208; doi:10.1039/b809244n

data_7004617
_publ_section_title
;
 Selective formation of a unique diphosphonium-diphosphine from a
 tetraphosphine double protonation induced by zirconium salts
;
_journal_issue                   32
_journal_name_full               'Dalton Transactions'
_journal_page_first              4206
_journal_page_last               4208
_journal_paper_doi               10.1039/b809244n
_journal_year                    2008
_chemical_formula_moiety
'C66 H64 Fe P4, 2(C4 H8 Cl5 O Zr), 2(C H2 Cl2)'
_chemical_formula_sum            'C76 H84 Cl14 Fe O2 P4 Zr2'
_chemical_formula_weight         1887.90
_chemical_name_systematic
;
?
;
_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
_audit_update_record
;
2008-04-07 # Formatted by publCIF
;
_cell_angle_alpha                75.800(5)
_cell_angle_beta                 89.510(5)
_cell_angle_gamma                87.002(5)
_cell_formula_units_Z            2
_cell_length_a                   12.302(5)
_cell_length_b                   18.324(5)
_cell_length_c                   19.112(5)
_cell_measurement_reflns_used    67796
_cell_measurement_temperature    115(2)
_cell_measurement_theta_max      27.485
_cell_measurement_theta_min      1
_cell_volume                     4171(2)
_computing_cell_refinement       'DENZO-SMN (Otwinowski & Minor, 1997)'
_computing_data_collection       'KappaCCD Server Software (Nonius,1997)'
_computing_data_reduction        'DENZO-SMN (Otwinowski & Minor, 1997)'
_computing_molecular_graphics    'ORTEPIII (Burnett, 1996)'
_computing_publication_material  'SHELXL97 and WinGX (Farrugia, 1999)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SIR92 (Altomare, 1993)'
_diffrn_ambient_temperature      115(2)
_diffrn_measured_fraction_theta_full 0.996
_diffrn_measured_fraction_theta_max 0.996
_diffrn_measurement_device_type  KappaCCD
_diffrn_measurement_method       '\f scans (\k = 0) + additional \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  0.0484
_diffrn_reflns_av_sigmaI/netI    0.0798
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       23
_diffrn_reflns_limit_k_min       -23
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_limit_l_min       -24
_diffrn_reflns_number            36100
_diffrn_reflns_theta_full        27.50
_diffrn_reflns_theta_max         27.50
_diffrn_reflns_theta_min         2.75
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.986
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            orange
_exptl_crystal_density_diffrn    1.503
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             1920
_exptl_crystal_size_max          0.35
_exptl_crystal_size_mid          0.15
_exptl_crystal_size_min          0.10
_refine_diff_density_max         1.302
_refine_diff_density_min         -0.829
_refine_diff_density_rms         0.092
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.057
_refine_ls_hydrogen_treatment    noref
_refine_ls_matrix_type           full
_refine_ls_number_parameters     898
_refine_ls_number_reflns         19066
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.057
_refine_ls_R_factor_all          0.0899
_refine_ls_R_factor_gt           0.0461
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0478P)^2^+0.6629P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1003
_refine_ls_wR_factor_ref         0.1131
_reflns_number_gt                12486
_reflns_number_total             19066
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            b809244n.txt
_cod_data_source_block           ali1gr
_cod_database_code               7004617